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Applications in the pharmaceutical industry

METTLER TOLEDO TitratorsApplication brochure 25

Introduction to the Application Brochure ´Applications in the Pharmaceutical Industry´ METTLER TOLEDO has in the past published numerous applications brochures for the various fields of industry. This new brochure, “Applications in the Pharmaceutical Industry” was however developed somewhat differently. It reflects the broad practical experience of the analytical laboratory Dr. Kade, Pharmazeutische Fabrik GmbH, in Berlin. All the applications in this brochure were developed by Kade in collaboration with an external engineering company. A selection of fifty determinations of important pharmaceutical compounds, active substances and auxiliary reagents are presented as titration applications, each with reference to the current Pharmacopoeia. The purpose or mode of action of the substances is also described in each method. Emphasis has especially been placed on detailed sample preparation, calculation of results and the chemical reactions behind the method. Multiple determinations were performed for each analysis achieving excellent standard deviations. This is due to the combination of carefully carried out analyses and the use of the Metter Toledo sample changer ST20A or Rondo60. All the methods developed and shown in this brochure were done using METTLER TOLEDO DL70ES and DL77 titrators. The DL7x range allows the use of condition functions (íf...then functions´). In this way the titration method automatically adjusts to the given conditions, such as the range of concentrations or choice of the correct equivalence point. Reliable measurements are therefore ensured throughout the analysis. With some modifications to the methods, the DL5x range of METTLER TOLEDO titrators may also be used. The presentation of this brochure mirrors the new layout developed for use with the applications found on the internet (www.titration.net). Each application has been described on three pages. The first page contains a description of the method, while the second and third pages show a copy of the method printout and the results. The method development team and METTLER TOLEDO hope that the numerous applications of METTLER TOLEDO titrators shown in this brochure will provide valuable support to the pharmaceutical industry in the development of their own methods. We wish you much success in your efforts! Dr. Kade pharmazeutische Fabrik METTLER TOLEDO Analytical Lutz Pludra Craig Gordon Dr. Walter Rathenow Dr. Hans-Joachim Muhr Dieter Rehwald METTLER TOLEDO would like to thank the development team, Lutz Pludra, Dr. Martin Rathenow and Dieter Rehwald for kindly developing this precious contribution to titration in the pharmaceutical industry.

Contents

Method Title Page

M037 Content Determination of Aspartame 1

M038 Content Determination of Benzylnicotinate 4

M039 Content Determination of Sodium Starch Glycolate 7

M040 Content Determination of Clotrimazole 10

M041 Content Determination of Dequalinium Chloride 13

M042 Content Determination of Diclofenac Sodium 16

M043 Content Determination of Diphenylpyraline Hydrochloride 19

M044 Content Determination of Diphenhydramine Hydrochloride 22

M045 Content Determination of Diprophylline 25

M046 Content Determination of Ephedrine Hydrochloride 28

M047 Content Determination of the Diethylaminoethyl Groups in Eudragit E12,5 31

M048 Content Determination of Ibuprofen-Sodium 34

M049 Content Determination of Lidocaine 37

M115 Content Determination of Piroxicam 40

M116 Content Determination of Tetrazepam 43

M117 Content Determination of Tramadol Hydrochloride 46

M118 Content Determination of Sodium Oleate in Glycerol Monostearate 49

M119 Content Determination of Acetylcysteine 52

M138 Content Determination of Acetylsalicylic Acid 55

M139 Content Determination of Allantoin 58

M140 Content Determination of Ammonium Chloride 61

M141 Content Determination of Benzyl Alcohol 64

M142 Content Determination of Carbomer 934P 67

M143 Content Determination of Cinchocain Hydrochloride 70

M144 Content Determination of Citric Acid Monohydrate 73

M145 Content Determination of Potassium Dihydrogen Phosphate 76

M146 Content Determination of Sodium Monohydrogen Phosphate 79

M147 Content Determination of Norethisterone Acetate 82

M148 Content Determination of Oxybutynine Hydrochloride 85

M149 Content Determination of Phenoxyethanol 88

M150 Content Determination of Triethanolamine 91

M160 Content Determination of Vanillin 94

M161 Content Determination of Rutoside 97

M162 Content Determination of Sodium Chloride in Sodium Starch Glycolate 100

M163 Content Determination of Hydroxyethylsalicylate 103

M164 Content Determination of Mephenesine 106

M165 Content Determination of Methyl-4-hydroxybenzoate 109

M166 Content Determination of Phenol in Liquified Phenol 112

M167 Content Determination of Ascorbic Acid (Vitamin C) 115

M168 Content Determination of Palmitoyl Ascorbic Acid 118

M169 Content Determination of Calcium in Calcium Stearate 121

M170 Content Determination of Magnesium in Magnesium Stearate 124

M171 Content Determination of 1-Monoglycerides in Solid Fat 127

M172 Content Determination of Glycerol 85% 130

M173 Content Determination of Glycerol Monostearate 40-50% 133

M174 Content Determination of Free Glycerol in Glycerol Monostearate 40-50% 136

M175 Content Determination of Ethylenediamine Disodiumacetate (Na2-EDTA) 139

M176 Content Determination of Ibuprofen 142

M177 Total Alkali and Carbonate Content of Sodium Hydroxide 145

M178 Content Determination of 2-Aminophenol 148

M037

Aspartame is an artificial sweetener which in a dilute solution has a sweetening strength of approximately180-200 times that of Saccharose. Since it is readily hydrolised, Aspartame is predominantly used as asweetener in products with a low water content.

Aspartame, M = 294.3 g/mol

Acetic acid 98% R,Formic acid, anhydrous R

c(HClO4) = 0.1 mol/L

METTLER TOLEDO DL70ES/DL77METTLER TOLEDO DL58/55+/53+

Protonation of the free amino group

R-NH2 + HClO4 → R-NH3+ClO4

-

Titration beaker ME-101974Temperature sensor DT120SP250 Peristaltic pumpRondo60 Sample changer

METTLER TOLEDO

Halogen-containing organic solvents waste.

Waste disposal

Ph. Eur. 1997; Monograph"Aspartame"

Sample preparation

Aspartame C14H18N2O5Sample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG113-SCIndication

Content Determination of Aspartame

Weigh a sample of 0.24 to 0.25 g Aspartame,accurately to 0.1 mg, in a titration beaker. Pipette1.5 mL of anhydrous formic acid into the beakerand dissolve the sample. Finally add 50 mL ofacetic acid 98%.

The previously determined loss on drying content issaved as the auxilliary value H20. As a result of thehigh expansion coefficient of the perchloric acidsolution, its temperature is measured duringstandardisation (H16) and titration (T) and acorrection factor (H5) is then calculated.

Remarks

R(%) = (Q • H5 • M/(10 • m)) + H20

Q = Titrant consumption in mmolM = Molar mass Aspartamem = Sample size in gH5 = Volume correction factorH20 = % Loss on drying of Aspartame

Calculation

Method for the acidimetric content determination of Aspartame in a non-aqueous medium

Standard THAM Tris-hydroxymethylaminomethane (M524)

L. Pludra

Author

Structure

1

EQP ET Volume Signal 1st Deriv. Time mL mV mV/mL min:s

ET1 0.0000 336.1 0:03 2.8570 348.9 4.5 0:16 4.2850 358.7 6.9 0:26

ET2 5.0000 365.0 8.8 0:34 5.2000 367.0 9.8 0:38 5.4000 369.5 12.3 0:43 5.6000 371.5 10.2 0:46 5.8000 374.4 14.7 0:52 6.0000 377.2 14.0 0:57 6.2000 380.0 14.0 1:01 6.4000 383.6 17.9 1:07 6.6000 387.4 19.3 1:13 6.8000 391.7 21.4 1:19 7.0000 396.8 25.5 1:26 7.2000 402.5 28.3 1:32 7.4000 410.5 39.9 1:40 7.5550 419.0 55.1 1:48 7.6680 427.2 72.5 1:57 7.7570 435.4 92.0 2:05 7.8280 445.0 135.1 2:13 7.8720 453.5 194.1 2:21 7.9030 461.8 266.4 2:28 7.9260 469.1 319.6 2:36 7.9470 479.1 476.7 2:44 7.9670 494.0 742.0 2:54 7.9870 523.6 1480.5 3:08

EQP1 8.0070 559.5 1795.5 3:21 8.0270 577.4 896.0 3:32 8.0470 589.0 581.0 3:41

Table of measured values

METTLER DL77 Titrator V3.1 Dr. Kade Pharm. Fabrik GmbH

Tante Elfriede Quality Control laboratory

Method: G082 Cont. Aspartame Date: 19-11-1999 11:36

User: **Pludra** Measured: 19-11-1999 11:51

RESULTS

No. ID1 Sample size and results

1/1 970820 0.2456 g R1 = 99.08 % C14H18N2O5

1/2 970820 0.2442 g R1 = 98.86 % C14H18N2O5

1/3 970820 0.2435 g R1 = 98.66 % C14H18N2O5

1/4 970820 0.2426 g R1 = 98.62 % C14H18N2O5

1/5 970820 0.2493 g R1 = 98.55 % C14H18N2O5

1/6 970820 0.2469 g R1 = 98.54 % C14H18N2O5

R2 = 22.6 °C T Titer det.

R3 = 21.7 °C T measured

STATISTICS

Number of results R1 n = 6

Mean value x = 98.72 % C14H18N2O5

Standard deviation s = 0.211833 % C14H18N2O5

Rel. standard deviation srel = 0.215 %

AUXILIARY VALUE

H5 = 1.001001 Volume corr. factor

Titration curve

Results

2

Method: G082 Cont. Aspartame Version: 19-11-1999 11:36

Title Method ID . . . . . . . . . . . . . G082 Title . . . . . . . . . . . . . . . Cont. Aspartame Date/time . . . . . . . . . . . . . 19-Nov-1999 11:36 Temperature Sensor . . . . . . . . . . . . . . . TEMP A Unit of meas. . . . . . . . . . . . oC dT [oC,oF,K] . . . . . . . . . . . . 0.02 dt [s] . . . . . . . . . . . . . . . 2.0 t(min) mode . . . . . . . . . . . . Fix t(min) [s] . . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . . . . 30.0 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.24 Upper limit [g] . . . . . . . . . 0.25 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 294.3 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . TEMP A Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . HClO4 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG113-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 5 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 250.0 Maximum volume [mL] . . . . . . . 10.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Auxiliary value ID text . . . . . . . . . . . . . . Volume corr. factor Formula . . . . . . . . . . . . . . H5=1+(H16-T)*0.0011 Calculation Result name . . . . . . . . . . . . C30H40Cl2N4 Formula . . . . . . . . . . . . . . R=(Q*H5*C/m)+H20 Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Rinse Auxiliary reagent . . . . . . . . . CH3COOH Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Calculation Result name . . . . . . . . . . . . T Titer det. Formula . . . . . . . . . . . . . . R2=H16 Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Calculation Result name . . . . . . . . . . . . T measured Formula . . . . . . . . . . . . . . R3=T Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Record Output unit . . . . . . . . . . . . Printer+Computer All results . . . . . . . . . . . . Yes

Method

3

M038

Benzylnicotinate improves local blood circulation and is used as a supportive medication in the treatment ofrheumatism.

BenzylnicotinateMG = 212.2 g/mol

50 mL Acetic anhydrideAcetic acid 98%



Protonation of the nitrogen in thepyridine ring

R-C5H4N + HClO4 → R-C5H4NH+ClO4-

Titration beaker ME-101974SP250 Peristaltic pumpTemperature sensor DT120Rondo60 Sample changer

METTLER TOLEDO

Halogen-free organic solvents waste.

Waste disposal

DAB 10.2. Nachtrag 1993;Monographie "Benzylnicotinat"(German)

Sample preparation

Benzylnicotinate C13H11NO2Sample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG113-SCIndication

Content Determination of Benzylnicotinate

Weigh a sample of 0.17 to 0.19 g Benzylnicotinate,accurately to 0.1 mg, into a titration beaker. Add50 mL of acetic anhydride R and dissolve thesample. According to DAB 10.2. Nachtrag 1993, ablank determination must be performed for each 50mL of acetic anhydride used.

As a result of the high expansion coefficient of theperchloric acid solution, its temperature is measuredduring standardisation (H16) and titration (T) and acorrection factor (H5) is then calculated.

Remarks

R(%) = (Q[2]-x) • H5 • M/(10 • m)

Q[2] = Titrant consumption in mmolx = Mean value of the blank determination inmmolM = Molar mass Benzylnicotinatem = Sample size in gH5 = Volume correction factor

Calculation

Method for the acidimetric content determination of Benzylnicotinate in a non-aqueous medium


L. Pludra

Author

Structure

4


ET1 0.0000 203.8 0:04 2.8570 421.2 76.1 0:39 4.2850 442.0 14.6 0:51

ET2 5.0000 452.0 14.0 0:59 5.2000 455.6 17.9 1:04 5.4000 458.5 14.7 1:10 5.6000 461.2 13.7 1:15 5.8000 464.3 15.4 1:20 6.0000 467.3 15.1 1:25 6.2000 470.2 14.4 1:30 6.4000 473.6 17.2 1:36 6.6000 477.3 18.2 1:42 6.8000 480.9 18.2 1:48 7.0000 485.0 20.7 1:54 7.2000 489.6 22.7 2:00 7.4000 495.1 27.7 2:06 7.6000 501.5 32.2 2:13 7.8000 510.4 44.1 2:20 7.9420 518.8 59.2 2:27 8.0490 527.5 81.8 2:35 8.1250 536.2 114.2 2:42 8.1790 544.6 155.6 2:50 8.2190 553.1 213.5 2:57 8.2480 561.3 282.4 3:04 8.2700 570.5 416.8 3:12 8.2900 582.8 616.0 3:20 8.3100 606.3 1172.5 3:29

EQP1 8.3300 698.0 4588.3 3:54 8.3500 732.3 1711.5 4:04 8.3700 752.4 1008.0 4:14



Tante Elfriede Quality Control Laboratory

Method: G018 Cont. Benzyl nicotinate Date: 07-09-1999 13:03


RESULTS


1/1 992230 40.0 mL R1 = 0.003 mmol Blank

1/2 992230 40.0 mL R1 = 0.000 mmol Blank

1/3 992230 40.0 mL R1 = 0.002 mmol Blank

1/1 992230 0.1814 g R2 = 97.954 % C13H11NO2

1/2 992230 0.1869 g R2 = 97.873 % C13H11NO2

1/3 992230 0.1899 g R2 = 97.900 % C13H11NO2

1/4 992230 0.1795 g R2 = 97.943 % C13H11NO2

1/5 992230 0.1777 g R2 = 97.872 % C13H11NO2

1/6 992230 0.1732 g R2 = 97.984 % C13H11NO2

R3 = 22.7 oC T Titer det.

R4 = 23.1 oC T measured

STATISTICS


Mean value x = 0.002 mmol Blank

Standard deviation s = 0.001622 mmol Blank


STATISTICS


Mean value x = 97.921 % C13H11NO2

Standard deviation s = 0.046187 % C13H11NO2


AUXILIARY VALUE


Titration curve

Results

5

Method: G018 Cont. Benzylnicotinate Version: 07-09-1999 13:03

Title Method ID . . . . . . . . . . . . . G018 Title . . . . . . . . . . . . . . . Cont. Benzylnicotinate Date/time . . . . . . . . . . . . . 08-Sep-1999 11:03 Temperature Sensor . . . . . . . . . . . . . . . TEMP A Unit of meas. . . . . . . . . . . . oC dT [oC,oF,K] . . . . . . . . . . . . 0.02 dt [s] . . . . . . . . . . . . . . . 2.0 t(min) mode . . . . . . . . . . . . Fix t(min) [s] . . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . . . . 30.0 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Fixed volume U Volume [mL] . . . . . . . . . . . 40.0 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 100.0 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . TEMP A Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . HClO4 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG113-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.005 dV(max) [mL] . . . . . . . 0.1 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 250.0 Maximum volume [mL] . . . . . . . 2.0 Evaluation procedure . . . . . . Standard Steepest jump only . . . . . . . Yes Calculation Result name . . . . . . . . . . . . Blank det. Formula . . . . . . . . . . . . . . R1=Q Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . mmol Decimal places . . . . . . . . . . . 3 Rinse Auxiliary reagent . . . . . . . . . CH3COOH Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes

Method Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.17 Upper limit [g] . . . . . . . . . 0.19 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 213.2 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . TEMP A Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 30 Titration Titrant . . . . . . . . . . . . . . HClO4 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG113-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 5 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 250.0 Maximum volume [mL] . . . . . . . 10.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Auxiliary value ID text . . . . . . . . . . . . . . Volume corr. Factor Formula . . . . . . . . . . . . . . H5=1+(H16-T)*0.0011 Calculation Result name . . . . . . . . . . . . C13H11NO2 Formula . . . . . . . . . . . . . . R2=(Q[2]-x)*H5*C/m Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 3 Rinse Auxiliary reagent . . . . . . . . . CH3COOH Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R2 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Calculation Result name . . . . . . . . . . . . T Titer det. Formula . . . . . . . . . . . . . . R3=H16 Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Calculation Result name . . . . . . . . . . . . T measured Formula . . . . . . . . . . . . . . R4=T Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Record Output unit . . . . . . . . . . . . Printer+Computer All results . . . . . . . . . . . . Yes

6

M039

Sodium starch glycolate, also known as Primojel, improves the disintegration time of solid drug preparationssuch as tablets and capsules.

SodiumMG= 22.99 g/mol

Acetic acid, anhydrous R



Protonation of the carboxyl group

R-COO-Na++ HClO4 → R-COOH +NaClO4

Titration beaker ME-101974SP250 Peristaltic pumpTemperature sensor DT120

METTLER TOLEDO


Waste disposal

Ph. Eur. 1997, Monograph "SodiumStarch Glycolate (Type A)"

Sample preparation

Sodium Starch GlycolateSample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG113-SCIndication

Content Determination of Sodium Starch Glycolate

Dry and crush the resulting residue from thedetermination of sodium chloride in sodium starchglycolate. Weigh 0.49 to 0.51 g of the crushedresidue, accurately to 0.1 mg, in a round bottomedflask. Add 80 mL acetic acid anhydrous to the flaskas well as to an addtional 3 empty flasks for theblank determinations, and reflux for 2 hours.Transfer the contents of the round bottomed flasksinto a titration beaker, add 20 mL anhydrous aceticacid and titrate.

As a result of the high expansion coefficient of theperchloric acid solution, its temperature is measuredduring standardisation (H16) and titration (T) and acorrection factor (H5) is then calculated.

Remarks

R(%) = (Q[2]-x) • H5 • M/(10 • m)

Q[2] = Titrant consumption in mmolx = Mean value of the blank determination inmmolM = Molar mass Sodiumm = Sample size in gH5 = Volume correction factor

Calculation

Method for the acidimetric content determination of sodium in the sodium salt of starch glycolate in anon-aqueous medium


L. Pludra

Author

Structure

7


ET1 0.0000 403.7 0:30 2.2850 431.2 12.0 0:41 3.4270 446.9 13.7 0:49

ET2 4.0000 454.3 12.9 0:55 4.2000 458.1 18.9 1:04 4.4000 463.3 26.2 1:15 4.6000 466.7 16.8 1:20 4.8000 471.0 21.4 1:24 5.0000 475.1 20.7 1:28 5.2000 481.3 31.1 1:33 5.3920 487.3 31.0 1:40 5.5920 494.5 36.4 1:45 5.7830 505.2 55.7 1:54 5.8890 511.1 56.1 1:58 6.0300 523.4 86.9 2:05 6.0980 530.4 104.0 2:13 6.1640 540.5 152.7 2:20 6.2030 547.9 190.3 2:24 6.2380 556.0 230.0 2:29 6.2670 565.0 309.0 2:34 6.2870 572.8 392.0 2:38 6.3070 582.2 472.5 2:43

EQP1 6.3270 594.2 598.5 2:49 6.3470 603.3 455.0 2:53 6.3720 614.7 456.4 2:58




Method: G032 Na Cont. in Primojel Date: 10-06-1999 8:47

User: Kuntze/Rechenb. Measured: 10-06-1999 11:48

RESULTS


1/1 992512 0.4904 g R2 = 2.948 % Na

1/2 992512 0.5018 g R2 = 2.960 % Na

1/3 992512 0.5027 g R2 = 2.955 % Na



STATISTICS


Mean value x = 2.954 % Na

Standard deviation s = 0.005867 % Na


AUXILIARY VALUE


Titration curve

Results

8

Method: G032 Na cont. in Primojel Version: 06-10-1999 8:47

Title Method ID . . . . . . . . . . . . . G032 Title . . . . . . . . . . . . . . . Na cont. in Primojel Date/time . . . . . . . . . . . . . 16-Dec-1999 14:01 Temperature Sensor . . . . . . . . . . . . . . . TEMP A Unit of meas. . . . . . . . . . . . oC dT [oC,oF,K] . . . . . . . . . . . . 0.02 dt [s] . . . . . . . . . . . . . . . 2.0 t(min) mode . . . . . . . . . . . . Fix t(min) [s] . . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . . . . 30.0 Sample Number samples . . . . . . . . . . . 2 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Fixed volume U Volume [mL] . . . . . . . . . . . 80.0 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 100.0 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . HClO4 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG113-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 0.0 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.01 dV(max) [mL] . . . . . . . 0.1 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 50.0 Maximum volume [mL] . . . . . . . 1.0 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . Blank det. Formula . . . . . . . . . . . . . . R1=Q Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . mmol Decimal places . . . . . . . . . . . 3 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes

Method Sample Number samples . . . . . . . . . . . 4 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.49 Upper limit [g] . . . . . . . . . 0.51 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 22.99 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . TEMP A Stir Speed [%] . . . . . . . . . . . . . 75 Time [s] . . . . . . . . . . . . . . 15 Titration Titrant . . . . . . . . . . . . . . HClO4 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG113-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 4.0 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 100.0 Maximum volume [mL] . . . . . . . 13.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Steepest jump only . . . . . . . Yes Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Auxiliary value ID text . . . . . . . . . . . . . . Volume corr.factor Formula . . . . . . . . . . . . . . H5=1+(H16-T)*0.0011 Calculation Result name . . . . . . . . . . . . Na Formula . . . . . . . . . . . . . . R2=(Q[2]-x)*H5*C2/m Constant . . . . . . . . . . . . . . C2=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R2 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Calculation Result name . . . . . . . . . . . . T Titer det. Formula . . . . . . . . . . . . . . R3=H16 Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Calculation Result name . . . . . . . . . . . . T measured Formula . . . . . . . . . . . . . . R4=T Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Record Output unit . . . . . . . . . . . . Printer Short-form method . . . . . . . . . Yes All results . . . . . . . . . . . . Yes

9

M040

Clotrimazole is a broad spectrum antifungal agent of the Imidazole type.

ClotrimazoleM = 344.8 g/mol

Acetic acid 98%



Protonation of the nitrogen inposition 1 of the Imidazole ring

R-NC3H3N + HClO4 →R-NH+C3H3NClO4

-


METTLER TOLEDO


Waste disposal

Ph. Eur. 1997; Monograph"Clotrimazole"

Sample preparation

Clotrimazole C22H17ClN2Sample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG113-SCIndication

Content Determination of Clotrimazole

Weigh a sample of 0.29 to 0.31 g Clotrimazol,accurately to 0.1 mg, in a titration beaker. Add 40mL acetic acid 98% into the beaker and dissolve thesample.


Remarks

R(%) = (Q • H5 • M/(10 • m)) + H20

Q = Titrant consumption in mmolM = Molar mass Clotrimazolem = Sample size in gH5 = Volume correction factorH20 = % Loss on drying of Clotrimazole

Calculation

Method for the acidimetric content determination of Clotrimazole in a non-aqueous medium


L. Pludra

Author

Structure

10


ET1 0.0000 357.3 0:03 4.2780 376.1 4.4 0:18 6.4170 394.2 8.4 0:30

ET2 7.4880 410.9 15.6 0:42 7.6880 416.2 26.6 0:49 7.8880 422.2 29.7 0:56 8.0880 429.6 37.1 1:04 8.2880 439.4 49.0 1:12 8.4520 451.2 72.1 1:21 8.5560 462.7 110.4 1:29 8.6230 472.6 147.3 1:37 8.6770 484.1 213.9 1:46 8.7120 493.7 274.0 1:54 8.7410 504.6 374.1 2:03 8.7620 513.8 440.0 2:11 8.7820 527.3 675.5 2:21 8.8020 552.1 1238.9 2:34

EQP1 8.8220 585.6 1676.5 2:47 8.8420 611.7 1305.4 2:58 8.8620 626.4 735.0 3:08




Method: G019 Cont. Clotrimazole Date: 28-09-1999 6:57

User: Ch.Dzionara Measured: 28-09-1999 15:12

RESULTS


1/1 992495 0.3049 g R1 = 100.049 % C22H17ClN2

1/2 992495 0.3016 g R1 = 99.925 % C22H17ClN2

1/3 992495 0.3078 g R1 = 99.891 % C22H17ClN2

1/4 992495 0.3097 g R1 = 100.023 % C22H17ClN2

1/5 992495 0.3101 g R1 = 99.954 % C22H17ClN2

1/6 992495 0.2929 g R1 = 100.021 % C22H17ClN2



STATISTICS


Mean value x = 99.977 % C22H17ClN2

Standard deviation s = 0.063055 % C22H17ClN2


AUXILIARY VALUE


Titration curve

Results

11

Method: G019 Cont. Clotrimazole Version: 28-09-1999 6:57

Title Method ID . . . . . . . . . . . . . G019 Title . . . . . . . . . . . . . . . Cont. Clotrimazole Date/time . . . . . . . . . . . . . 29-Jul-1999 13:46 Temperature Sensor . . . . . . . . . . . . . . . TEMP A Unit of meas. . . . . . . . . . . . oC dT [oC,oF,K] . . . . . . . . . . . . 0.02 dt [s] . . . . . . . . . . . . . . . 2.0 t(min) mode . . . . . . . . . . . . Fix t(min) [s] . . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . . . . 30.0 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.29 Upper limit [g] . . . . . . . . . 0.31 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 344.8 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . TEMP A Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 30 Titration Titrant . . . . . . . . . . . . . . HClO4 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG113-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 5 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 10.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 250.0 Maximum volume [mL] . . . . . . . 12.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Auxiliary value ID text . . . . . . . . . . . . . . Volume corr. factor Formula . . . . . . . . . . . . . . H5=1+(H16-T)*0.0011 Calculation Result name . . . . . . . . . . . . C22H17ClN2 Formula . . . . . . . . . . . . . . R=(Q*H5*C/m)+H20 Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 3 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes E - V curve . . . . . . . . . . . . Yes dE/dV - V curve . . . . . . . . . . Yes Rinse Auxiliary reagent . . . . . . . . . Acetic acid Volume [mL] . . . . . . . . . . . . 20.0 Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Calculation Result name . . . . . . . . . . . . T Titer det. Formula . . . . . . . . . . . . . . R2=H16 Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Calculation Result name . . . . . . . . . . . . T measured Formula . . . . . . . . . . . . . . R3=T Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Record Output unit . . . . . . . . . . . . Printer+Computer Short-form method . . . . . . . . . Yes All results . . . . . . . . . . . . Yes

Method

12

M041

Dequalinium Chloride is both an antibacterial and an anti-fungal agent. It is used for infections of the skinand of the mouth and throat area.

Dequalinium ChlorideM = 527.6 g/mol

Acetic anhydride RFormic acid, anhydrous R



Protonation of both free aminogroups

H2N-R-NH2 + 2HClO4 →[H3N-R-NH3]

2+(ClO4-)2


METTLER TOLEDO


Waste disposal

DAB 10; Monographie"Dequaliniumchlorid"(German)

Sample preparation

Dequalinium Chloride C30H40Cl2N4Sample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG113-SCIndication

Content Determination of Dequalinium Chloride

Weigh a sample of 0.19 to 0.21 g DequaliniumChloride, accurately to 0.1 mg, in a titration beaker.Pipette 5 mL anhydrous formic acid into the beakerand dissolve the sample. Finally add 50 mL aceticanhydride.


Remarks

R(%) = (Q • H5 • M/(10 • m)) + H20

Q = Titrant consumption in mmolM = Molar mass Dequalinium Chloridem = Sample size in gH5 = Volume correction factorH20 = % Loss on drying of Dequalinium Chloride

Calculation

Method for the acidimetric content determination of Dequalinium Chloride in a non-aqueous medium


L. Pludra

Author

Structure

13


ET1 0.0000 434.0 0:04 2.8570 468.4 12.0 0:24 4.2850 484.2 11.1 0:37

ET2 5.0000 493.9 13.6 0:46 5.2000 497.0 15.4 0:54 5.4000 500.4 17.2 1:01 5.6000 504.2 18.9 1:07 5.8000 508.1 19.6 1:12 6.0000 512.3 21.0 1:18 6.2000 517.3 24.9 1:21 6.4000 522.5 26.2 1:25 6.6000 528.8 31.5 1:29 6.8000 537.2 41.6 1:33 6.9540 546.3 59.5 1:38 7.0570 554.7 81.6 1:44 7.1340 563.2 110.0 1:50 7.1910 572.0 154.7 1:56 7.2310 580.4 208.2 2:01 7.2610 589.1 291.7 2:07 7.2820 596.1 333.3 2:13 7.3030 607.2 526.6 2:19 7.3230 624.3 857.5 2:27 7.3430 666.7 2117.5 2:44

EQP1 7.3630 710.5 2191.0 2:56 7.3830 732.0 1074.5 3:03 7.4030 743.9 598.5 3:09




Method: G021 Cont. Dequalinium chloride Date: 14-10-1999 14:25


RESULTS


1/1 991569 0.2024 g R1 = 98.09 % C30H40Cl2N4

1/2 991569 0.1944 g R1 = 98.01 % C30H40Cl2N4

1/3 991569 0.2043 g R1 = 98.10 % C30H40Cl2N4

1/4 991569 0.2004 g R1 = 98.01 % C30H40Cl2N4

1/5 991569 0.1961 g R1 = 98.06 % C30H40Cl2N4

1/6 991569 0.1999 g R1 = 97.81 % C30H40Cl2N4



STATISTICS


Mean value x = 98.01 % C30H40Cl2N4

Standard deviation s = 0.108130 % C30H40Cl2N4


AUXILIARY VALUE


Titration curve

Results

14

Method: G021 Cont. Dequalinium chloride Version: 14-10-1999 14:25

Title Method ID . . . . . . . . . . . . . G021 Title . . . . . . . . . . . . . . . Cont. Dequaliniumchloride Date/time . . . . . . . . . . . . . 14-Oct-1999 14:25 Temperature Sensor . . . . . . . . . . . . . . . TEMP A Unit of meas. . . . . . . . . . . . oC dT [oC,oF,K] . . . . . . . . . . . . 0.02 dt [s] . . . . . . . . . . . . . . . 2.0 t(min) mode . . . . . . . . . . . . Fix t(min) [s] . . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . . . . 30.0 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.19 Upper limit [g] . . . . . . . . . 0.21 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 527.6 Equivalent number z . . . . . . . . 2 Temperature sensor . . . . . . . . . TEMP A Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . HClO4 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG113-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 5 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 250.0 Maximum volume [mL] . . . . . . . 10.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Auxiliary value ID text . . . . . . . . . . . . . . Volume corr. Factor Formula . . . . . . . . . . . . . . H5=1+(H16-T)*0.0011 Calculation Result name . . . . . . . . . . . . C30H40Cl2N4 Formula . . . . . . . . . . . . . . R=(Q*H5*C/m)+H20 Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Rinse Auxiliary reagent . . . . . . . . . CH3COOH Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Printer+Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Calculation Result name . . . . . . . . . . . . T Titer det. Formula . . . . . . . . . . . . . . R2=H16 Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Calculation Result name . . . . . . . . . . . . T measured Formula . . . . . . . . . . . . . . R3=T Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Record Output unit . . . . . . . . . . . . Printer+Computer All results . . . . . . . . . . . . Yes

Method

15

M042

Diclofenac has anti-inflammatory, fever reducing and pain killing properties. It prevents the aggregation ofthrombocytes, and is not as intolerable as other similar drugs.

Diclofenac-SodiumM = 318.1 g/mol

Acetic acid 98%



Protonation of the carboxyl group.



METTLER TOLEDO


Waste disposal

Ph. Eur. 1997; Monograph"Diclofenac-Sodium"

Sample preparation

Diclofenac-Sodium C14H10Cl2NNaO2Sample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG113-SCIndication

Content Determination of Diclofenac Sodium

Weigh a sample of 0.24 to 0.26 gDiclofenac-Sodium, accurately to 0.1 mg, into atitration beaker. Add 40 mL acetic acid 98% into thebeaker and dissolve the sample.


Remarks

R(%) = (Q • H5 • M/(10 • m)) + H20

Q = Titrant consumption in mmolM = Molar mass Diclofenac-Nam = Sample size in gH5 = Volume correction factorH20 = % Loss on drying of Diclofenac -Na

Calculation

Method for the acidimetric content determination of Diclofenac-Sodium in a non-aqueous medium


L. Pludra

Author

Structure

16


ET1 0.0000 384.4 0:02 3.9440 422.4 9.7 0:20 5.9160 445.5 11.7 0:34

ET2 6.9030 464.0 18.7 0:47 7.2910 475.7 30.3 0:57 7.5290 485.5 41.2 1:05 7.7210 496.6 57.6 1:14 7.8560 507.5 80.9 1:22 7.9510 520.0 131.9 1:32 8.0050 530.3 190.6 1:41 8.0450 541.2 273.0 1:50 8.0730 553.1 422.5 2:00 8.0930 564.7 581.0 2:09 8.1130 583.4 938.0 2:20

EQP1 8.1330 610.0 1329.9 2:31 8.1530 626.5 822.5 2:42 8.1840 644.8 589.3 2:53




Method: G047 Cont. Diclofenac-Sodium Date: 16-09-1999 6:47

User: ~~Rechenberger~ Measured: 16-09-1999 7:42

RESULTS


1/1 992361 0.2593 g R1 = 100.167 % C14H10Cl2NNaO2

1/2 992361 0.2470 g R1 = 100.143 % C14H10Cl2NNaO2

1/3 992361 0.2528 g R1 = 100.411 % C14H10Cl2NNaO2

1/4 992361 0.2513 g R1 = 100.135 % C14H10Cl2NNaO2

1/5 992361 0.2524 g R1 = 100.187 % C14H10Cl2NNaO2

1/6 992361 0.2501 g R1 = 100.145 % C14H10Cl2NNaO2



STATISTICS


Mean value x = 100.198 % C14H10Cl2NNaO2

Standard deviation s = 0.105871 % C14H10Cl2NNaO2


AUXILIARY VALUE


Titration curve

Results

17

Method: G047 Cont. Diclofenac-Sodium Version: 16-09-1999 6:47

Title Method ID . . . . . . . . . . . . . G047 Title . . . . . . . . . . . . . . . Cont.Diclofenac-sodium Date/time . . . . . . . . . . . . . 16-09-1999 6:47 Temperature Sensor . . . . . . . . . . . . . . . TEMP A Unit of meas. . . . . . . . . . . . oC dT [oC,oF,K] . . . . . . . . . . . . 0.05 dt [s] . . . . . . . . . . . . . . . 2.0 t(min) mode . . . . . . . . . . . . Fix t(min) [s] . . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . . . . 30.0 Sample Number samples . . . . . . . . . . . 6 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.24 Upper limit [g] . . . . . . . . . 0.26 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 318.1 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . TEMP A Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . HClO4 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG113-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . % nom. content Metered amount [%] . . . . . . 85.0 Nominal content . . . . . . . 100.0 Conversion const. . . . . . . M/(10*z) Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 10.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.5 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 2.0 t(max) [s] . . . . . . . . . . 20.0 Threshold . . . . . . . . . . . . 100.0 Maximum volume [mL] . . . . . . . 15.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Auxiliary value ID text . . . . . . . . . . . . . . Volume corr. factor Formula . . . . . . . . . . . . . . H5=1+(H16-T)*0.0011 Calculation Result name . . . . . . . . . . . . C14H10Cl2NNaO2 Formula . . . . . . . . . . . . . . R=(Q*H5*C/m)+H20 Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 3 Rinse Auxiliary reagent . . . . . . . . . CH3COOH Volume [mL] . . . . . . . . . . . . 30.0 Record Output unit . . . . . . . . . . . . Printer+Computer Raw results last sample . . . . . . Yes Table of measured values . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Calculation Result name . . . . . . . . . . . . T Titer det. Formula . . . . . . . . . . . . . . R2=H16 Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Calculation Result name . . . . . . . . . . . . T measured Formula . . . . . . . . . . . . . . R3=T Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Record Output unit . . . . . . . . . . . . Printer+Computer All results . . . . . . . . . . . . Yes

Method

18

M043

Diphenylpyraline is an antihistamine used to treat allergic conditions.

Diphenylpyraline HydrochlorideM = 317.9 g/mol

Acetic acid, anhydrous RMercury(II)-acetate solution R:3,19 g mercury(II)-acetate in100 mL anhydrous acetic acid,neutralised with 0,1M HClO4



1. Release of the amine from theamine-hydrochloride by reaction withmercury acetate.2R-NH3

+Cl- + Hg(OAc)2 → 2R-NH2 +HgCl2 + 2HOAc2. Protonation of the amino groupR-NH2 + HClO4 → R-NH3

+ClO4-


METTLER TOLEDO

Halogen-free organic solvents waste, mercurycontaining.

Waste disposal

Ph. Eur. 1997; Monograph"Diphenylpyraline Hydrochloride"

Sample preparation

Diphenylpyraline-HCl C19H24ClNOSample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG113-SCIndication

Content Determination of Diphenylpyraline Hydrochloride

Weigh a sample of 0.19 to 0.21 gDiphenylpyraline-HCl, accurately to 0.1 mg, into atitration beaker. Pipette 30 mL anhydrous acetic acidinto the beaker and dissolve the sample. Finally add10 mL mercury(II)-acetate solution.


Remarks

R(%) = (Q • H5 • M/(10 • m)) + H20

Q = Titrant consumption in mmolM = Molar mass Diphenylpyraline-HClm = Sample size in gH5 = Volume correction factorH20 = % Loss on drying of Diphenylpyraline-HCl

Calculation

Method for the acidimetric content determination of Diphenylpyraline Hydrochloride in a non-aqueousmedium


L. Pludra

Author

Structure

19


ET1 0.0000 329.2 0:03 3.3500 344.3 4.5 0:16 5.0250 361.8 10.4 0:27

ET2 5.8630 382.2 24.4 0:38 6.0630 391.5 46.5 0:46 6.2080 401.9 71.4 0:54 6.3110 412.9 106.7 1:02 6.3810 424.8 171.0 1:10 6.4230 436.9 288.3 1:19 6.4470 446.7 405.4 1:27 6.4670 459.8 654.5 1:37 6.4870 484.8 1253.0 1:48

EQP1 6.5070 559.5 3734.4 2:05 6.5270 590.7 1561.0 2:17 6.5470 605.6 745.5 2:27




Method: G009 Cont. Diphenylpyraline-HCl Date: 22-12-1999 8:45


RESULTS


1/1 970124 0.2072 g R1 = 100.01 % C19H24ClNO

1/2 970124 0.2037 g R1 = 100.03 % C19H24ClNO

1/3 970124 0.2003 g R1 = 99.96 % C19H24ClNO

1/4 970124 0.1931 g R1 = 100.04 % C19H24ClNO

1/5 970124 0.1974 g R1 = 99.84 % C19H24ClNO

1/6 970124 0.2009 g R1 = 99.53 % C19H24ClNO



STATISTICS


Mean value x = 99.90 % C19H24ClNO

Standard deviation s = 0.195825 % C19H24ClNO


AUXILIARY VALUE


Titration curve

Results

20

Method: G009 Cont. Diphenylpyraline-HCl Version: 22-12-1999 8:45

Title Method ID . . . . . . . . . . . . . G009 Title . . . . . . . . . . . . . . Cont.Diphenylpyraline-HCl Date/time . . . . . . . . . . . . . 22-Dec-1999 8:45 Temperature Sensor . . . . . . . . . . . . . . . TEMP A Unit of meas. . . . . . . . . . . . oC dT [oC,oF,K] . . . . . . . . . . . . 0.02 dt [s] . . . . . . . . . . . . . . . 2.0 t(min) mode . . . . . . . . . . . . Fix t(min) [s] . . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . . . . 30.0 Sample Number samples . . . . . . . . . . . 6 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.19 Upper limit [g] . . . . . . . . . 0.21 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 317.9 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . TEMP A Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 30 Titration Titrant . . . . . . . . . . . . . . HClO4 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG113-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . % nom. content Metered amount [%] . . . . . . 90.0 Nominal content . . . . . . . 100.0 Conversion const. . . . . . . M/(10*z) Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 10.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 200.0 Maximum volume [mL] . . . . . . . 10.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Auxiliary value ID text . . . . . . . . . . . . . . Volume corr. factor Formula . . . . . . . . . . . . . . H5=1+(H16-T)*0.0011 Calculation Result name . . . . . . . . . . . . C19H24ClNO Formula . . . . . . . . . . . . . . R=(Q*H5*C/m)+H20 Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Rinse Auxiliary reagent . . . . . . . . . CH3COOH Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Calculation Result name . . . . . . . . . . . . T Titer det. Formula . . . . . . . . . . . . . . R2=H16 Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Calculation Result name . . . . . . . . . . . . T measured Formula . . . . . . . . . . . . . . R3=T Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes

Method

21

M044

Diphenhydramine is one of the classic antihistamines used to treat local odemas, allergic rhinitis, drugallergies and insect bites.

Diphenhydramine-HClM = 291.8 g/mol






+ClO4-


METTLER TOLEDO


Waste disposal

Ph. Eur. 1997; Monograph"Diphenhydramine Hydrochloride"

Sample preparation

Diphenhydramine-HCl C17H22ClNOSample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG113-SCIndication

Content Determination of Diphenhydramine Hydrochloride

Weigh a sample of 0.24 to 0.26 gDiphenhydramine-HCl, accurately to 0.1 mg, into atitration beaker. Pipette 30 mL anhydrous acetic acidinto the beaker and dissolve the sample. Finally add10 mL mercury(II)-acetate solution.


Remarks

R(%) = (Q • H5 • M/(10 • m)) + H20

Q = Titrant consumption in mmolM = Molar mass Diphenhydramine-HClm = Sample size in gH5 = Volume correction factorH20 = % Loss on drying of Diphen- hydramine-HCl

Calculation

Method for the acidimetric content determination of Diphenhydramine Hydrochloride in a non-aqueousmedium


L. Pludra

Author

Structure

22


ET1 0.0000 375.2 0:03 4.4220 390.6 3.5 0:18 6.6330 408.7 8.2 0:30

ET2 7.7400 429.2 18.5 0:40 7.9400 436.3 35.7 0:47 8.1280 445.3 47.7 0:55 8.2950 457.4 72.9 1:03 8.3960 469.0 114.4 1:12 8.4600 480.2 175.0 1:20 8.5020 491.3 265.0 1:29 8.5300 501.7 370.0 1:37 8.5510 513.4 560.0 1:45 8.5710 532.3 941.5 1:54

EQP1 8.5910 576.9 2229.5 2:07 8.6110 620.2 2166.4 2:20 8.6310 636.2 801.5 2:29




Method: G017 Cont. Diphenhydramine-HCl Date: 15-12-1999 7:23


RESULTS


1/1 993262 0.2511 g R1 = 100.89 % C17H22ClNO

1/2 993262 0.2502 g R1 = 100.79 % C17H22ClNO

1/3 993262 0.2415 g R1 = 100.78 % C17H22ClNO

1/4 993262 0.2481 g R1 = 100.73 % C17H22ClNO

1/5 993262 0.2467 g R1 = 100.75 % C17H22ClNO

1/6 993262 0.2433 g R1 = 100.48 % C17H22ClNO



STATISTICS





AUXILIARY VALUE


Titration curve

Results

23

Method: G017 Cont. Diphenhydramine-HCl Version: 15-12-1999 7:23

Title Method ID . . . . . . . . . . . . . G017 Title . . . . . . . . . . . . . . . Cont.Diphenhydramine-HCl Date/time . . . . . . . . . . . . . 15-Dec-1999 7:23 Temperature Sensor . . . . . . . . . . . . . . . TEMP A Unit of meas. . . . . . . . . . . . oC dT [oC,oF,K] . . . . . . . . . . . . 0.02 dt [s] . . . . . . . . . . . . . . . 2.0 t(min) mode . . . . . . . . . . . . Fix t(min) [s] . . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . . . . 30.0 Sample Number samples . . . . . . . . . . . 6 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.24 Upper limit [g] . . . . . . . . . 0.26 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 291.8 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . TEMP A Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 30 Titration Titrant . . . . . . . . . . . . . . HClO4 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG113-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . % nom. content Metered amount [%] . . . . . . 90.0 Nominal content . . . . . . . 100.0 Conversion const. . . . . . . M/(10*z) Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 10.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 200.0 Maximum volume [mL] . . . . . . . 12.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Auxiliary value ID text . . . . . . . . . . . . . . Volume corr. factor Formula . . . . . . . . . . . . . . H5=1+(H16-T)*0.0011 Calculation Result name . . . . . . . . . . . . C17H22ClNO Formula . . . . . . . . . . . . . . R=(Q*H5*C/m)+H20 Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Rinse Auxiliary reagent . . . . . . . . . CH3COOH Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Calculation Result name . . . . . . . . . . . . T Titer det. Formula . . . . . . . . . . . . . . R2=H16 Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Calculation Result name . . . . . . . . . . . . T measured Formula . . . . . . . . . . . . . . R3=T Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes

Method

24

M045

Diprophylline stimulates the central nervous system, gets rid of tiredness, improves mood and reduces thereaction time. Gastrointestinal complaints and nausea tend to be fewer than with other products such asTheophyllin.

DiprophyllineM = 254.2 g/mol

Acetic anhydride R,Formic acid, anhydrous R



Protonation of the nitrogen inposition 1 of the imidazole ring

R-NC3(CONCH3)2N + HClO4 →R-NH+C3(CONCH3)2N ClO4

-


METTLER TOLEDO


Waste disposal

Ph. Eur. 1997; Monograph"Diprophylline"

Sample preparation

Diprohylline C10H14N4O4Sample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG113-SCIndication

Content Determination of Diprophylline

Weigh a sample of 0.19 to 0.21 g Diprophylline,accurately to 0.1 mg, into a titration beaker. Pipette3 mL anhydrous formic acid into the beaker anddissolve the sample. Add 50 mL acetic anhydride.


Remarks

R(%) = (Q • H5 • M/(10 • m)) + H20

Q = Titrant consumption in mmolM = Molar mass Diprophyllinem = Sample size in gH5 = Volume correction factorH20 =% Loss on drying of Diprophylline

Calculation

Method for the acidimetric content determination of Diprophylline in a non-aqueous medium


L. Pludra

Author

Structure

25


ET1 0.0000 471.8 0:03 3.9290 581.2 27.8 0:26 5.8930 610.0 14.7 0:42

ET2 6.8760 632.2 22.5 0:56 7.0760 639.9 38.5 1:04 7.2220 647.1 49.4 1:13 7.3540 654.0 52.5 1:21 7.4970 662.4 58.7 1:30 7.6200 671.1 70.6 1:39 7.7170 679.3 85.2 1:48 7.7970 688.2 110.2 1:58 7.8560 695.2 118.6 2:06 7.9180 703.1 127.6 2:14 7.9760 711.8 150.9 2:22 8.0210 719.2 163.3 2:28 8.0660 729.0 219.3 2:37 8.0950 736.0 239.0 2:44 8.1250 743.2 242.7 2:50 8.1570 752.0 273.4 2:57 8.1830 758.9 266.5 3:03

EQP1 8.2130 767.2 275.3 3:09 8.2410 774.5 262.5 3:15 8.2730 781.5 218.7 3:21




Method: G067 Cont. Diprophylline Date: 27-09-1999 7:24


RESULTS


1/1 992459 0.2064 g R1 = 101.083 % C10H14N4O4

1/2 992459 0.1954 g R1 = 100.107 % C10H14N4O4

1/3 992459 0.1904 g R1 = 99.452 % C10H14N4O4

1/4 992459 0.1923 g R1 = 100.082 % C10H14N4O4

1/5 992459 0.1998 g R1 = 100.145 % C10H14N4O4

1/6 992459 0.1963 g R1 = 100.161 % C10H14N4O4

STATISTICS





AUXILIARY VALUE


Titration curve

Results

26

Method: G067 Cont. Diprophyllin Version: 27-09-1999 7:24

Title Method ID . . . . . . . . . . . . . G067 Title . . . . . . . . . . . . . . . Cont. Diprophyllin Date/time . . . . . . . . . . . . . 27-Sep-1999 7:24 Temperature Sensor . . . . . . . . . . . . . . . TEMP A Unit of meas. . . . . . . . . . . . oC dT [oC,oF,K] . . . . . . . . . . . . 0.02 dt [s] . . . . . . . . . . . . . . . 2.0 t(min) mode . . . . . . . . . . . . Fix t(min) [s] . . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . . . . 30.0 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.19 Upper limit [g] . . . . . . . . . 0.21 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 254.2 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . TEMP A Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 30 Titration Titrant . . . . . . . . . . . . . . HClO4 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG113-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . % nom. content Metered amount [%] . . . . . . 85.0 Nominal content . . . . . . . 100.0 Conversion const. . . . . . . M/(10*z) Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 150.0 Maximum volume [mL] . . . . . . . 10.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Auxiliary value ID text . . . . . . . . . . . . . . Volume corr. factor Formula . . . . . . . . . . . . . . H5=1+(H16-T)*0.0011 Calculation Result name . . . . . . . . . . . . C10H14N4O4 Formula . . . . . . . . . . . . . . R=(Q*H5*C/m)+H20 Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 3 Rinse Auxiliary reagent . . . . . . . . . Acetic acid Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Printer+Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Calculation Result name . . . . . . . . . . . . T Titer det. Formula . . . . . . . . . . . . . . R2=H16 Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Calculation Result name . . . . . . . . . . . . T measured Formula . . . . . . . . . . . . . . R3=T Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Record Output unit . . . . . . . . . . . . Printer+Computer All results . . . . . . . . . . . . Yes

Method

27

M046

Ephedrine Hydrochloride is an indirectly acting sympathomimeticum. It is often used in cough mixtures andcombination preparations for the treatment of bronchial asthma.

Ephedrine HydrochlorideM = 201,7 g/mol




1. Release of the amine from theamine-hydrochloride by reactionwith mercury acetate.2R-NH3


+ClO4-


METTLER TOLEDO


Waste disposal

Ph. Eur. 1997; Monograph"Ephedrine Hydrochloride"

Sample preparation

Ephedrine Hydrochloride C10H16ClNOSample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG113-SCIndication

Content Determination of Ephedrine Hydrochloride

Weigh a sample of 0.16 to 0.18 g Ephedrine-HCl,accurately to 0.1 mg, into a titration beaker. Pipette30 mL anhydrous acetic acid into the beaker anddissolve the sample. Add 10 mL mercury(II)-acetatesolution.


Remarks

R(%) = (Q • H5 • M/(10 • m)) + H20

Q = Titrant consumption in mmolM = Molar mass Ephedrine-HClm = Sample size in gH5 = Volume correction factorH20 = % Loss on drying of Ephedrine-HCl

Calculation

Method for the acidimetric content determination of Ephedrine Hydrochloride in a non-aqueous medium


L. Pludra

Author

Structure

28


ET1 0.0000 323.7 0:03 4.3320 338.4 3.4 0:18 6.4980 356.2 8.2 0:30

ET2 7.5810 376.0 18.4 0:42 7.7810 383.0 35.0 0:49 7.9740 392.3 48.2 0:58 8.1360 403.8 70.9 1:07 8.2420 416.1 116.2 1:16 8.3030 427.4 184.8 1:25 8.3420 438.5 285.4 1:34 8.3670 449.1 422.8 1:42 8.3870 462.9 689.5 1:52 8.4070 497.8 1746.5 2:06

EQP1 8.4270 571.0 3657.3 2:24 8.4470 595.9 1246.0 2:36 8.4670 609.3 672.0 2:47




Method: G086 Cont. Ephedrine-HCl Date: 22-12-1999 8:28


RESULTS


1/1 993416 0.1700 g R1 = 100.06 % C10H16ClNO

1/2 993416 0.1721 g R1 = 100.02 % C10H16ClNO

1/3 993416 0.1669 g R1 = 99.95 % C10H16ClNO

1/4 993416 0.1700 g R1 = 99.96 % C10H16ClNO

1/5 993416 0.1689 g R1 = 100.02 % C10H16ClNO

1/6 993416 0.1698 g R1 = 99.92 % C10H16ClNO



STATISTICS





AUXILIARY VALUE


Titration curve

Results

29

Method: G086 Cont. Ephedrine-HCl Version: 22-12-1999 8:28

Title Method ID . . . . . . . . . . . . . G086 Title . . . . . . . . . . . . . . . Cont. Ephedrine-HCl Date/time . . . . . . . . . . . . . 22-Dec-1999 8:28 Temperature Sensor . . . . . . . . . . . . . . . TEMP A Unit of meas. . . . . . . . . . . . oC dT [oC,oF,K] . . . . . . . . . . . . 0.02 dt [s] . . . . . . . . . . . . . . . 2.0 t(min) mode . . . . . . . . . . . . Fix t(min) [s] . . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . . . . 30.0 Sample Number samples . . . . . . . . . . . 6 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.16 Upper limit [g] . . . . . . . . . 0.18 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 201.7 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . TEMP A Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 30 Titration Titrant . . . . . . . . . . . . . . HClO4 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG113-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . % nom. content Metered amount [%] . . . . . . 90.0 Nominal content . . . . . . . 100.0 Conversion const. . . . . . . M/(10*z) Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 10.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 200.0 Maximum volume [mL] . . . . . . . 12.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Auxiliary value ID text . . . . . . . . . . . . . . Volume corr. factor Formula . . . . . . . . . . . . . . H5=1+(H16-T)*0.0011 Calculation Result name . . . . . . . . . . . . C10H16ClNO Formula . . . . . . . . . . . . . . R=(Q*H5*C/m)+H20 Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Rinse Auxiliary reagent . . . . . . . . . CH3COOH Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Calculation Result name . . . . . . . . . . . . T Titer det. Formula . . . . . . . . . . . . . . R2=H16 Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Calculation Result name . . . . . . . . . . . . T measured Formula . . . . . . . . . . . . . . R3=T Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes

Method

30

M047

Eudragit is an auxiliary reagent which when dissolved in a suitable solvent is applied for the coating oftablets, dragées and capsules. It is further used during granulation for isolating intolerable medicinalsubstances. It improves the storage and pressing properties in the process of producing tablets.

Diethylaminoethyl groupsM = 72.1 g/mol

Acetic acid, anhydrous RDeionised water R



Protonation of the Diethylaminoethylgroups.

R-C2H4N(C2H5)2 + HClO4 →R-C2H4NH+(C2H5)2 ClO4

-


METTLER TOLEDO


Waste disposal

DAB 1999, Monograph"Butylmethacrylate-(2-Diethyl-aminoethyl)methacrylate-Methyl-methacrylate-Copolymer (1:2:1)"(German)

Sample preparation

Eudragit E 12,5Sample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG113-SCIndication

Content Determination of the Diethylaminoethyl Groups in Eudragit E12,5

Weigh a sample of 0.24 to 0.26 g Eudragit E 12,5,accurately to 0.1 mg, into a titration beaker. Pipette40 mL of a mixture of 40 mL anhydrous acetic acidand 4 mL deionised water, into the beaker.


Remarks

R(%) = (Q • H5 • M/(10 • m)) + H20

Q = Titrant consumption in mmolM = Molar mass of one of the Diethylaminoethylgroupsm = Sample size in gH5 = Volume correction factorH20 =% Loss on drying of Eudragit

Calculation

Acidimetric content determination method of the Diethylaminoethyl groups in Eudragit E12,5 in anon-aqueous medium

Standard THAM Tris-hydroxymethylaminomethan (M524)

L. Pludra

Author

Structure

31


ET1 0.0000 398.1 0:03 2.8570 404.0 2.1 0:15 4.2850 409.4 3.7 0:25

ET2 5.0000 413.1 5.2 0:34 5.5000 416.5 6.9 0:43 6.0000 420.8 8.7 0:53 6.4760 426.6 12.1 1:04 6.7990 432.0 16.9 1:16 7.0280 437.1 22.0 1:28 7.2120 441.8 25.9 1:40 7.3800 447.4 32.9 1:53 7.5050 452.6 42.0 2:06 7.6020 457.6 51.2 2:18 7.6840 462.3 57.2 2:30 7.7630 467.0 59.4 2:43

EQP1 7.8440 472.4 66.5 2:58 7.9110 476.6 62.7 3:09 7.9950 482.0 65.0 3:22




Method: G040 Cont. Eudragit E 12,5 Date: 29-06-1999 7:48

User: Rechenb.Kuntze Measured: 29-06-1999 8:23

RESULTS


1/1 991499 1.978 g R1 = 23.02 % C4H10N

1/2 991499 1.9358 g R1 = 23.06 % C4H10N

1/3 991499 1.9554 g R1 = 23.19 % C4H10N

1/4 991499 1.9892 g R1 = 23.18 % C4H10N

STATISTICS


Mean value x = 23.11 % C4H10N

Standard deviation s = 0.086318 % C4H10N


AUXILIARY VALUE


Titration curve

Results

32

Method: G040 Cont. Eudragit E 12,5 Version: 29-06-1999 7:48

Title Method ID . . . . . . . . . . . . . G040 Title . . . . . . . . . . . . . . . Cont. Eudragit E 12,5 Date/time . . . . . . . . . . . . . 09-12-1999 9:56 Temperature Sensor . . . . . . . . . . . . . . . TEMP A Unit of meas. . . . . . . . . . . . oC dT [oC,oF,K] . . . . . . . . . . . . 0.05 dt [s] . . . . . . . . . . . . . . . 2.0 t(min) mode . . . . . . . . . . . . Fix t(min) [s] . . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . . . . 30.0 Sample Number samples . . . . . . . . . . . 4 Titration stand . . . . . . . . . . Stand 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.24 Upper limit [g] . . . . . . . . . 0.26 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 72.1 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . TEMP A Stir Speed [%] . . . . . . . . . . . . . 65 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . HClO4 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG113-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 5 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 5.0 Limits dV . . . . . . . . . . Relative dV(min) [%dosVol] . . . . .0.5 dV(max) [%buVol] . . . . . 5.0 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.25 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 2.0 t(max) [s] . . . . . . . . . . 20.0 Threshold . . . . . . . . . . . . 15.0 Maximum volume [mL] . . . . . . . 12.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Steepest jump only . . . . . . . .Yes Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Auxiliary value ID text . . . . . . . . . . . . . . Volume corr. factor Formula . . . . . . . . . . . . . . H5=1+(H16-T)*0.0011 Calculation Result name . . . . . . . . . . . . C4H10N Formula . . . . . . . . . . . . . . R=(Q*H5*C/(m*H20/100)) Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Record Output unit . . . . . . . . . . . . Printer+Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Calculation Result name . . . . . . . . . . . . T Titer det. Formula . . . . . . . . . . . . . . R2=H16 Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Calculation Result name . . . . . . . . . . . . T measured Formula . . . . . . . . . . . . . . R3=T Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Record Output unit . . . . . . . . . . . . Printer+Computer All results . . . . . . . . . . . . Yes

Method

33

M048

Like Ibuprofen, Ibuprofen-Sodium is an anti-inflammatory, anagelsic and fever reducing agent. It has apotency in vivo approximately 2.5 - 3 times stronger than that of acetylsalicylic acid.

Ibuprofen-SodiumM = 228.27 g/mol

Acetic acid, anhydrous R



Protonation of the carboxyl group.



METTLER TOLEDO


Waste disposal

Company Monograph"Ibuprofen-Sodium"

Sample preparation

Ibuprofen-Sodium C13H1702NaSample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG113-SCIndication

Content Determination of Ibuprofen-Sodium

Weigh a sample of 0.33 to 0.35 g Ibuprofen,accurately to 0.1 mg, into a titration beaker. Add50 mL anhydrous acetic acid to the beaker anddissolve the sample.


Remarks

R(%) = (Q • H5 • M/(10 • m)) + H20

Q = Titrant consumption in mmolM = Molar mass Ibuprofen-Nam = Sample size in gH5 = Volume correction factorH20 = % Loss on drying of Ibuprofen-Na

Calculation

Method for the acidimetric content determination of Ibuprofen-Sodium in a non-aqueous medium


L. Pludra

Author

Structure

34


ET1 0.0000 361.3 0:03 5.7140 392.2 5.4 0:21 8.5710 409.7 6.1 0:33

ET2 10.0000 421.7 8.4 0:42 10.4000 426.6 12.3 1:16 10.8000 431.5 12.3 1:22 11.2000 437.1 14.0 1:29 11.6000 444.1 17.7 1:36 12.0000 453.4 23.1 1:43 12.3500 465.4 34.2 1:51 12.5700 476.8 52.2 2:00 12.7120 488.0 78.4 2:08 12.8070 498.3 108.3 2:15 12.8790 509.7 159.4 2:23 12.9430 525.3 242.8 2:32 13.0080 557.8 500.8 2:43

EQP1 13.0730 596.5 595.5 2:54 13.1380 614.4 275.7 3:03 13.2040 625.2 163.3 3:11




Method: G068 Cont. Ibuprofen-Sodium Date: 14-10-1999 13:31


RESULTS


1/1 990598 0.3460 g R2 = 99.85 % C13H17O2Na

1/2 990598 0.3416 g R2 = 100.00 % C13H17O2Na

1/3 990598 0.3373 g R2 = 99.99 % C13H17O2Na

1/4 990598 0.3346 g R2 = 99.96 % C13H17O2Na

1/5 990598 0.3385 g R2 = 99.92 % C13H17O2Na

1/6 990598 0.3389 g R2 = 99.95 % C13H17O2Na



STATISTICS


Mean value x = 99.94 % C13H17O2Na

Standard deviation s = 0.054206 % C13H17O2Na


AUXILIARY VALUE


Titration curve

Results

35

Method: G068 Cont. Ibuprofen-Sodium Version: 14-10-1999 13:31

Title Method ID . . . . . . . . . . . . . G068 Title . . . . . . . . . . . . . . . Cont. Ibuprofen-Sodium Date/time . . . . . . . . . . . . . 14-Oct-1999 13:31 Temperature Sensor . . . . . . . . . . . . . . . TEMP A Unit of meas. . . . . . . . . . . . oC dT [oC,oF,K] . . . . . . . . . . . . 0.02 dt [s] . . . . . . . . . . . . . . . 2.0 t(min) mode . . . . . . . . . . . . Fix t(min) [s] . . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . . . . 30.0 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.33 Upper limit [g] . . . . . . . . . 0.35 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 228.27 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . TEMP A Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 30 Titration Titrant . . . . . . . . . . . . . . HClO4 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG113-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 10 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 10.0 Limits dV . . . . . . . . . . Relative dV(min) [%dosVol] . . . . . 0.5 dV(max) [%buVol] . . . . . 4.0 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 100.0 Maximum volume [mL] . . . . . . . 20.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Auxiliary value ID text . . . . . . . . . . . . . . Volume corr. factor Formula . . . . . . . . . . . . . . H5=1+(H16-T)*0.0011 Calculation Result name . . . . . . . . . . . . C13H17O2Na Formula . . . . . . . . . . . . . . R1=(Q*H5*C1/m)+H20 Constant . . . . . . . . . . . . . . C1=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Rinse Auxiliary reagent . . . . . . . . . CH3COOH Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Printer+Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Calculation Result name . . . . . . . . . . . . T Titer det. Formula . . . . . . . . . . . . . . R2=H16 Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Calculation Result name . . . . . . . . . . . . T measured Formula . . . . . . . . . . . . . . R3=T Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Record Output unit . . . . . . . . . . . . Printer+Computer All results . . . . . . . . . . . . Yes

Method

36

M049

Lidocaine is a fast acting local anaesthetic of mild strength and duration.

LidocaineM = 234.3 g/mol

Acetic anhydride R



Protonation of theDiethylamino groups

R-N(C2H5)2 + HClO4 →R-NH+(C2H5)2 ClO4

-


METTLER TOLEDO


Waste disposal

Ph. Eur. 1997; Monograph"Lidocaine"

Sample preparation

Lidocaine C14H22N2OSample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG113-SCIndication

Content Determination of Lidocaine

Weigh a sample of 0.19 to 0.21 g Lidocaine,accurately to 0.1 mg, into a titration beaker. Add50 mL acetic anhydride to the beaker and dissolvethe sample.


Remarks

R(%) = (Q • H5 • M/(10 • m)) + H20

Q = Titrant consumption in mmolM =Molar mass Lidocainem = Sample size in gH5 = Volume correction factorH20 = % Loss on drying of Lidocaine

Calculation

Method for the acidimetric content determination of Lidocaine in a non-aqueous medium


L. Pludra

Author

Structure

37


ET1 0.0000 337.0 0:03 4.0000 348.1 2.8 0:15 6.0000 361.5 6.7 0:25

ET2 7.0000 375.0 13.4 0:34 7.2000 379.2 21.0 0:40 7.4000 384.3 25.5 0:46 7.6000 390.9 33.2 0:52 7.7950 399.9 45.9 0:59 7.9310 409.4 70.0 1:06 8.0160 417.7 97.2 1:13 8.0800 426.2 132.3 1:20 8.1270 434.2 171.3 1:26 8.1650 442.4 215.5 1:33 8.1950 450.4 266.0 1:39 8.2200 458.4 322.0 1:46 8.2410 466.7 393.3 1:53 8.2610 476.1 472.5 2:00 8.2810 487.5 567.0 2:07 8.3010 504.2 836.5 2:16 8.3210 533.5 1466.4 2:26

EQP1 8.3410 577.2 2184.0 2:38 8.3610 599.2 1099.0 2:47 8.4010 621.0 544.2 2:57




Method: G027 Cont. Lidocaine Date: 14-10-1999 14:03


RESULTS


1/1 991929 0.1957 g R1 = 100.07 % C14H22N2O

1/2 991929 0.1984 g R1 = 100.14 % C14H22N2O

1/3 991929 0.1965 g R1 = 99.97 % C14H22N2O

1/4 991929 0.2097 g R1 = 100.11 % C14H22N2O

1/5 991929 0.1933 g R1 = 100.15 % C14H22N2O

1/6 991929 0.2014 g R1 = 100.15 % C14H22N2O

R2 = 22.7 °C Aux.value H16

R3 = 23.2 °C Temperature

STATISTICS


Mean value x = 100.10 % C14H22N2O

Standard deviation s = 0.070172 % C14H22N2O


AUXILIARY VALUE


Titration curve

Results

38

Method: G027 Cont. Lidocaine Version: 14-10-1999 14:03

Title Method ID . . . . . . . . . . . . . G027 Title . . . . . . . . . . . . . . . Cont. Lidocaine Date/time . . . . . . . . . . . . . 14-Oct-1999 14:03 Temperature Sensor . . . . . . . . . . . . . . . TEMP A Unit of meas. . . . . . . . . . . . oC dT [oC,oF,K] . . . . . . . . . . . . 0.02 dt [s] . . . . . . . . . . . . . . . 2.0 t(min) mode . . . . . . . . . . . . Fix t(min) [s] . . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . . . . 30.0 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.19 Upper limit [g] . . . . . . . . . 0.21 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 234.3 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . TEMP A Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 30 Titration Titrant . . . . . . . . . . . . . . HClO4 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG113-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 7.0 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 250.0 Maximum volume [mL] . . . . . . . 10.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Auxiliary value ID text . . . . . . . . . . . . . . Corr. Volume Formula . . . . . . . . . . . . . . H5=1+(H16-T)*0.0011 Calculation Result name . . . . . . . . . . . . C14H22N2O Formula . . . . . . . . . . . . . . R=(Q*H5*C/m)+H20 Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Rinse Auxiliary reagent . . . . . . . . . CH3COOH Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Printer+Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Calculation Result name . . . . . . . . . . . . Aux. value H16 Formula . . . . . . . . . . . . . . R2=H16 Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Calculation Result name . . . . . . . . . . . . Temperature Formula . . . . . . . . . . . . . . R3=T Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Record Output unit . . . . . . . . . . . . Printer+Computer All results . . . . . . . . . . . . Yes

Method

39

M115

Piroxicam is a nonsteroidal antirheumatic drug used in the treatment of rheumatoid arthritis as well as forsciatic pain.

PiroxicamM = 331.4 g/mol

Acetic anhydride RAcetic acid, anhydrous R



Protonation of the nitrogen in thepyridine ring

R-C5H4N + HClO4 → R-C5H4NH+ClO4-


METTLER TOLEDO


Waste disposal

Ph. Eur. 1997; Monograph"Piroxicam"

Sample preparation

Piroxicam C15H13N3O4SSample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG113-SCIndication

Content Determination of Piroxicam

Weigh a sample of 0.24 to 0.26 g Piroxicam,accurately to 0.1 mg, into a titration beaker.Dissolve in 60 mL of a 1:1 solution of acetic acidand acetic anhydride.


Remarks

R(%) = (Q • H5 • M/(10 • m)) + H20

Q = Titrant consumption in mmolM = Molar mass Pyroxicamm = Sample size in gH5 = Volume correction factorH20 = % Loss on drying of Pyroxicam

Calculation

Method for the acidimetric content determination of Piroxicam in a non-aqueous medium


L. Pludra

Author

Structure

40


ET1 0.0000 385.9 0:02 2.8570 424.2 13.4 0:15 4.2850 439.6 10.8 0:25

ET2 5.0000 448.7 12.7 0:32 5.2000 451.8 15.4 0:37 5.4000 454.8 15.1 0:42 5.6000 457.9 15.8 0:47 5.8000 461.4 17.5 0:53 6.0000 464.9 17.2 0:58 6.2000 468.8 19.6 1:04 6.4000 472.9 20.7 1:09 6.6000 478.0 25.5 1:14 6.8000 484.0 29.7 1:20 7.0000 491.3 36.7 1:27 7.2000 501.2 49.3 1:33 7.3610 513.2 74.8 1:40 7.4600 524.6 114.5 1:48 7.5240 536.0 178.3 1:54 7.5650 547.1 271.5 2:01 7.5920 557.7 391.5 2:09 7.6120 569.6 598.5 2:15 7.6320 587.3 882.0 2:24

EQP1 7.6520 607.5 1011.5 2:32 7.6720 622.4 745.5 2:40 7.6920 633.1 532.0 2:47




Method: G001 Cont. Piroxicam Date: 08-11-1999 11:47


RESULTS


1/1 980530 0.2529 g R1 = 100.53 % C15H13N3O4S

1/2 980530 0.2559 g R1 = 100.25 % C15H13N3O4S

1/3 980530 0.2448 g R1 = 100.38 % C15H13N3O4S

1/4 980530 0.2457 g R1 = 100.34 % C15H13N3O4S

1/5 980530 0.2551 g R1 = 100.26 % C15H13N3O4S

1/6 980530 0.2458 g R1 = 100.24 % C15H13N3O4S



STATISTICS


Mean value x = 100.33 % C15H13N3O4S

Standard deviation s = 0.111737 % C15H13N3O4S


AUXILIARY VALUE


Titration curve

Results

41

Method: G001 Cont. Piroxicam Version: 08-11-1999 11:47

Title Method ID . . . . . . . . . . . . . G001 Title . . . . . . . . . . . . . . . Cont. Piroxicam Date/time . . . . . . . . . . . . . 08-Nov-1999 11:47 Temperature Sensor . . . . . . . . . . . . . . . TEMP A Unit of meas. . . . . . . . . . . . oC dT [oC,oF,K] . . . . . . . . . . . . 0.05 dt [s] . . . . . . . . . . . . . . . 2.0 t(min) mode . . . . . . . . . . . . Fix t(min) [s] . . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . . . . 30.0 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.24 Upper limit [g] . . . . . . . . . 0.26 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 331.4 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . TEMP A Stir Speed [%] . . . . . . . . . . . . . 65 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . HClO4 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG113-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 5.0 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 10.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 2.0 t(max) [s] . . . . . . . . . . 20.0 Threshold . . . . . . . . . . . . 100.0 Maximum volume [mL] . . . . . . . 10.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Auxiliary value ID text . . . . . . . . . . . . . . Volume corr. factor Formula . . . . . . . . . . . . . . H4=1+(H16-T)*0.0011 Calculation Result name . . . . . . . . . . . . C15H13N3O4S Formula . . . . . . . . . . . . . . R=(Q*H4*C/m)+H20 Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Rinse Auxiliary reagent . . . . . . . . . Acetic acid 100% Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Calculation Result name . . . . . . . . . . . . T Titer det. Formula . . . . . . . . . . . . . . R2=T Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Calculation Result name . . . . . . . . . . . . T measured Formula . . . . . . . . . . . . . . R3=H16 Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Record Output unit . . . . . . . . . . . . Printer+Computer All results . . . . . . . . . . . . Yes

Method

42

M116

Tetrazepam is a tranquiliser and muscle relaxant.

TetrazepamM = 288.78 g/mol

Acetic acid 98%



Protonation of the unsaturatednitrogen in position 4 of thediazepin-2-one ring under theformation of hydroperchlorate salt.

R2N + HClO4 → R2NH+ClO4-


METTLER TOLEDO


Waste disposal

Method COD 1265 of 21.10.94 ofthe F.I.S. Producers, using apotentiometric end-pointdetermination according to Ph. Eur.1997 Method 2.2.20

Sample preparation

Tetrazepam C16H17ClN2OSample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG113-SCIndication

Content Determination of Tetrazepam

Weigh a sample of 0.19 to 0.21 g Tetrazepam,accurately to 0.1 mg, into a titration beaker. Add40 mL acetic acid 98% into the beaker and dissolvethe sample.


Remarks

R(%) = (Q • H5 • M/(10 • m)) + H20

Q = Titrant consumption in mmolM = Molar mass Tetrazepamm = Sample size in gH5 = Volume correction factorH20 = % Loss on drying of Tetrazepam

Calculation

Method for the acidimetric content determination of Tetrazepam in a non-aqueous medium


L. Pludra

Author

Structure

43


ET1 0.0000 405.9 0:03 3.4700 421.5 4.5 0:16 5.2050 438.2 9.6 0:28

ET2 6.0730 453.5 17.6 0:38 6.2730 459.0 27.6 0:44 6.4730 466.1 35.7 0:52 6.6730 475.4 46.2 0:59 6.8490 487.6 69.6 1:08 6.9560 499.7 112.5 1:17 7.0200 510.3 166.2 1:25 7.0650 522.0 259.8 1:33 7.0930 531.9 355.0 1:42 7.1150 543.2 512.3 1:50 7.1350 557.7 728.0 1:59 7.1550 586.2 1424.5 2:11

EQP1 7.1750 623.8 1879.5 2:25 7.1950 649.9 1305.5 2:37 7.2150 664.4 724.5 2:47




Method: G036 Cont. Tetrazepam Date: 27-09-1999 8:40


RESULTS


1/1 992229 0.2071 g R1 = 100.158 % C16H17ClN2O

1/2 992229 0.1944 g R1 = 100.066 % C16H17ClN2O

1/3 992229 0.1944 g R1 = 100.060 % C16H17ClN2O

1/4 992229 0.1922 g R1 = 99.968 % C16H17ClN2O

1/5 992229 0.1983 g R1 = 99.917 % C16H17ClN2O

1/6 992229 0.1988 g R1 = 99.935 % C16H17ClN2O



STATISTICS


Mean value x = 100.017 % C16H17ClN2O

Standard deviation s = 0.092839 % C16H17ClN2O


AUXILIARY VALUE


Titration curve

Results

44

Method: G036 Cont. Tetrazepam Version: 27-09-1999 8:40

Title Method ID . . . . . . . . . . . . . G036 Title . . . . . . . . . . . . . . . Cont. Tetrazepam Date/time . . . . . . . . . . . . . 27-Sep-1999 8:40 Temperature Sensor . . . . . . . . . . . . . . . TEMP A Unit of meas. . . . . . . . . . . . oC dT [oC,oF,K] . . . . . . . . . . . . 0.02 dt [s] . . . . . . . . . . . . . . . 2.0 t(min) mode . . . . . . . . . . . . Fix t(min) [s] . . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . . . . 30.0 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.19 Upper limit [g] . . . . . . . . . 0.21 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 288.78 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . TEMP A Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 30 Titration Titrant . . . . . . . . . . . . . . HClO4 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG113-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . % nom. content Metered amount [%] . . . . . . 85.0 Nominal content . . . . . . . 100.0 Conversion const. . . . . . . M/(10*z) Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 10.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 200.0 Maximum volume [mL] . . . . . . . 10.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Rinse Auxiliary reagent . . . . . . . . . Acetic acid Volume [mL] . . . . . . . . . . . . 30.0 Auxiliary value ID text . . . . . . . . . . . . . . Volumen corr. factor Formula . . . . . . . . . . . . . . H5=1+(H16-T)*0.0011 Calculation Result name . . . . . . . . . . . . C16H17ClN2O Formula . . . . . . . . . . . . . . R=(Q*H5*C/m)+H20 Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 3 Record Output unit . . . . . . . . . . . . Printer+Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Calculation Result name . . . . . . . . . . . . T Titer det. Formula . . . . . . . . . . . . . . R2=H16 Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Calculation Result name . . . . . . . . . . . . T measured Formula . . . . . . . . . . . . . . R3=T Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Record Output unit . . . . . . . . . . . . Printer+Computer Short-form method . . . . . . . . . Yes All results . . . . . . . . . . . . Yes

Method

45

M117

Tramadol Hydrochloride is a weaker acting synthetic derivative of Morphine. It is used for strong pain.

Tramadol HydrochlorideM = 299.8 g/mol

Acetic anhydride RAcetic acid, anhydrous RMercury(II)acetate-solution R:3,19 g mercury(II)-acetate in 100 mLanhydrous acetic acid, neutralised with0,1M HClO4





+ClO4-


METTLER TOLEDO


Waste disposal

DAC 1986, 3. Ergänzung 1991;Monographie "Tramadolhydrochlorid"(German)

Sample preparation

Tramadol Hydrochloride C16H26ClNO2Sample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG113-SCIndication

Content Determination of Tramadol Hydrochloride

Weigh a sample of 0.17 to 0.19 g TramadolHydrochloride, accurately to 0.1 mg, in a titrationbeaker. Add a mixture of 25 mL anhydrous aceticacid and 10 mL acetanhydride and dissolve thesample. Finally add 6 mL mercury(II)acetatesolution.


Remarks

R(%) = (Q • H5 • M/(10 • m)) + H20

Q = Titrant consumption in mmolM = Molar mass Tramadol-HClm = Sample size in gH5 = Volume correction factorH20 = % Loss on drying of Tramadol-HCl

Calculation

Method for the acidimetric content determination of Tramadol Hydrochloride in a non-aqueous medium


L. Pludra

Author

Structure

46

EQP ET Volumen Signal 1. Ableit. Zeit mL mV mV/mL min:s

ET1 0.0000 327.7 0:03 1.7140 336.0 4.9 0:12 2.5710 342.2 7.2 0:19

ET2 3.0000 345.7 8.2 0:25 3.2000 347.5 9.1 0:29 3.4000 349.6 10.9 0:33 3.6000 351.7 10.5 0:37 3.8000 354.3 12.6 0:42 4.0000 357.0 13.7 0:46 4.2000 360.1 15.8 0:52 4.4000 363.6 17.5 0:57 4.6000 367.6 19.6 1:03 4.8000 372.5 24.5 1:09 5.0000 378.3 29.4 1:15 5.2000 386.4 40.2 1:23 5.3950 397.2 55.3 1:31 5.5370 409.7 88.2 1:39 5.6190 420.7 134.0 1:47 5.6740 430.9 185.8 1:55 5.7160 441.0 240.0 2:03 5.7490 451.0 303.3 2:10 5.7760 460.9 368.1 2:18 5.7990 471.6 462.6 2:25 5.8190 483.4 591.5 2:34 5.8390 499.2 791.0 2:43 5.8590 533.8 1729.0 2:55

EQP1 5.8790 581.1 2362.5 3:08 5.8990 603.0 1095.5 3:18 5.9190 617.4 721.0 3:27




Method: G002 Cont. Tramadol-HCl Date: 14-10-1999 13:12


RESULTS


1/1 992133 0.1752 g R1 = 100.797 % C16H26ClNO2

1/2 992133 0.1870 g R1 = 100.363 % C16H26ClNO2

1/3 992133 0.1741 g R1 = 100.426 % C16H26ClNO2

1/4 992133 0.1787 g R1 = 100.293 % C16H26ClNO2

1/5 992133 0.1749 g R1 = 100.276 % C16H26ClNO2

1/6 992133 0.1737 g R1 = 100.244 % C16H26ClNO2



STATISTICS


Mean value x = 100.400 % C16H26ClNO2

Standard deviation s = 0.205173 % C16H26ClNO2


AUXILIARY VALUE


Titration curve

Results

47

Method: G002 Cont Tramadol-HCl Version: 14-10-1999 13:12

Title Method ID . . . . . . . . . . . . . G002 Title . . . . . . . . . . . . . . . Cont. Tramadol-HCl Date/time . . . . . . . . . . . . . 14-Oct-1999 13:12 Temperature Sensor . . . . . . . . . . . . . . . TEMP A Unit of meas. . . . . . . . . . . . oC dT [oC,oF,K] . . . . . . . . . . . . 0.02 dt [s] . . . . . . . . . . . . . . . 2.0 t(min) mode . . . . . . . . . . . . Fix t(min) [s] . . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . . . . 30.0 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.17 Upper limit [g] . . . . . . . . . 0.19 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 299.8 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . TEMP A Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 30 Titration Titrant . . . . . . . . . . . . . . HClO4 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG113-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 3 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 10.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 200.0 Maximum volume [mL] . . . . . . . 10.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Auxiliary value ID text . . . . . . . . . . . . . . Volume corr. factor Formula . . . . . . . . . . . . . . H5=1+(H16-T)*0.0011 Calculation Result name . . . . . . . . . . . . C16H26ClNO2 Formula . . . . . . . . . . . . . . R=(Q*H5*C/m)+H20 Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 3 Rinse Auxiliary reagent . . . . . . . . . CH3COOH Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Printer+Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Calculation Result name . . . . . . . . . . . . T Titer det. Formula . . . . . . . . . . . . . . R2=H16 Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Calculation Result name . . . . . . . . . . . . T measured Formula . . . . . . . . . . . . . . R3=T Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . oC Decimal places . . . . . . . . . . . 1 Record Output unit . . . . . . . . . . . . Printer+Computer All results . . . . . . . . . . . . Yes

Method

48

M118

Sodium Oleate is a water-in-oil emulsifier used as the consistency-giving factor in ointments and creams. Itis also used as a lubricant in the production of tablets and as an additive for controlled-release preparations.

Sodium OleateM = 304.45 g/mol

Acetone R

c(HCl) = 0.1 mol/L

METTLER TOLEDO DL70ES/DL77METTLER TOLEDODL58/55/53/50Graphix

Protonation of the carboxyl group


Titration beaker ME-101974SP250 Peristaltic pumpRondo60 Sample changerHeat exchanger ME-23834

METTLER TOLEDO


Waste disposal

Ph. Eur. 1997; Monograph "GlycerolMonostearate 40-50%"

Sample preparation

Glycerol Monostearate C18H33NaO2Sample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG111-SCIndication

Content Determination of Sodium Oleate in Glycerol Monostearate

Weigh a sample of 9.9 to 10.1 g GlycerolMonostereate, accurately to 0.1 mg, in a 100 mLtitration beaker. Add 60 mL acetone.

The dissolution of the sample occurs on the titrator atapproximately 50°C. Where no sample heater isused, the sample must be pre-heated in a water orultrasonic bath at approximately 50°C, until a milkysuspension appears.

Remarks

R(%) = (Q + 0.016)• M/(10 • m)

Q = Titrant consumption in mmolM = Molar mass Sodium Oleatem = Sample size in g0.016 mmol = Previously determined blank valuederived from the neutralisation of acetone

Calculation

Method for the acidimetric content determination of Sodium Oleate in a non-aqueous medium


L. Pludra

Author

Structure

49


ET1 0.0000 -124.2 0:03 0.0200 -124.0 10.5 0:06 0.0400 -123.7 17.5 0:09 0.0800 -123.1 15.8 0:13 \\ \\ \\ \\ 17.0650 25.8 21.3 8:40 17.2650 30.7 24.5 8:44 17.4650 36.4 28.3 8:48 17.6650 42.8 32.2 8:53 17.8650 50.8 39.9 8:57 18.0330 58.9 47.9 9:01 18.1760 67.0 56.8 9:06 18.2975 75.2 67.4 9:10 18.4000 83.2 77.9 9:15 18.4905 91.2 88.9 9:20 18.5700 99.4 103.0 9:25 18.6380 107.2 114.3 9:30 18.7015 115.6 132.3 9:36 18.7545 124.1 161.1 9:42 18.7965 131.5 175.0 9:48 18.8385 140.4 213.3 9:55 18.8700 147.8 233.3 10:02 18.9015 156.2 268.9 10:09

EQP1 18.9275 164.1 304.2 10:16 18.9510 170.4 265.1 10:22 18.9860 180.7 294.0 10:29




Method: G049 Cont. Sodium oleate Date: 16-12-1999 10:52


RESULTS


1/1 993268 9.9202 g R1 = 5.89 % C18H33NaO2

1/2 993268 10.0341 g R1 = 5.89 % C18H33NaO2

1/3 993268 10.0194 g R1 = 5.87 % C18H33NaO2

1/4 993268 10.0042 g R1 = 5.90 % C18H33NaO2

1/5 993268 9.9648 g R1 = 5.93 % C18H33NaO2

1/6 993268 9.9636 g R1 = 5.83 % C18H33NaO2

STATISTICS

No. results R1 n = 6

Mean value x = 5.89 % C18H33NaO2

Standard deviation s = 0.034472 % C18H33NaO2

Rel. standard deviation srel = 0.586

Titration curve

Results

50

Method: G049 Cont. Sodium oleate Version: 16-12-1999 10:52

Title Method ID . . . . . . . . . . . . . G049 Title . . . . . . . . . . . . . . . Cont. Sodium Oleate Date/time . . . . . . . . . . . . . 16-Dec-1999 11:47 Sample Number samples . . . . . . . . . . . 6 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 9.9 Upper limit [g] . . . . . . . . . 10.1 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 304.45 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 75 Time [s] . . . . . . . . . . . . . . 120 Titration Titrant . . . . . . . . . . . . . . HCl Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG111-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 15 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 100.0 Maximum volume [mL] . . . . . . . 30.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . C18H33NaO2 Formula . . . . . . . . . . . . . . R=(Q+0.016)*C/m Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Rinse Auxiliary reagent . . . . . . . . . Water Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes

Method

51

M119

Acetylcysteine is an expectorant which works by reducing the viscosity of tough mucous in the air passages.

AcetylcysteineM = 163.2 g/mol

Deionised water

c(NaOH) = 0.5 mol/L


Deprotonation of the carboxyl group

R-COOH + NaOH → RCOONa +H2O

Titration beaker ME-101974SP250 Peristaltic pumpRondo60 Sample changer

METTLER TOLEDO


Waste disposal

Ph. Eur. 1997; Monograph"Acetylcysteine"

Sample preparation

Acetylcysteine C5H9NO3SSample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG111-SCIndication

Content Determination of Acetylcysteine

Weigh a sample of 0.14 to 0.16 g Acetylcysteine,accurately to 0.1 mg, in a 100 mL titration beaker.Dissolve in 50 mL deionised water.

The previously determined loss on drying content issaved as the auxilliary value H20.

Remarks

R(%) = (Q • M/(10 • m)) + H20

Q = Titrant consumption in mmolM = Molar mass Acetylcysteinem = Sample size in gH20 = % Loss on drying of Acetylcysteine

Calculation

Method for the alkalimetric content determination of Acetylcysteine.

Standard Potassium hydrogen phthalate(M521)

L. Pludra

Author

Structure

52


ET1 0.0000 257.0 0:03 3.4280 229.7 -8.0 0:16 5.1420 214.9 -8.6 0:24

ET2 6.0000 206.5 -9.8 0:31 6.2000 204.5 -9.8 0:34 6.4000 202.3 -11.2 0:39 6.6000 200.3 -10.2 0:43 6.8000 197.7 -13.0 0:47 7.0000 195.0 -13.3 0:51 \\ \\ \\ \\ 9.0410 124.7 -134.9 2:08 9.0900 116.9 -158.6 2:17 9.1330 106.1 -250.7 2:29 9.1560 100.2 -258.7 2:38 9.1850 87.4 -441.7 2:52 9.2050 77.2 -507.5 3:07 9.2250 68.7 -423.5 3:19 9.2480 54.7 -611.7 3:37 9.2680 42.0 -633.5 3:54 9.2880 24.0 -899.5 4:20

EQP1 9.3080 2.7 -1064.0 4:49 9.3280 -14.9 -882.0 5:15 9.3480 -26.9 -598.5 5:33




Method: G012 Cont. Acetylcysteine Date: 09-11-1999 11:03


RESULTS


1/1 941726 0.1508 g R1 = 100.56 % C5H9NO3S

1/2 941726 0.155 g R1 = 100.48 % C5H9NO3S

1/3 941726 0.1465 g R1 = 100.36 % C5H9NO3S

1/4 941726 0.1579 g R1 = 100.31 % C5H9NO3S

1/5 941726 0.1482 g R1 = 100.70 % C5H9NO3S

1/6 941726 0.1456 g R1 = 100.44 % C5H9NO3S

STATISTICS


Mean value x = 100.47 % C5H9NO3S

Standard deviation s = 0.140367 % C5H9NO3S


Titration curve

Results

53

Method: G012 Cont. Acetylcysteine Version: 09-11-1999 11:03

Title Method ID . . . . . . . . . . . . . G012 Title . . . . . . . . . . . . . . . Cont. Acetylcysteine Date/time . . . . . . . . . . . . . 09-Nov-1999 11:03 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.14 Upper limit [g] . . . . . . . . . 0.16 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 163.2 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 65 Time [s] . . . . . . . . . . . . . . 45 Titration Titrant . . . . . . . . . . . . . . NaOH Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG111-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 6 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 500.0 Maximum volume [mL] . . . . . . . 11.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . C5H9NO3S Formula . . . . . . . . . . . . . . R=(Q*C/m)+H20 Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Rinse Auxiliary reagent . . . . . . . . . Water Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes

Method

54

M138

Acetylsalicylic Acid belongs to the group of non-opioid analgesics. It reduces fever and is a good pain killerand anti-inflammatory.

Acetylsalicylic AcidM = 180.2 g/mol

Deionised water REthanol 96% R

c(NaOH) = 0.1 mol/Lc(HCl) = 0.5 mol/L

METTLER TOLEDO DL70ES/DL77METTLER TOLEDO DL58/55

1. Deprotonation of the carboxylgroup with sodium hydroxide inexcessR-COOH + NaOH → RCOONa +H2O2. Neutralisation of the excesssodium hydroxide

NaOH+ HCl → H O + NaCl


METTLER TOLEDO


Waste disposal

Ph. Eur. 1997; Monographie"Acetylsalicylic Acid"

Sample preparation

Acetylsalicylic Acid C9H8O4Sample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG111-SCIndication

Content Determination of Acetylsalicylic Acid

Weigh a sample of 0.450 to 0.550 g AcetylsalicylicAcid, accurately to 0.1 mg, in a 100 mL titrationbeaker and dissolve with 10 mL ethanol R. Add30 mL deionised water. Dose with 25.0 mL 0.1 Msodium hydroxide solution and titrate with 0.5 Mhydrochloric acid.For the blank determination, prepare three titrationbeakers, each with 10 mL ethanol 96% in 30 mLdeionised water.

The previously determined loss on drying content issaved as the auxilliary value H20.The amount of titrant used in the blank determinationis greater than that used in the actual determinationsince the content of acidic substances is muchlower.

Remarks

R(%) = (x-Q) • M • F/(10 • m)Q = Titrant consumption in mmolx = Mean value of the blank determination inmmolF = 100/(100-H20) Formula for the loss ondrying of Acetylsalicylic acidM = Molar mass Acetylsalicylic acidm = Sample size in g

Calculation

Method for the alkalimetric content determination of Acetylsalicylic Acid

Standard Potassium hydrogen phthalate(M521), THAM (M522)

L. Pludra

Author

Structure

55


ET1 0.0000 -375.8 0:03 5.7140 -364.8 1.9 0:19 8.5710 -353.9 3.8 0:30

ET2 10.0000 -345.8 5.7 0:38 10.2000 -342.8 15.1 1:09 10.4000 -341.4 7.0 1:13 10.6000 -340.0 7.0 1:17 10.8000 -338.2 8.8 1:21 11.0000 -336.5 8.8 1:25

\\ \\ \\ \\ 13.0000 -307.2 23.4 2:12 13.2000 -301.3 29.0 2:18 13.4000 -293.6 38.8 2:24 13.5640 -284.7 54.2 2:30 13.6790 -276.1 74.9 2:36 13.7620 -267.0 109.6 2:43 13.8170 -258.5 154.0 2:49 13.8570 -250.0 211.7 2:55 13.8860 -241.3 301.7 3:02 13.9060 -234.3 350.0 3:08 13.9260 -222.5 588.0 3:15 13.9460 -206.3 812.0 3:23 13.9660 -162.8 2173.4 3:39 13.9860 -87.1 3783.5 4:09

EQP1 14.0060 122.8 10496.0 4:32 14.0260 156.4 1683.5 4:41 14.0460 167.6 556.5 4:47




Method: G084 Acetylsalicylic acid Date: 21-12-1999 9:49


RESULTS


1/1 982047 25.0 mL R1 = 12.564 mmol Blank

1/2 982047 25.0 mL R1 = 12.560 mmol Blank

1/3 982047 25.0 mL R1 = 12.560 mmol Blank

2/1 982047 0.1814 g R2 = 99.65 % C9H8O4

2/2 982047 0.1869 g R2 = 99.53 % C9H8O4

2/3 982047 0.1899 g R2 = 99.45 % C9H8O4

2/4 982047 0.1795 g R2 = 99.59 % C9H8O4

2/5 982047 0.1777 g R2 = 99.49 % C9H8O4

2/6 982047 0.1732 g R2 = 99.59 % C9H8O4

STATISTICS





STATISTICS


Mean value x = 99.55 % C9H8O4

Standard deviation s = 0.072442 % C9H8O4


Titration curve

Results

56

Method: G084 Cont. Acetylsalicylic acid Version: 21-12-1999 9:49

Title Method ID . . . . . . . . . . . . . G084 Title . . . . . . . . . . . . . .Cont. Acetylsalicylicacid Date/time . . . . . . . . . . . . . 21-Dec-1999 9:49 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Fixed volume U Volume [mL] . . . . . . . . . . . 25.0 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 100.0 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . HCl Concentration [mol/L] . . . . . . . 0.5 Sensor . . . . . . . . . . . . . . . DG111-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 20 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 150.0 Maximum volume [mL] . . . . . . . 30.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . Blank Formula . . . . . . . . . . . . . . R1=Q Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . mmol Decimal places . . . . . . . . . . . 3 Rinse Auxiliary reagent . . . . . . . . . Water Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Computer Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes

Method Sample Number samples . . . . . . . . . . . 6 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.4 Upper limit [g] . . . . . . . . . 0.6 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 180.2 Equivalent number z . . . . . . . . 2 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . HCl Concentration [mol/L] . . . . . . . 0.5 Sensor . . . . . . . . . . . . . . . DG111-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 10 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 150.0 Maximum volume [mL] . . . . . . . 30.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . C9H8O4 Formula . . . . . . . . . . . . . . R2=(x-Q[2])*C*100/m Constant . . . . . . . . . . . . . . C=M/(10*z*(100-H20)) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Rinse Auxiliary reagent . . . . . . . . . Water Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Computer Statistics Ri (i=index) . . . . . . . . . . . . R2 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes

57

M139

Allantoin is applied externally for the treatment of wounds. It is also used in cosmetic and sun-protectioncreams.

AllantoinM = 158.1 g/mol

Deionised water R

c(NaOH) = 0.1 mol/L


Allantoin acts as a weak acid becauseof the tautomerisation of the keto- toenol- forms in an aqueous medium.R-CO-NH-R (Keto) ↔ R-COH=N-R (Enol)

R-COH=N-R + NaOH →[RCO=N-R]-Na+ + H2O


METTLER TOLEDO


Waste disposal

Ph. Eur. 1997 supplement 1999;Monograph "Allantoin"

Sample preparation

Allantoin C4H6N4O3Sample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG111-SCIndication

Content Determination of Allantoin

Weigh a sample of 0.11 to 0.13 g Allantoin,accurately to 0.1 mg, into a 100 mL titration beakerand dissolve in 50 mL deionised water.


Remarks

R(%) = (Q • M/(10 • m)) + H20

Q = Titrant consumption in mmolM = Molar mass Allantoinm = Sample size in gH20 = % Loss on drying of Allantoin

Calculation

Method for the alkalimetric content determination of Allantoin


L. Pludra

Author

Structure

58


ET1 0.0000 65.0 0:30 3.4280 -88.4 -44.7 0:50 5.1420 -109.3 -12.2 1:02

ET2 6.0000 -121.0 -13.5 1:11 6.2000 -124.3 -16.8 1:17 6.4000 -127.7 -16.8 1:23 6.6000 -131.1 -17.2 1:29 6.8000 -134.7 -17.9 1:35 7.0000 -138.9 -21.0 1:42 7.2000 -143.4 -22.4 1:49 7.4000 -148.4 -25.2 1:56 7.6000 -154.3 -29.4 2:04 7.8000 -161.1 -33.9 2:11 8.0000 -169.8 -43.7 2:19 8.1490 -178.1 -55.9 2:29 8.2660 -185.2 -60.4 2:36 8.3890 -193.7 -68.9 2:44

EQP1 8.4920 -201.0 -71.4 2:52 8.6000 -208.5 -69.4 3:00 8.7180 -215.4 -58.1 3:07 8.8880 -223.7 -49.0 3:14 9.0000 -228.1 -38.7 3:20




Method: G010 Cont. Allantoin Date: 09-11-1999 13:52


RESULTS


1/1 991423 0.1318 g R1 = 100.98 % C4H6N4O3

1/2 991423 0.1182 g R1 = 100.57 % C4H6N4O3

1/3 991423 0.1197 g R1 = 100.52 % C4H6N4O3

1/4 991423 0.1225 g R1 = 100.61 % C4H6N4O3

1/5 991423 0.1292 g R1 = 100.91 % C4H6N4O3

1/6 991423 0.1295 g R1 = 100.70 % C4H6N4O3

STATISTICS





Titration curve

Results

59

Method: G010 Cont. Allantoin Version: 09-11-1999 13:52

Title Method ID . . . . . . . . . . . . . G010 Title . . . . . . . . . . . . . . . Cont. Allantoin Date/time . . . . . . . . . . . . . 09-Nov-1999 13:52 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.11 Upper limit [g] . . . . . . . . . 0.13 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 158.1 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 30 Titration Titrant . . . . . . . . . . . . . . NaOH Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG111-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 6.0 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 10.0 Maximum volume [mL] . . . . . . . 9.0 Evaluation procedure . . . . . . Standard Steepest jump only . . . . . . . Yes Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . C4H6N4O3 Formula . . . . . . . . . . . . . . R=(Q*C/m)+H20 Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Rinse Auxiliary reagent . . . . . . . . . Water Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes

Method

60

M140

Ammonium Chloride is an expectorant. It promotes secretion production in the bronchi and accelerates therelease of the secretions. It also promotes the elimination of lead and basic drugs (amphetamines) and istherefore used in cases of poisoning.

Ammonium ChlorideM = 53.49 g/mol

Formaldehyde solution 35% RDeionised water

c(NaOH) = 1 mol/Lc(NaOH) = 0.1 mol/L


1. Formaldehyde reacts withammonium chloride to givehexamethylenetetramine while releasinghydrochloric acid:4NH4Cl + 6H2CO → (CH2)6N4 + 4HCl +6H2O2. Titration of hydrochloric acid withNaOH:HCl N OH N Cl H O


METTLER TOLEDO


Waste disposal

Ph. Eur. 1997; Monograph"Ammonium Chloride"

Sample preparation

Ammonium Chloride, NH4ClSample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG111-SCIndication

Content Determination of Ammonium Chloride

Add 40 mL formaldehyde solution into a titrationbeaker and neutralise with 0.1M NaOH. Weigh 0.99to 1.01 g ammonium chloride in a 100 mL titrationbeaker. Add 40 mL deionised water and 5 mL of theneutralised formaldehyde solution.


Remarks

R(%) = (Q • M/(10 • m)) + H20

Q = Titrant consumption in mmolM = Molar mass Ammonium Chloridem = Sample size in gH20 = % Loss on drying of Ammonium Chloride

Calculation

Method for the alkalimetric content determination of Ammonium Chloride


L. Pludra

Author

Structure

61


ET1 0.0000 198.0 0:17 9.7140 83.7 -11.8 0:57 14.5710 61.5 -4.6 1:53

ET2 17.0000 34.0 -11.3 2:18 17.2000 30.7 -16.8 2:29 17.4000 25.8 -24.5 2:37 17.5550 22.5 -21.2 2:49 17.7550 15.1 -36.7 2:54 17.8500 11.5 -38.3 2:58 17.9750 5.5 -47.6 3:03 18.0620 1.4 -47.5 3:09 18.1670 -4.8 -58.7 3:13 18.2380 -9.2 -63.1 3:19 18.3120 -15.1 -79.5 3:23 18.3640 -19.6 -86.2 3:30 18.4170 -24.8 -97.7 3:36 18.4620 -29.9 -113.6 3:42 18.5000 -35.8 -154.7 3:46 18.5250 -40.2 -179.2 3:53 18.5490 -44.7 -183.7 3:59 18.5750 -51.4 -261.2 4:08 18.5950 -57.3 -294.0 4:16 18.6150 -64.8 -374.5 4:25 18.6350 -75.2 -521.5 4:35 18.6550 -90.4 -756.0 4:48

EQP1 18.6750 -112.9 -1127.0 5:01 18.6950 -134.5 -1081.5 5:14 18.7150 -151.3 -840.0 5:25




Method: G053 Cont. Ammonium chloride Date: 08-09-1999 11:42


RESULTS


1/1 992224 1.0072 g R1 = 99.70 % NH4Cl

1/2 992224 0.9923 g R1 = 99.46 % NH4Cl

1/3 992224 1.001 g R1 = 99.45 % NH4Cl

1/4 992224 1.0024 g R1 = 99.41 % NH4Cl

1/5 992224 0.9921 g R1 = 99.41 % NH4Cl

1/6 992224 0.9932 g R1 = 99.38 % NH4Cl

STATISTICS


Mean value x = 99.47 % NH4Cl

Standard deviation s = 0.119971 % NH4Cl

Rel.standard deviation srel = 0.121 %

Titration curve

Results

62

Method: G053 Cont. Ammonium chloride Version: 08-09-1999 11:42

Title Method ID . . . . . . . . . . . . . G053 Title . . . . . . . . . . . . . . . Cont. AmmoniumChloride Date/time . . . . . . . . . . . . . 08-Sep-1999 11:02 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.99 Upper limit [g] . . . . . . . . . 1.01 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 53.49 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . NaOH Concentration [mol/L] . . . . . . . 1.0 Sensor . . . . . . . . . . . . . . . DG111-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 17.0 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 5.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.25 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 2.0 t(max) [s] . . . . . . . . . . 20.0 Threshold . . . . . . . . . . . . 500.0 Maximum volume [mL] . . . . . . . 20.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Steepest jump only . . . . . . . Yes Calculation Result name . . . . . . . . . . . . NH4Cl Formula . . . . . . . . . . . . . . R=(Q*C/m)+H20 Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 3 Rinse Auxiliary reagent . . . . . . . . . Water Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Printer+Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer+Computer All results . . . . . . . . . . . . Yes

Method

63

M141

Benzyl Alcohol is a bacteriostatic agent and is used as a preservative. It also has weak local anaestheticproperties and is therefore used as an additive in solutions for intramuscular and subcutaneous injections.

Benzyl AlcoholM = 108.1 g/mol

Acetic anhydride RPyridine RDeionised water

c(NaOH) = 1 mol/L


1. Reaction of benzyl alcohol with aceticanhydride to acetic acid benzyl ester with therelease of pyridinium acetate:

BzOH + CH3CO-O-COCH3 + C5H5N →Bz-O-COCH3 + C5H5NH+OAc-

2. Titration of pyridinium acetate with NaOH:C5H5NH+OAc- + NaOH → C5H5N + NaOAc + H2O


METTLER TOLEDO


Waste disposal

Ph. Eur. 1997; Monograph "BenzylAlcohol"

Sample preparation

Benzyl Alcohol C7H8OSample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG111-SCIndication

Content Determination of Benzyl Alcohol

Weigh a sample of 0.89 to 0.91 g benzyl alcohol,accurately to 0.1 mg, into a 150 mL roundbottomed flask. Add 15.0 mL of a freshly madesolution of 1 part acetic anhydride to 7 partspyridine. An equal volume of this solution isnecessary for a blank determination. Both thesample and the blank must boil for 30 minutes byrefluxing in a waterbath. Finally transfer into 100 mLtitration beakers, rinsing twice with 25 mL deionisedwater.

The titrant consumtion for the blank determination isgreater than for the benzyl alcohol determination,since the pyridinium acetate content is higher.

Remarks

R(%) = (x-Q[2]) • M • /(10 • m)

Q = Titrant consumption in mmolx = Mean value of the blank determination inmmolM = Molar mass Benzyl Alcoholm = Sample size in g

Calculation

Method for the alkalimetric content determination of Benzyl Alcohol


L. Pludra

Author

Structure

64


ET1 0.0000 59.5 0:03 14.2850 35.5 -1.7 1:01 21.4270 16.1 -2.7 1:45

ET2 25.0000 0.0 -4.5 1:56 25.2000 -1.4 -7.0 1:59 25.4000 -2.8 -7.0 2:03 25.6000 -4.1 -6.7 2:07 25.8000 -5.6 -7.4 2:10 26.0000 -7.1 -7.4 2:14

\\ \\ \\ \\ 29.0000 -58.3 -41.6 3:14 29.1560 -67.8 -61.0 3:19 29.2550 -75.9 -82.0 3:24 29.3320 -84.8 -115.5 3:29 29.3850 -93.3 -159.8 3:34 29.4240 -101.5 -210.0 3:39 29.4540 -110.3 -294.0 3:43 29.4750 -118.8 -403.3 3:48 29.4950 -128.9 -507.5 3:52 29.5150 -147.1 -906.5 4:04 29.5350 -173.1 -1301.9 4:16

EQP1 29.5550 -200.8 -1382.6 4:28 29.5750 -218.5 -889.0 4:38 29.5950 -230.9 -616.0 4:44




Method: G057 Cont. Benzyl alcohol Date: 09-12-1999 13:11

User: Salomon Measured: 10-12-1999 10:59

RESULTS


1/1 993230 15.0 mL R1 = 36.854 mmol Blank

1/2 993230 15.0 mL R1 = 36.950 mmol Blank

1/3 993230 15.0 mL R1 = 36.951 mmol Blank

2/1 993230 0.8980 g R2 = 100.62 % C7H8O

2/2 993230 0.8986 g R2 = 100.48 % C7H8O

2/3 993230 0.9027 g R2 = 100.81 % C7H8O

2/4 993230 0.8959 g R2 = 99.88 % C7H8O

2/5 993230 0.9087 g R2 = 100.46 % C7H8O

2/6 993230 0.9083 g R2 = 100.27 % C7H8O

STATISTICS





STATISTICS


Mean value x = 100.42 % C7H8O

Standard deviation s = 0.320334 % C7H8O


Titration curve

Results

65

Method: G057 Cont. Benzyl alcohol Version: 09-12-1999 13:11

Title Method ID . . . . . . . . . . . . . G057 Title . . . . . . . . . . . . . . . Cont. Benzyl alcohol Date/time . . . . . . . . . . . . . 09-Dec-1999 13:11 Sample Number samples . . . . . . . . . . . 2 Titration stand . . . . . . . . . . Stand 1 Entry type . . . . . . . . . . . . . Fixed volume U Volume [mL] . . . . . . . . . . . 15.0 ID1 . . . . . . . . . . . . . . . . Test-Nr. Molar mass M . . . . . . . . . . . . 100.0 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . NaOH Concentration [mol/L] . . . . . . . 1.0 Sensor . . . . . . . . . . . . . . . DG111-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 35.0 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 250.0 Maximum volume [mL] . . . . . . . 50.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Steepest jump only . . . . . . . Yes Calculation Result name . . . . . . . . . . . . Blank det. Formula . . . . . . . . . . . . . . R1=Q Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . mmol Decimal places . . . . . . . . . . . 3 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes

Method Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . Stand 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.89 Upper limit [g] . . . . . . . . . 0.91 ID1 . . . . . . . . . . . . . . . . Test-Nr. Molar mass M . . . . . . . . . . . . 108.1 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . NaOH Concentration [mol/L] . . . . . . . 1.0 Sensor . . . . . . . . . . . . . . . DG111-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 25.0 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 250.0 Maximum volume [mL] . . . . . . . 50.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Steepest jump only . . . . . . . Yes Calculation Result name . . . . . . . . . . . . C7H8O Formula . . . . . . . . . . . . . . R2=(x-Q[2])*C2/m Constant . . . . . . . . . . . . . . C2=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 3 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R2 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer Short-form method . . . . . . . . . Yes All results . . . . . . . . . . . . Yes

66

M142

Carbomer 934 P is a ground component in gels.

Carboxyl groupsM = 45.02 g/mol

Deionised water R

c(NaOH) = 0.5 mol/L


Deprotonation of the carboxyl group


Titration stand

METTLER TOLEDO


Waste disposal

Ph. Eur. 1997, supplement 1999;Monograph "Carbomer"

Sample preparation

Carbomer 934 PSample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG111-SCIndication

Content Determination of Carbomer 934P

Weigh a sample of 0.39 to 0.41 g Carbomer 934P, accurately to 0.1 mg, into a 1000 mL glassbeaker, add 400 mL deionised water and allow thesolution to stir at 1000 rpm with a paddle stirrer.Then reduce the stirring speed to ca. 500 rpm.Lower the burette attached to the stand so that the tipis about 2 cm deep in the solution. Similarly, placethe electrode such that the diaphragm is totallyimmersed in the solution.

The previously determined loss on drying content issaved as the auxilliary value H20.The determination is performed using a separatetitration stand.

Remarks

R(%) = (Q • M/(10 • m)) + H20

Q = Titrant consumption in mmolM = Molar mass Carboxyl groupsm = Sample size in gH20 = % Loss on drying of Carbomer 934P

Calculation

Method for the alkalimetric content determination of the carboxyl groups in the Carbomer 934P


L. Pludra

Author

Structure

67


ET1 0.0000 193.1 0:02 1.1420 124.9 -59.7 0:17 1.7120 103.9 -36.7 0:33

ET2 2.0000 93.5 -36.2 0:47 2.2240 87.4 -27.2 0:57 2.6640 76.5 -24.8 1:10

\\ \\ \\ \\ 9.0760 -72.6 -41.8 5:26 9.2080 -78.5 -45.1 5:36 9.3720 -86.6 -49.1 5:50 9.5220 -92.6 -40.1 6:00 9.7780 -106.7 -55.0 6:17 9.8920 -113.5 -60.2 6:27 10.0140 -123.2 -79.2 6:40 10.0940 -130.0 -84.9 6:51 10.1820 -138.0 -90.7 7:01 10.2640 -147.4 -115.2 7:12 10.3200 -154.8 -131.2 7:22 10.3740 -162.2 -137.4 7:31 10.4280 -170.1 -146.5 7:41

EQP1 10.4800 -177.8 -148.1 7:50 10.5320 -184.7 -133.3 7:59 10.5980 -193.3 -129.4 8:09 10.6600 -199.8 -106.1 8:16 10.7560 -208.9 -94.1 8:24

\\ \\ \\ \\


METTLER DL70ES Titrator V3.1 Dr. Kade Pharm. Fabrik GmbH

Onkel Tuka DL70 Quality Control Laboratory

Method: G039 Cont. Carbomer 934P Date: 17-12-1999 9:45


RESULTS


1/1 993331 0.3921 g R1 = 60.84 % COOH

1/2 993331 0.3975 g R1 = 60.47 % COOH

1/3 993331 0.3963 g R1 = 59.64 % COOH

1/4 993331 0.3987 g R1 = 61.71 % COOH

1/5 993331 0.4035 g R1 = 61.03 % COOH

1/6 993331 0.4304 g R1 = 57.75 % COOH

STATISTICS


Mean value x = 60.24 % COOH

Standard deviation s = 1.394574 % COOH


Titration curve

Results

68

Method: G039 Gehalt Carbomer 934P Version: 17-12-1999 9:45

Title Method ID . . . . . . . . . . . . . G039 Title . . . . . . . . . . . . . . . Cont. Carbomer 934P Date/time . . . . . . . . . . . . . 17-Dec-1999 9:45 Sample Number samples . . . . . . . . . . . 6 Titration stand . . . . . . . . . . Free stand Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.39 Upper limit [g] . . . . . . . . . 0.41 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 45.02 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Titration Titrant . . . . . . . . . . . . . . NaOH Concentration [mol/L] . . . . . . . 0.5 Sensor . . . . . . . . . . . . . . . DG111-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 2.0 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Relative dV(min) [%dosVol] . . . . . 0.5 dV(max) [%buVol] . . . . . 5.0 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 2.0 t(max) [s] . . . . . . . . . . 20.0 Threshold . . . . . . . . . . . . 10.0 Maximum volume [mL] . . . . . . . 40.0 Termination at potential . . . . Yes Potential . . . . . . . . . . -271.91 Evaluation procedure . . . . . . Standard Steepest jump only . . . . . . . Yes Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . COOH Formula . . . . . . . . . . . . . . R=(Q*C/m)+H20 Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes

Method

69

M143

Cinchocain, known in the United States as Dibucain, is a strong acting local anaesthetic of the amino acidtype.

Cinchocain HydrochlorideM = 379.9 g/mol

Ethanol 96% R0.1 M Hydrochloric acid



Deprotonation of the aminohydrochloride

[R-NH(Et)2]+Cl- + NaOH →

R-N(Et)2 + H2O + NaCl


METTLER TOLEDO


Waste disposal

Monographieentwurf "CinchocainiHydrochloridum" der PharmeuropaVol. 7, Nr. 1, März 1995(German)

Sample preparation

Cinchocain Hydrochloride C20H30ClN3O2Sample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG111-SCIndication

Content Determination of Cinchocain Hydrochloride

Weigh a sample of 0.29 to 0.31 g CinchocainHydrochloride, accurately to 0.1 mg, into a 100 mLtitration beaker and dissolve with 50 mL ethanol96%.

The previously determined loss on drying content issaved as the auxilliary value H20.0.1M HCl is added so as to bind any existing freeCinchocain. The titration curve therefore shows twoequivalence points, the first from the neutralisation ofexcess HCl and the second from the hydrochloride.The content is calculated from the difference betweenthe first and second equivalence points.

Remarks

R(%) = (Q[2] • M/(10 • m)) + H20

Q[2] = Titrant consumption between the first andsecond equivalence point in mmolM = Molar mass Cinchocain Hydrochloridem = Sample size in gH20 = % Loss on drying of Cinchocain-HCl

Calculation

Method for the alkalimetric content determination of Cinchocain Hydrochloride


L. Pludra

Author

Structure

70


ET1 0.0000 249.1 0:03 0.5710 235.5 -23.9 0:13 0.8560 224.7 -37.8 0:22

ET2 1.0000 217.4 -50.6 0:30 1.1260 209.0 -66.7 0:39 1.2220 201.8 -75.1 0:48 1.3170 190.3 -121.6 0:59 1.3640 182.3 -168.3 1:09 1.4010 173.8 -230.8 1:20 1.4280 166.0 -290.4 1:30 1.4500 156.8 -416.8 1:43 1.4700 145.9 -542.5 1:58

EQP1 1.4900 130.2 -787.5 2:19 1.5100 115.6 -731.5 2:39 1.5300 103.5 -602.0 2:56 1.5500 93.4 -504.0 3:11 1.5700 86.3 -357.0 3:23 1.6080 75.9 -272.6 3:37

\\ \\ \\ \\ 8.9540 -156.6 -158.4 9:18 8.9950 -168.3 -285.1 9:34 9.0150 -173.7 -269.5 9:44 9.0460 -189.3 -505.8 10:06 9.0660 -212.1 -1137.5 10:37

EQP2 9.0860 -235.9 -1190.0 11:07 9.1060 -255.6 -983.5 11:34 9.1260 -268.4 -644.0 11:52




Method: G020 Cont. Cinchocain-HCl Date: 19-11-1999 10:55


RESULTS


1/1 941817 0.2925 g R1 = 100.44 % C20H30ClN3O2

1/2 941817 0.3058 g R1 = 100.41 % C20H30ClN3O2

1/3 941817 0.2911 g R1 = 100.71 % C20H30ClN3O2

1/4 941817 0.2937 g R1 = 100.70 % C20H30ClN3O2

1/5 941817 0.2978 g R1 = 100.43 % C20H30ClN3O2

1/6 941817 0.2937 g R1 = 100.62 % C20H30ClN3O2

STATISTICS


Mean value x = 100.55 % C20H30ClN3O2

Standard deviation s = 0.142034 % C20H30ClN3O2


Titration curve

Results

71

Method: G020 Cont. Cinchocain-HCl Version: 19-11-1999 10:55

Title Method ID . . . . . . . . . . . . . G020 Title . . . . . . . . . . . . . . . Cont. Cinchocain-HCl Date/time . . . . . . . . . . . . . 19-Nov-1999 10:55 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.29 Upper limit [g] . . . . . . . . . 0.31 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 379.9 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . NaOH Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG111-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 1 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 250.0 Maximum volume [mL] . . . . . . . 15.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 2 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . C20H30ClN3O2 Formula . . . . . . . . . . . . . . R=(Q2*C/m)+H20 Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Rinse Auxiliary reagent . . . . . . . . . Water Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes

Method

72

M144

Citric Acid is generally used together with sodium and calcium citrate salts as a rinse for dry oral mucousmembranes, to alkalise the urine and to dissolve bladder stones. As an auxiliary reagent, it improves theefficacy of anti-oxidants and is used in the production of effervescent tablets and powders.

Citric Acid MonohydrateM = 192.1 g/mol

Deionised water R

c(NaOH) = 1.0 mol/L


Deprotonation of the carboxylgroups

R-(COOH)3 + 3 NaOH →R-(COONa)3 + 3H2O


METTLER TOLEDO


Waste disposal

Ph. Eur. 1997; Monograph"Citric Acid Monohydrate"

Sample preparation

Citric Acid C6H8O7Sample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG111-SCIndication

Content Determination of Citric Acid Monohydrate

Weigh a sample of 0.54 to 0.56 g citric acidmonohydrate, accurately to 0.1 mg, into a 100 mLtitration beaker and dissolve in 40 mL deionisedwater.


Remarks

R(%) = (Q • M/(10 •3•m)) + H20

Q = Titrant consumption in mmolM = Molar mass Citric Acidm = Sample size in gH20 = % Loss on drying of Citric Acid3 = Equivalent number

Calculation

Method for the alkalimetric content determination of Citric Acid


L. Pludra

Author

Structure

73


ET1 0.0000 241.8 0:03 4.4260 103.5 -31.2 0:20 6.6390 41.6 -28.0 0:33

ET2 7.7460 -9.7 -46.3 0:45 7.8690 -26.1 -133.7 0:54 7.9050 -33.5 -206.1 1:01 7.9330 -40.7 -257.5 1:08 7.9580 -48.8 -322.0 1:15 7.9780 -57.5 -437.5 1:22 7.9980 -72.9 -770.0 1:33 8.0180 -114.9 -2100.0 1:58

EQP1 8.0380 -199.9 -4248.8 2:20 8.0580 -232.7 -1638.0 2:31 8.0780 -251.7 -952.0 2:41




Method: G059 Cont. Citric acid Date: 22-12-1999 9:40


RESULTS


1/1 972536 0.5553 g R1 = 100.76 % C6H8O7

1/2 972536 0.5513 g R1 = 100.58 % C6H8O7

1/3 972536 0.548 g R1 = 100.63 % C6H8O7

1/4 972536 0.5540 g R1 = 100.44 % C6H8O7

1/5 972536 0.5487 g R1 = 100.47 % C6H8O7

1/6 972536 0.5485 g R1 = 100.31 % C6H8O7

STATISTICS





Titration curve

Results

74

Method: G059 Cont. Citric acid Version: 22-12-1999 9:40

Title Method ID . . . . . . . . . . . . . G059 Title . . . . . . . . . . . . . . . Cont. Citric acid Date/time . . . . . . . . . . . . . 22-Dec-1999 9:40 Sample Number samples . . . . . . . . . . . 6 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.54 Upper limit [g] . . . . . . . . . 0.56 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 192.1 Equivalent number z . . . . . . . . 3 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 30 Titration Titrant . . . . . . . . . . . . . . NaOH Concentration [mol/L] . . . . . . . 1.0 Sensor . . . . . . . . . . . . . . . DG111-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . % nom. content Metered amount [%] . . . . . . 90.0 Nominal content . . . . . . . 100.0 Conversion const. . . . . . . M/(10*z) Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 250.0 Maximum volume [mL] . . . . . . . 15.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Steepest jump only . . . . . . . Yes Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . C6H8O7 Formula . . . . . . . . . . . . . . R=(Q*C/m)+H20 Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Rinse Auxiliary reagent . . . . . . . . . Water Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes

Method

75

M145

Potassium dihydrogen phosphate is a saline laxative, which is used to treat hyperpotassaemia from poor ormalnourishment, or cases of high loss of potassium from vomiting or diarrhoea.

Potassium dihydrogen phosphateM = 136.1 g/mol

Deionised water R

c(NaOH) = 0.5 mol/l


Deprotonation of the dihydrogenphosphate anions to monohydrogenphosphate

H2PO4- + OH- → HPO4

2- + H2O


METTLER TOLEDO


Waste disposal

Ph. Eur. 1997; Monograph"Potassium dihydrogen phosphate"

Sample preparation

Potassium dihydrogen phosphateSample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG111-SCIndication

Content Determination of Potassium Dihydrogen Phosphate

Weigh a sample of 0.24 to 0.28 g potassiumdihydrogen phosphate, accurately to 0.1 mg, into a100 mL titration beaker and dissolve in 40 mLdeionised water.


Remarks

R(%) = (Q • M/(10 •m)) + H20

Q = Titrant consumption in mmolM = Molar mass K-dihydrogen phosphatem = Sample size in gH20 = % Loss on drying of KH2PO4

Calculation

Method for the alkalimetric content determination of Potassium Dihydrogen Phosphate


L. Pludra

Author

Structure

76


ET1 0.0000 108.1 0:02 9.9820 -25.7 -13.4 0:27 14.9730 -54.5 -5.8 1:10

ET2 17.4700 -78.7 -9.7 1:21 17.9700 -86.8 -16.1 1:28 18.3250 -94.3 -21.1 1:35 18.6310 -102.5 -27.0 1:42 18.8740 -111.4 -36.3 1:49 19.0490 -120.2 -50.4 1:56 19.1730 -128.5 -67.2 2:03 19.2680 -137.0 -89.2 2:11 19.3390 -145.5 -119.3 2:20 19.3920 -153.2 -145.3 2:28 19.4380 -160.2 -152.2 2:36

EQP1 19.4880 -168.8 -173.6 2:43 19.5290 -175.8 -170.7 2:51 19.5760 -183.2 -156.4 2:58 19.6320 -190.9 -137.5 3:06 19.6990 -198.0 -105.5 3:13 19.8070 -206.9 -83.0 3:20 19.9390 -215.2 -63.1 3:27 20.0000 -218.4 -51.6 3:33




Method: G056 Cont. KH2PO4 Date: 14-12-1999 13:40


RESULTS


1/1 992222 0.2564 g R1 = 100.403 % KH2PO4

1/2 992222 0.2453 g R1 = 100.270 % KH2PO4

1/3 992222 0.2443 g R1 = 100.278 % KH2PO4

1/4 992222 0.2581 g R1 = 100.294 % KH2PO4

1/5 992222 0.2471 g R1 = 100.243 % KH2PO4

1/6 992222 0.2553 g R1 = 100.171 % KH2PO4

STATISTICS


Mean value x = 100.276 % KH2PO4

Standard deviation s = 0.075597 % KH2PO4


Titration curve

Results

77

Method: G056 Cont. KH2PO4 Version: 14-12-1999 13:40

Title Method ID . . . . . . . . . . . . . G056 Title . . . . . . . . . . . . . . . Cont. KH2PO4 Date/time . . . . . . . . . . . . . 14-Dec-1999 13:29 Sample Number samples . . . . . . . . . . . 6 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.24 Upper limit [g] . . . . . . . . . 0.26 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 136.1 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . NaOH Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG111-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . % nom. content Metered amount [%] . . . . . . 90.0 Nominal content . . . . . . . 100.0 Conversion const. . . . . . . M/(10*z) Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.5 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 2.0 t(max) [s] . . . . . . . . . . 20.0 Threshold . . . . . . . . . . . . 50.0 Maximum volume [mL] . . . . . . . 20.0 Evaluation procedure . . . . . . Standard Steepest jump only . . . . . . . Yes Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . KH2PO4 Formula . . . . . . . . . . . . . . R=(Q*C/m)+H20 Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 3 Rinse Auxiliary reagent . . . . . . . . . Water Volume [mL] . . . . . . . . . . . . 30.0 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer Short-form method . . . . . . . . . Yes All results . . . . . . . . . . . . Yes

Method

78

M146

Sodium monohydrogen phosphate is a saline laxative which is used for emptying the bowels, alkalisingurine, hypercalcaemia and in cases of hypophosphataemia.

Na-monohydrogen phosphateM = 142.0 g/mol

Deionised water R


METTLER TOLEDO DL70ES/DL77

1. Protonation of the monohydrogen phosphate tophosphoric acid through hydrochloric acid

HPO42- + 2H3O

+ → H3PO4 + 2H2O

2. Neutralisation of the excess hydrochloric acid as wellas deprotonation to secondary phosphate in the firstequivalence point

H3PO4 + OH- → H2PO4- + H2O

3. Deprotonation to primary phosphate in the secondequivalence point

H2PO4- + OH- → HPO4

2-


METTLER TOLEDO


Waste disposal

Ph. Eur. 1997; Monograph "SodiumMonohydrogen Phosphate"

Sample preparation

Na-monohydrogen phosphateSample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG111-SCIndication

Content Determination of Sodium Monohydrogen Phosphate

Weigh a sample of 0.24 to 0.28 g sodiummonohydrogen phosphate, accurately to 0.1 mg,into a 100 mL titration beaker and dissolve in 40mL deionised water.

The previously determined loss on drying content issaved as the auxilliary value H20.The curve of the back titration shows twoequivalence points so that the content of sodiummonohydrogen phosphate as well as sodiumdihydrogen phosphate can be determined on aparallel basis.

Remarks

R(%) = (QDISP-Q) • M • F/(10 • m)

QDISP= Total amount of dispensed HCl in mmolQ = Titrant consumption in mmolF = 100/(100-H20) Formula for the loss ondrying of Na2HPO4

M = Molar mass Na2HPO4

m = Sample size in g

Calculation

Method for the alkalimetric content determination of Sodium Monohydrogen Phosphate


L. Pludra

Author

Structure

79


ET1 0.0000 320.3 0:03 5.7140 301.0 -3.4 0:13 8.5700 285.5 -5.4 0:20

ET2 10.0000 275.7 -6.9 0:26 10.2000 273.8 -9.5 0:29 10.4000 272.1 -8.8 0:33 10.6000 270.4 -8.4 0:36 10.8000 268.5 -9.5 0:40 11.0000 267.0 -7.4 0:44

\\ \\ \\ \\ 14.5440 173.9 -148.1 2:10 14.5880 165.2 -198.9 2:19 14.6200 158.0 -225.3 2:25 14.6500 150.7 -242.7 2:31

EQP1 14.6800 142.3 -280.0 2:38 14.7040 136.8 -227.5 2:45 14.7480 128.5 -189.3 2:51 14.8000 119.5 -173.7 2:59

\\ \\ \\ \\ 24.4040 -62.4 -44.8 6:53 24.5400 -68.9 -48.4 6:57 24.6920 -80.1 -73.2 7:02 24.7720 -87.1 -87.5 7:08 24.8500 -96.9 -126.5 7:14 24.8980 -105.1 -170.6 7:20 24.9340 -112.1 -192.5 7:26 24.9700 -119.8 -213.9 7:33

EQP2 25.0040 -127.9 -238.8 7:39 25.0340 -134.9 -233.3 7:45 25.0680 -142.2 -216.2 7:52




Method: G031 Cont. Na2HPO4 Date: 14-12-1999 13:20


RESULTS


1/1 992223 0.9178 g R1 = 100.38 % Na2HPO4

1/2 992223 0.9477 g R1 = 99.96 % Na2HPO4

1/3 992223 1.0699 g R1 = 99.72 % Na2HPO4

1/4 992223 1.0368 g R1 = 99.87 % Na2HPO4

1/5 992223 1.0046 g R1 = 100.05 % Na2HPO4

1/6 992223 0.9735 g R1 = 99.76 % Na2HPO4

R3 = 19.00 % Drying loss

STATISTICS


Mean value x = 99.96 % Na2HPO4

Standard deviation s = 0.238792 % Na2HPO4


Titration curve

Results

80

Method: G031 Cont. Na2HPO4 Version: 14-12-1999 13:20

Title Method ID . . . . . . . . . . . . . G031 Title . . . . . . . . . . . . . . . Cont. Na2HPO4 Date/time . . . . . . . . . . . . . 14-Dec-1999 13:20 Sample Number samples . . . . . . . . . . . 6 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.9 Upper limit [g] . . . . . . . . . 1.1 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 100.0 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Dispense Titrant . . . . . . . . . . . . . . HCl Concentration [mol/L] . . . . . . . 0.5 Volume [mL] . . . . . . . . . . . . 25 Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . NaOH Concentration [mol/L] . . . . . . . 0.5 Sensor . . . . . . . . . . . . . . . DG111-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 10 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 100.0 Maximum volume [mL] . . . . . . . 30.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 2 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq<2 Calculation Result name . . . . . . . . . . . . Na2HPO4 Formula . . . . . . . . . . . . . . R1=1420*(QDISP-Q1)/C Constant . . . . . . . . . . . . . . C=m*(100-H20) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Calculation Result name . . . . . . . . . . . . NaH2PO4 Formula . . . . . . . . . . . . . . R2=(Q1+Q2-QDISP)/C2 Constant . . . . . . . . . . . . . . C2=(QDISP-Q1)/100 Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Condition . . . . . . . . . . . . . Yes Condition . . . . . . . . . . . . Q1+Q2>QDISP Rinse Auxiliary reagent . . . . . . . . . Water Volume [mL] . . . . . . . . . . . . 30.0 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R2 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Calculation Result name . . . . . . . . . . . . Loss on drying Formula . . . . . . . . . . . . . . R3=H20 Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes

Method

81

M147

Norethisterone acetate, a synthetic progestational hormone, is a contraceptive also used to treatendometriosis.

Norethisterone AcetateM = 340.5 g/mol

Silver nitrate solution 10%Tetrahydrofuran R

c(NaOH) = 0.1 mol/L


Precipitation of acetylide with silvernitrate by release of a stoichiometricquantity of protons, which aretitrated with a sodium hydroxidesolution.

R-C≡CH + Ag+ → R-C≡CAg + H+


METTLER TOLEDO


Waste disposal

Ph. Eur. 1997, Supplement 1999;Monograph " Norethisterone Acetate"

Sample preparation

Norethisterone Acetate, C22H28O3Sample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG113-SCIndication

Content Determination of Norethisterone Acetate

Weigh a sample of 0.10 to 0.12 g NorethisteroneAcetate, accurately to 0.1 mg, into a 100 mLtitration beaker and dissolve in 40 mLtetrahydrofuran. Then add 10 mL silver nitratesolution 10%.

Remarks

R(%) = Q • M/(10 •m)

Q = Titrant consumption in mmolM = Molar mass Norethisterone Acetatem = Sample size in g

Calculation

Method for the alkalimetric content determination of Norethisterone Acetate in a non-aqueous medium


L. Pludra

Author

Structure

82


ET1 0.0000 127.6 0:10 1.1420 121.0 -5.8 0:16 1.7130 114.9 -10.5 0:22

ET2 2.0000 111.0 -13.7 0:27 2.2000 106.9 -20.7 0:32 2.4000 101.6 -26.6 0:38 2.6000 92.7 -44.4 0:44 2.7280 84.5 -64.0 0:50 2.8230 74.8 -101.7 0:57 2.8800 65.9 -157.2 1:04 2.9170 57.3 -232.7 1:11 2.9420 49.3 -319.2 1:18 2.9620 39.8 -472.5 1:27 2.9820 22.5 -868.0 1:38

EQP1 3.0020 -6.9 -1466.5 1:57 3.0220 -32.0 -1256.5 2:21 3.0420 -39.1 -353.5 2:34 3.0620 -41.0 -98.0 2:39

\\ \\ \\ \\




Method: G041 Cont. Norethisterone acet. Date: 09-11-1999 10:30


RESULTS


1/1 990456 0.1034 g R1 = 98.61 % C22H28O3

1/2 990456 0.1016 g R1 = 98.83 % C22H28O3

1/3 990456 0.1005 g R1 = 98.76 % C22H28O3

1/4 990456 0.1022 g R1 = 98.61 % C22H28O3

1/5 990456 0.1044 g R1 = 98.53 % C22H28O3

1/6 990456 0.1029 g R1 = 98.54 % C22H28O3

STATISTICS





Titration curve

Results

83

Method: G041 Cont. Norethisterone acet. Version: 09-11-1999 10:30

Title Method ID . . . . . . . . . . . . . G041 Title . . . . . . . . . . . . . . Cont. Norethisteroneacet. Date/time . . . . . . . . . . . . . 09-Nov-1999 10:30 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.1 Upper limit [g] . . . . . . . . . 0.12 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 340.5 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . NaOH Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG113-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 2 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 700.0 Maximum volume [mL] . . . . . . . 4.0 Evaluation procedure . . . . . . Standard Steepest jump only . . . . . . . Yes Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . C22H28O3 Formula . . . . . . . . . . . . . . R=Q*C/m Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Rinse Auxiliary reagent . . . . . . . . . Water Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes

Method

84

M148

Oxybutynine Hydrochloride is used to treat hyperfunction of the bladder.

Oxybutynine HydrochlorideM = 393.96 g/mol

Ethanol 96% R0.1M Hydrochloric acid



Deprotonation of the aminohydrochloride

[R-NH(Et)2]+Cl- + NaOH →

R-N(Et)2 + H2O + NaCl


METTLER TOLEDO


Waste disposal

Ph. Eur. 1997, Supplement 1999;Monograph "OxybutynineHydrochloride"

Sample preparation

Oxybutynine Hydrochloride,Sample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG111-SCIndication

Content Determination of Oxybutynine Hydrochloride

Weigh a sample of 0.29 to 0.31 g OxybutynineHydrochloride, accurately to 0.1 mg, into a 100 mLtitration beaker and dissolve in 50 mL ethanol 96%.

The previously determined loss on drying content is savedas the auxilliary value H20. To detect the existing freeoxybutynin in the titration, 0.1M hydrochloric acid isadded. As a result, the titration curve shows twoequivalence points, the first from the addition of excesshydrochloric acid and the second from the hydrochloride.The content is calculated from the volume differencebetween the two equivalence points.

Remarks

R(%) = (Q[2] • M/(10 • m)) + H20

Q[2] = Titrant consumption between the first andsecond equivalence point in mmolM = Molar mass Oxybutynine Hydrochloridem = Sample size in gH20 = % Loss on drying of Oxybutynine-HCl

Calculation

Method for the alkalimetric content determination of Oxybutynine Hydrochloride

Standard Potassium hydrogen phthalate(M521), THAM (522)

L. Pludra

Author

Structure

85


ET1 0.0000 248.3 0:09 ET2 0.0000 248.6 0:10

0.0200 249.3 31.5 0:14 0.0400 249.2 -3.5 0:17 0.0800 248.4 -21.0 0:20 0.1600 243.2 -64.7 0:29 0.2520 234.5 -94.3 0:40 0.3320 225.2 -116.4 0:53 0.4040 215.0 -141.9 1:08 0.4630 203.5 -194.6 1:24 0.5030 194.9 -213.5 1:38

EQP1 0.5460 185.5 -219.8 1:53 0.5900 177.3 -186.1 2:07 0.6550 166.2 -170.2 2:22 0.7190 157.6 -135.6 2:35 0.8170 148.1 -96.4 2:49 0.9910 134.9 -76.0 3:05

\\ \\ \\ \\ 8.0210 -49.6 -87.3 6:37 8.1170 -62.3 -132.0 6:52 8.1730 -72.4 -180.0 7:06 8.2160 -97.0 -573.0 7:37 8.2360 -119.3 -1116.5 8:06 8.2560 -145.7 -1316.0 8:37

EQP2 8.2760 -173.3 -1382.4 9:07 8.2960 -200.3 -1351.0 9:38 8.3160 -226.0 -1284.4 10:08




Method: G078 Cont. Oxybutynine-HCl Date: 09-11-1999 11:42


RESULTS


1/1 992625 0.3061 g R1 = 100.87 % C22H31NO3*HCl

1/2 992625 0.2982 g R1 = 100.82 % C22H31NO3*HCl

1/3 992625 0.3111 g R1 = 100.65 % C22H31NO3*HCl

1/4 992625 0.306 g R1 = 100.79 % C22H31NO3*HCl

1/5 992625 0.305 g R1 = 100.78 % C22H31NO3*HCl

1/6 992625 0.3003 g R1 = 100.96 % C22H31NO3*HCl

STATISTICS


Mean value x = 100.81 % C22H31NO3*HCl

Standard deviation s = 0.104192 % C22H31NO3*HCl


Titration curve

Results

86

Method: G078 Cont. Oxybutynine-HCl Version: 09-11-1999 11:42

Title Method ID . . . . . . . . . . . . . G078 Title . . . . . . . . . . . . . . . Cont. Oxybutynine-HCl Date/time . . . . . . . . . . . . . 09-Nov-1999 11:42 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.29 Upper limit [g] . . . . . . . . . 0.31 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 393.96 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 65 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . NaOH Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG111-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 0 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 10.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.5 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 50.0 Maximum volume [mL] . . . . . . . 15.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 2 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . C22H31NO3*HCl Formula . . . . . . . . . . . . . . R1=(Q2*C/m)+H20 Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Rinse Auxiliary reagent . . . . . . . . . Water Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes

Method

87

M149

Phenoxyethanol is an antibacterial preservative which is used in semi-solid preparations and cosmetics.

PhenoxyethanolM = 138.2 g/mol

1-Butanol RDeionised water RAnhydrous pyridine RAcetylation mixture R1(25,0 mL acetic anhydride R in100,0 mL anhydrous pyridine)

c(NaOH) = 1 mol/L


1. Conversion of phenoxyethanol with aceticanhydride to acetic acid phenoxyethyl acid by theformation of pyridinium acetate

PhenOH + CH3CO-O-COCH3 + C5H5N →Phen-O-COCH3 + C5H5NH+OAc-

2. Titration of pyridinium acetate with NaOHC5H5NH+OAc- + NaOH → C5H5N + NaOAc + H2O


METTLER TOLEDO


Waste disposal

Ph. Eur. 1997; Monograph"Phenoxyethanol"

Sample preparation

Phenoxyethanol, C8H10O2Sample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG111-SCIndication

Content Determination of Phenoxyethanol

Weigh a sample of 1.90 to 2.10 g Phenoxyethanol,accurately to 0.1 mg, into a 150 mL acetylationflask. Add 10 mL freshly prepared acetylationmixture to the sample-containing flask as well as totwo additional empty flasks to be used for the blankdetermination. Attach to the reflux condenser. Stir for45 min while heating in a boiling waterbath.Transfer into a 100 mL titration beaker. Rinse theflask out with 4 times 5 mL deionised water and addto the beaker. Add 10 mL 1-butanol and heat forapproximately 2 minutes in the waterbath.

Remarks

R(%) = (x-Q[2]) • M • /(10 • m)

Q = Titrant consumption in mmolx = Mean value of the blank determination inmmolM = Molar mass of Phenoxyethanolm = Sample size in g

Calculation

Method for the alkalimetric content determination of Phenoxyethanol


L. Pludra

Author

Structure

88


ET1 0.0000 105.6 0:03 7.0030 95.8 -1.4 0:20 10.5040 91.0 -1.4 0:57

ET2 12.2560 88.3 -1.6 1:04 12.4560 87.9 -1.8 1:08 12.6560 87.7 -1.1 1:11 12.8560 87.4 -1.8 1:15

\\ \\ \\ \\ 35.6560 11.1 -13.3 9:18 35.8560 8.6 -12.6 9:22 36.0560 5.5 -15.8 9:26 36.2560 2.5 -15.1 9:29 36.4560 -2.0 -22.0 9:33 36.6560 -5.9 -19.6 9:37 36.8560 -11.6 -28.3 9:43 37.0560 -18.4 -34.3 9:47 37.2540 -27.5 -46.0 9:51 37.3920 -36.0 -61.4 9:56 37.4960 -45.2 -88.8 10:00 37.5640 -54.2 -131.8 10:04 37.6090 -60.7 -144.7 10:10 37.6590 -72.2 -231.0 10:17 37.6840 -80.8 -344.4 10:23 37.7040 -88.3 -371.0 10:29 37.7240 -100.4 -605.5 10:38 37.7440 -117.6 -861.0 10:49

EQP1 37.7640 -142.0 -1217.9 11:05 37.7840 -162.3 -1015.0 11:18 37.8040 -182.1 -994.0 11:30




Method: G062 Cont. Phenoxyethanol Date: 25-10-1999 12:04


RESULTS


1/1 992617 10.0 mL R1 = 52.365 mmol Blank

1/2 992617 10.0 mL R1 = 52.501 mmol Blank

2/1 992617 2.0078 g R2 = 98.986 % C8H10O2

2/2 992617 2.0440 g R2 = 99.310 % C8H10O2

2/3 992617 2.0463 g R2 = 100.735 % C8H10O2

STATISTICS





STATISTICS





Titration curve

Results

89

Method: G062 Cont. Phenoxyethanol Version: 25-10-1999 12:04

Title Method ID . . . . . . . . . . . . . G062 Title . . . . . . . . . . . . . . . Cont. Phenoxyethanol Date/time . . . . . . . . . . . . . 25-Oct-1999 12:04 Sample Number samples . . . . . . . . . . . 2 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Fixed volume U Volume [mL] . . . . . . . . . . . 10.0 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 100.0 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . NaOH Concentration [mol/L] . . . . . . . 1.0 Sensor . . . . . . . . . . . . . . . DG111-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 45.0 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 100.0 Maximum volume [mL] . . . . . . . 55.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Rinse Auxiliary reagent . . . . . . . . . H2O Volume [mL] . . . . . . . . . . . . 20.0 Calculation Result name . . . . . . . . . . . . Blank Formula . . . . . . . . . . . . . . R1=Q Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . mmol Decimal places . . . . . . . . . . . 3 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes

Method Sample Number samples . . . . . . . . . . . 4 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 1.9 Upper limit [g] . . . . . . . . . 2.1 ID1 . . . . . . . . . . . . . . . . Test-Nr. Molar mass M . . . . . . . . . . . . 138.2 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . NaOH Concentration [mol/L] . . . . . . . 1.0 Sensor . . . . . . . . . . . . . . . DG111-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . % nom. content Metered amount [%] . . . . . . 85.0 Nominal content . . . . . . . 100.0 Conversion const. . . . . . . M/(10*z) Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 250.0 Maximum volume [mL] . . . . . . . 45.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Steepest jump only . . . . . . . Yes Rinse Auxiliary reagent . . . . . . . . . H2O Volume [mL] . . . . . . . . . . . . 20.0 Calculation Result name . . . . . . . . . . . . C8H10O2 Formula . . . . . . . . . . . . . . R2=(x-Q[2])*C/m Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 3 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R2 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer+Computer Short-form method . . . . . . . . . Yes All results . . . . . . . . . . . . Yes

90

M150

Triethanolamine is an oil-in-water emulsifier.

TriethanolamineM = 149.2 g/mol

Deionised water R

c(HCl) = 0.1 mol/L


Protonation of the tertiary aminewith hydrochloric acid

R3N + HCl → R3NH+Cl-


METTLER TOLEDO


Waste disposal

Ph. Helv. 8 - 1997; Monographie"Triethanolamin"(German)

Sample preparation

Triethanolamine, C6H15NO3Sample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG111-SCIndication

Content Determination of Triethanolamine

Weigh a sample of 0.18 to 0.22 g Triethanolamine,accurately to 0.1 mg, in a 100 mL titration beakerand dissolve in 40 mL deionised water.


Remarks

R(%) = (Q • M/(10 •m)) + H20

Q = Titrant consumption in mmolM = Molar mass Triethanolaminem = Sample size in gH20 = % Loss on drying of Triethanolamine

Calculation

Method for the acidimetric content determination of Triethanolamine


L. Pludra

Author

Structure

91


ET1 0.0000 -217.9 0:02 7.1825 -81.1 19.0 1:02 10.7735 -51.0 8.4 1:48

ET2 12.5700 -25.3 14.3 2:01 12.9640 -15.1 25.8 2:09 13.1790 -7.5 35.5 2:16 13.3555 0.3 44.0 2:22 13.5075 9.9 63.6 2:29 13.6035 18.2 86.0 2:36 13.6770 26.5 113.3 2:43 13.7335 35.9 166.0 2:51 13.7700 44.2 226.3 2:59 13.7975 52.4 297.8 3:07 13.8190 61.6 429.8 3:16 13.8390 74.1 623.0 3:27 13.8590 91.4 868.0 3:38

EQP1 13.8790 113.0 1078.0 3:50 13.8990 128.3 766.5 3:58 13.9190 139.4 556.5 4:06




Method: G083 Cont. Triethanolamine Date: 14-12-1999 14:46


RESULTS


1/1 993229 0.2081 g R1 = 99.28 % C6H15NO3

1/2 993229 0.1914 g R1 = 99.13 % C6H15NO3

1/3 993229 0.1975 g R1 = 99.30 % C6H15NO3

1/4 993229 0.2189 g R1 = 99.24 % C6H15NO3

1/5 993229 0.2092 g R1 = 99.14 % C6H15NO3

1/6 993229 0.1898 g R1 = 99.04 % C6H15NO3

STATISTICS


Mean value x = 99.19 % C6H15NO3

Standard deviation s = 0.100611 % C6H15NO3


Titration curve

Results

92

Method: G083 Cont. Triethanolamine Version: 14-12-1999 14:46

Title Method ID . . . . . . . . . . . . . G083 Title . . . . . . . . . . . . . . . Cont. Triethanolamine Date/time . . . . . . . . . . . . . 14-Apr-2000 15:06 Sample Number samples . . . . . . . . . . . 6 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.18 Upper limit [g] . . . . . . . . . 0.22 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 149.2 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . NaOH Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG111-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . % nom. content Metered amount [%] . . . . . . 90.0 Nominal content . . . . . . . 100.0 Conversion const. . . . . . . M/(10*z) Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.5 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 2.0 t(max) [s] . . . . . . . . . . 20.0 Threshold . . . . . . . . . . . . 50.0 Maximum volume [mL] . . . . . . . 20.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=1 Calculation Result name . . . . . . . . . . . . C6H15NO3 Formula . . . . . . . . . . . . . . R=(Q*C/m)+H20 Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Rinse Auxiliary reagent . . . . . . . . . Water Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Computer All results . . . . . . . . . . . . Yes

Method

93

M160

Vanillin is used as a flavouring substance in liquid and solid pharmaceutical preparations.

VanillinM = 152.1 g/mol

Deionised water REthanol 96% R

c(NaOH) = 0.1 mol/L


Deprotonation of the alcohol groups

R-OH + NaOH → R-ONa + H2O


METTLER TOLEDO


Waste disposal

Ph. Eur. 1997; Monograph "Vanillin"

Sample preparation

Vanillin, C8H8O3Sample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG111-SCIndication

Content Determination of Vanillin

Weigh a sample of 0.11 to 0.13 g Vanillin,accurately to 0.1 mg, in a 100 mL titration beaker.Dissolve in 10 mL ethanol R and then add 30 mLdeionised water.


Remarks

R(%) = (Q • M/(10 •m)) + H20

Q = Titrant consumption in mmolM = Molar mass Vanillinm = Sample size in gH20 = % Loss on drying of Vanillin

Calculation

Method for the alkalimetric content determination of Vanillin


L. Pludra

Author

Structure

94


ET1 0.0000 74.8 0:03 4.1850 -103.7 -42.7 0:20 6.2770 -130.8 -12.9 0:31

ET2 7.3240 -154.8 -22.9 0:43 7.5240 -162.9 -40.6 0:51 7.6610 -169.7 -50.1 0:58 7.7950 -178.6 -66.3 1:06 7.8910 -187.2 -89.7 1:15 7.9610 -196.0 -125.0 1:23 8.0100 -204.0 -162.9 1:31 8.0490 -212.4 -215.4 1:40 8.0780 -220.7 -287.2 1:50 8.1000 -227.1 -292.7 1:58

EQP1 8.1260 -237.0 -379.6 2:07 8.1460 -244.2 -357.0 2:15 8.1690 -251.2 -304.3 2:23




Method: G087 Cont. Vanillin Date: 22-12-1999 10:02


RESULTS


1/1 992451 0.1234 g R1 = 99.78 % C8H8O3

1/2 992451 0.1232 g R1 = 99.83 % C8H8O3

1/3 992451 0.1189 g R1 = 100.40 % C8H8O3

1/4 992451 0.1114 g R1 = 100.29 % C8H8O3

1/5 992451 0.1150 g R1 = 99.88 % C8H8O3

1/6 992451 0.1174 g R1 = 100.47 % C8H8O3

STATISTICS





Titration curve

Results

95

Method: G087 Cont. Vanillin

Version: 22-12-1999 10:02

Title Method ID . . . . . . . . . . . . . G087 Title . . . . . . . . . . . . . . . Cont. Vanillin Date/time . . . . . . . . . . . . . 22-Dec-1999 10:02 Sample Number samples . . . . . . . . . . . 6 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.11 Upper limit [g] . . . . . . . . . 0.13 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 152.1 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 30 Titration Titrant . . . . . . . . . . . . . . NaOH Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG111-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . % nom. content Metered amount [%] . . . . . . 90.0 Nominal content . . . . . . . 100.0 Conversion const. . . . . . . M/(10*z) Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 250.0 Maximum volume [mL] . . . . . . . 10.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . C8H8O3 Formula . . . . . . . . . . . . . . R=(Q*C/m)+H20 Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Rinse Auxiliary reagent . . . . . . . . . Water Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes

Method

96

M161

Rutoside, also previously called Rutin or Vitamin P, prevents local oedemas while at the same timeimproving venous bloodflow. It is also used for the treatment of varicose veins.

RutosideM = 610.5 g/mol

Dimethylformamide R

c(TBAH) = 0.1 mol/L


Deprotonation of two of the fouralcohol groups

R-(OH)2 + 2TBAOH → R-O2Na2 +2H2O


METTLER TOLEDO


Waste disposal

DAB 1999; Monographie "Rutosid"(German)

Sample preparation

Rutoside, C27H30O16Sample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG113-SCIndication

Content Determination of Rutoside

Weigh a sample of 0.19 to 0.21 g Rutoside,accurately to 0.1 mg, in a 100 mL titration beakerand dissolve in 50 mL dimethyl formamide.


Remarks

R(%) = (Q • M/(10 •2•m)) + H20

Q = Titrant consumption in mmolM = Molar mass Rutosidem = Sample size in gH20 = % Loss on drying of Rutoside2 = Equivalent number

Calculation

Method for the alkalimetric content determination of Rutoside

Standard Benzoic acid (M523)

L. Pludra

Author

Structure

97


ET1 0.0000 -215.0 0:04 2.2850 -304.1 -39.0 0:19 3.4270 -320.4 -14.3 0:28

ET2 4.0000 -325.5 -8.9 0:33 4.2000 -327.1 -8.1 0:37 4.4000 -328.9 -8.8 0:41 4.6000 -330.7 -9.5 0:45 4.8000 -332.4 -8.1 0:49 5.0000 -333.9 -7.7 0:53 5.2000 -335.7 -9.1 0:57 5.4000 -338.0 -11.6 1:01 5.6000 -340.3 -11.2 1:05 5.8000 -344.0 -18.9 1:11 6.0000 -351.0 -34.6 1:19 6.1580 -377.4 -167.0 1:23 6.1840 -396.4 -732.3 1:35

EQP1 6.2040 -416.6 -1008.0 1:47 6.2240 -432.3 -787.5 1:56 6.2440 -442.7 -521.5 2:04




Method: G025 Cont. Rutosid Date: 18-11-1999 15:28


RESULTS


1/1 993008 0.1986 g R1 = 100.48 % C27H30O16

1/2 993008 0.2009 g R1 = 99.95 % C27H30O16

1/3 993008 0.1985 g R1 = 100.15 % C27H30O16

1/4 993008 0.1997 g R1 = 99.76 % C27H30O16

1/5 993008 0.1987 g R1 = 99.95 % C27H30O16

1/6 993008 0.1963 g R1 = 99.29 % C27H30O16

STATISTICS





Titration curve

Results

98

Method: G025 Cont. Rutosid Version: 8-11-1999 15:28

Title Method ID . . . . . . . . . . . . . G025 Title . . . . . . . . . . . . . . . Cont. Rutosid Date/time . . . . . . . . . . . . . 18-Nov-1999 15:28 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.19 Upper limit [g] . . . . . . . . . 0.21 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 610.5 Equivalent number z . . . . . . . . 2 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 30 Titration Titrant . . . . . . . . . . . . . . TBAH Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG113-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 4 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 250.0 Maximum volume [mL] . . . . . . . 10.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . C27H30O16 Formula . . . . . . . . . . . . . . R=(Q*C/m)+H20 Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Rinse Auxiliary reagent . . . . . . . . . Methanol Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes

Method

99

M162

Sodium Starch Glycolate, also known as Primojel, aids in improving the disintegration time of solid drugpreparations such as tablets and capsules.

Sodium chlorideM = 58.443 g/mol

Ethanol 80% RDeionised water RNitric acid 12.5% R

c(AgNO3) = 0.1 mol/L


Precipitation of chloride with silvernitrate

AgNO3 + NaCl → AgCl + NaNO3


METTLER TOLEDO


Waste disposal

Ph. Eur. 1997, Monograph "SodiumStarch Glycolate, (Type A)"

Sample preparation

Sodium Starch GlycolateSample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DM141-SCIndication

Content Determination of Sodium Chloride in Sodium Starch Glycolate

Weigh a sample of 0.90 to 1.10 g Primojel into a100 mL Erlenmeyer flask, add 20 mL ethanol 80 %(V/V) and shake for 10 min. Filter the resultingsuspension through a pleated filter into a 250 mLevaporating flask. Wash the residue four times inEthanol 80 % (V/V), each time using 20 mL. Whatremains in the filter will be used for the contentdetermination.Combine the filtrates and dry to a small bulk on arotary evaporator. Wash out the residue of the driedfiltrate with 5 mL deion. water. Transfer into a 25 mLvolumetric flask with 15 mL deion. water and fill upto the mark. Finally, transfer 10 mL of this samplesolution with 5 mL nitric acid 12.5% and 30 mLdeion. water, into a 100 mL titration beaker.

The dried and crushed residue is used for the contentdetermination.

Remarks

R(%) = Q • M•2.5/(10 •m)

Q = Titrant consumption in mmolM = Molar mass Sodium Chloridem = Sample size in g2.5 = Factor from the aliquotation of the samplesolution, i.e. 10 mL are used for thedetermination.

Calculation

Method for the argentometric determination of sodium chloride in Primojel

Standard Sodium chloride (vgl. M525)

L. Pludra

Author

Structure

100


ET1 0.0000 -55.1 0:04 0.0025 -54.7 140.0 0:08 0.0050 -54.5 84.0 0:12 0.0100 -54.1 84.0 0:16 0.0200 -53.8 35.0 0:21 0.0400 -53.3 21.0 0:25 0.0800 -52.8 14.0 0:29 0.1600 -51.9 11.4 0:34 0.3200 -50.3 9.6 0:39 0.5700 -47.9 9.8 0:44

\\ \\ \\ \\ 1.0700 -42.0 12.3 0:55 2.8090 40.5 364.7 2:10 2.8230 46.4 420.0 2:16 2.8370 53.8 530.0 2:21 2.8510 64.0 730.0 2:27 2.8655 80.0 1100.7 2:36

EQP1 2.8800 101.4 1472.4 2:45 2.8945 121.0 1356.5 2:55 2.9090 133.4 854.5 3:01




Method: G037 Cont. NaCl in Primojel Date: 05-10-1999 14:52

User: Rechenb.Kuntze Measured: 05-10-1999 14:59

RESULTS


1/1 992512 1.0038 g R1 = 4.220 % NaCl

1/2 992512 1.0079 g R1 = 4.247 % NaCl

1/3 992512 1.0086 g R2 = 4.182 % NaCl

STATISTICS


Mean value x = 4.216 % NaCl

Standard deviation s = 0.032776 % NaCl

Rel. standard deviation srel = 0.777

Titration curve

Results

101

Method: G037 Cont. NaCl in Primojel Version: 05-10-1999 14:52

Title Method ID . . . . . . . . . . . . . G037 Title . . . . . . . . . . . . . . . Cont. NaCl in Primojel Date/time . . . . . . . . . . . . . 16-Dec-1999 13:58 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.9 Upper limit [g] . . . . . . . . . 1.1 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 58.443 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 85 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . AgNO3 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DM141-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 6.0 Limits dV . . . . . . . . . . Relative dV(min) [%dosVol] . . . . . 0.5 dV(max) [%buVol] . . . . . 5.0 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 2.0 t(min) [s] . . . . . . . . . . 4.0 t(max) [s] . . . . . . . . . . 45.0 Threshold . . . . . . . . . . . . 50.0 Maximum volume [mL] . . . . . . . 20.0 Evaluation procedure . . . . . . Standard Steepest jump only . . . . . . . Yes Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . NaCl Formula . . . . . . . . . . . . . . R=Q*C*2.5/m Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Rinse Auxiliary reagent . . . . . . . . . Water Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer Short-form method . . . . . . . . . Yes All results . . . . . . . . . . . . Yes

Method

102

M163

Hydroxyethylsalicylate, like salicylic acid and other of its derivatives, is a pain killer, reduces fever and is aweak anti-inflammatory.

HydroxyethylsalicylateM = 182.2 g/mol

Acetic acid 98% RSulphuric acid 10% RPotassium bromide RDeionised water RPotassium iodide solution 16.6% R

c(KBrO3) = 0.1 mol/Lc(Na2S2O3) = 0.1 mol/L


1. Conproportionation of bromate and bromide in an acidicmedium to bromine

BrO3- + 5Br- + 6H+ → 3Br2 + 3 H20

2. Electrophilic bromination of hydroxyethylsalicylate to(2-hydroxyethyl)-3,5-dibrom-2-hydroxybenzoate with bromine

3. Excess bromine is reduced by iodide under the formation ofiodine

Br2 + 2I- → I2 + 2Br-

4. Iodine is reduced with thiosulphate to iodideI2 + 2S2O3

2- → 2I- + S4O62-

Brown glass titration beaker

METTLER TOLEDO


Waste disposal

Ph. Eur. 1997; Monograph"Hydroxyethylsalicylate"

Sample preparation

Hydroxyethylsalicylate C9H10O4Sample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DM140-SCIndication

Content Determination of Hydroxyethylsalicylate

Weigh a sample of 0.14 to 0.16 g hydroxyethyl-salicylate, accurately to 0.1 mg, into a 100 mLbrown glass titration beaker and dissolve in 30 mLacetic acid 98%. Add 10 mL sulphuric acid 10%and 1.5 g potassium bromide to the solution.

Remarks

R(%) = (QDISP-Q)• M/(10 •m•4)

QDISP = Total amount of dispensed Bromate inmmolQ = Thiosulphate consumption in mmolM = Molar mass Hydroxylsalicylatem = Sample size in g4 = Equivalent number

Calculation

Method for the bromatometric content determination of Hydroxyethylsalicylate

Standard Arsenic trioxidePotassium iodate (M526)

L. Pludra

Author

Structure

103


ET1 0.0000 358.5 0:02 7.4280 351.5 -1.0 0:12 11.1420 345.3 -1.7 0:19

ET2 13.0000 340.4 -2.6 0:23 14.0000 336.6 -3.9 0:27 15.0000 331.2 -5.4 0:31 16.0000 321.6 -9.5 0:35 16.5860 307.7 -23.8 0:41 16.7960 292.9 -70.3 0:48 16.8640 278.2 -216.2 0:59 16.8860 271.6 -302.3 1:06 16.9060 262.5 -455.0 1:15 16.9260 250.9 -577.5 1:27

EQP1 16.9460 233.6 -868.0 1:48 16.9660 220.1 -675.5 2:05 16.9860 211.0 -451.5 2:16




Method: G023 Cont. Hydroxysalicylate Date: 05-07-1999 10:04


RESULTS


1/1 991573 0.1543 g R1 = 99.735 % C9H10O4

1/2 991573 0.1472 g R1 = 99.779 % C9H10O4

1/3 991573 0.1420 g R1 = 100.100 % C9H10O4

1/4 991573 0.1417 g R1 = 99.682 % C9H10O4

STATISTICS





Titration curve

Results

104

Method: G023 Cont. Hydroxylsalicylate Version: 05-07-1999 10:04

Title Method ID . . . . . . . . . . . . . G023 Title . . . . . . . . . . . . . . . Cont.Hydroxylsalicylate Date/time . . . . . . . . . . . . . 05-Jul-1999 10:04 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . Stand 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.14 Upper limit [g] . . . . . . . . . 0.16 ID1 . . . . . . . . . . . . . . . . Test-Nr. Molar mass M . . . . . . . . . . . . 182.2 Equivalent number z . . . . . . . . 4 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 10 Dispense Titrant . . . . . . . . . . . . . . KBrO3 Concentration [mol/L] . . . . . . . 0.1 Volume [mL] . . . . . . . . . . . . 50 Stir Speed [%] . . . . . . . . . . . . . 40 Time [s] . . . . . . . . . . . . . . 900 Dispense Titrant . . . . . . . . . . . . . . KI Concentration [mol/L] . . . . . . . 1.0 Volume [mL] . . . . . . . . . . . . 10 Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 15 Titration Titrant . . . . . . . . . . . . . . Na2S2O3 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DM140-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 13 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 1.0 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 2.0 t(max) [s] . . . . . . . . . . 20.0 Threshold . . . . . . . . . . . . 100.0 Maximum volume [mL] . . . . . . . 22.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Calculation Result name . . . . . . . . . . . . C9H10O4 Formula . . . . . . . . . . . . . . R=(QDISP-Q)*C/m Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 3 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer+Computer All results . . . . . . . . . . . . Yes

Method

105

M164

Mephenesine is a muscle relaxant.

MephenesineM = 182.2 g/mol

Chloroform REthanol 96% RPotassium bromide RPotassium iodide solution 16.6%RHydrochloric acid 25% R

c(KBrO3) = 0,1 mol/Lc(Na2S2O3) = 0,1 mol/L


1. Conproportionation of bromate and bromide in an acidicmedium to bromine

BrO3- + 5Br- + 6H+ → 3Br2 + 3 H20

2. Electrophilic bromination of the Benzol rings of Mephe -nesinon positions 3, 4 and 6 with excess bromine

3. Excess bromine is reduced by iodide under the formation ofiodine

Br2 + 2I- → I2 + 2Br-

4. Iodine is reduced with thiosulphate to iodideI2 + 2S2O3

2- → 2I- + S4O62-


METTLER TOLEDO


Waste disposal

IP (Italian Pharmacopoeia) 1985;Monograph "Mephenesina"

Sample preparation

Mephenesine, C10H14O3Sample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DM140-SCIndication

Content Determination of Mephenesine

Weigh a sample of 0.24 to 0.26 g Mephenesine,accurately to 0.1 mg, into a 100 mL titration beaker.Add 20 mL ethanol 96% and dissolve in anultrasonic bath. Then add 2.0 g potassium bromideand 5 mL hydrochloric acid 25%.

The previously determined loss on drying content issaved as the auxilliary value H20.The Rondo60 sample changer is used for thecompletely automated analysis. If the titration isdone manually on the titration stand, an additional 5mL chloroform must be added to each titrationbeaker before titrating.

Remarks

R(%) = ((QDISP-Q)• M/(10 •m•2))+H20

QDISP = Total amount of dispensed Bromate inmmolQ = Thiosulphate consumption in mmolM = Molar mass Hydroxyl Salicylatem = Sample size in gH20 = % Loss on drying of Mephenesine2 = Equivalent number

Calculation

Method for the bromatometric content determination of Mephenesine


L. Pludra

Author

Structure

106


ET1 0.0000 322.3 0:05 ET2 0.0000 322.2 0:06

0.0040 322.2 0.0 0:11 0.0120 322.3 8.7 0:16 0.0280 322.1 -8.7 0:21 0.0600 322.0 -4.4 0:27 0.1240 321.6 -6.6 0:32 0.2520 320.9 -4.9 0:38 0.4520 319.9 -5.3 0:43 0.6520 318.8 -5.6 0:49 0.8520 317.5 -6.3 0:54 1.0520 316.4 -5.6 1:00 1.2520 314.9 -7.7 1:05 1.4520 313.3 -7.7 1:11 1.6520 311.4 -9.5 1:17 1.8520 309.2 -11.2 1:22 2.0520 306.7 -12.6 1:28 2.2520 303.4 -16.5 1:33 2.4520 299.1 -21.4 1:39 2.6520 292.7 -31.8 1:44 2.8400 280.8 -63.3 1:50 2.9240 267.6 -157.5 1:55 2.9540 255.6 -399.0 2:01 2.9660 242.1 -1125.8 2:06 2.9700 240.2 -490.0 2:11 2.9740 228.3 -2957.5 2:20 2.9780 213.1 -3815.0 2:32

EQP1 2.9820 193.6 -4865.0 2:44 2.9860 190.0 -910.0 2:50 2.9900 182.2 -1942.4 2:57




Method: G072 Cont. Mephenesine Date: 27-07-1999 14:10

User: **Ehrlich** Measured: 28-07-1999 8:06

RESULTS


1/1 991898 0.2460 g R1 = 100.32 % C10H14O3

1/2 991898 0.2458 g R1 = 100.01 % C10H14O3

1/3 991898 0.2502 g R1 = 99.84 % C10H14O3

1/4 991898 0.2445 g R1 = 99.85 % C10H14O3

1/5 991898 0.2419 g R1 = 99.49 % C10H14O3

1/6 991898 0.2490 g R1 = 99.64 % C10H14O3

STATISTICS





Titration curve

Results

107

Method: G072 Cont. Mephenesine

Version: 27-07-1999 14:10

Title Method ID . . . . . . . . . . . . . G072 Title . . . . . . . . . . . . . . . Cont. Mephenesine Date/time . . . . . . . . . . . . . 28-Jul-1999 9:49 Sample Number samples . . . . . . . . . . . 4 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.24 Upper limit [g] . . . . . . . . . 0.26 ID1 . . . . . . . . . . . . . . . . Test-Nr. Molar mass M . . . . . . . . . . . . 182.2 Equivalent number z . . . . . . . . 2 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 10 Dispense Titrant . . . . . . . . . . . . . . KBrO3 Concentration [mol/L] . . . . . . . 0.1 Volume [mL] . . . . . . . . . . . . 30 Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 60 Dispense Titrant . . . . . . . . . . . . . . KJ 16,6% Concentration [mol/L] . . . . . . . 1.0 Volume [mL] . . . . . . . . . . . . 5 Stir Speed [%] . . . . . . . . . . . . . 75 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . Na2S2O3 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DM140-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 0 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Relative dV(min) [%dosVol] . . . . . 0.05 dV(max) [%buVol] . . . . . 1.0 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 5.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 50.0 Maximum volume [mL] . . . . . . . 15.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Steepest jump only . . . . . . . Yes Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . C10H14O3 Formula . . . . . . . . . . . . . . R=((QDISP-Q)*C/m)+H20 Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Rinse Auxiliary reagent . . . . . . . . . Water Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes

Method

108

M165

Methyl-4-hydroxybenzoate is especially used as a preservative in eye medications and topical preparations.

Methyl-4-hydroxybenzoateM = 152.15 g/mol

Potassium bromide RHydrochloric acid 37% RAcetic acid 98% RPotassium iodide solution 16.6% RSodium hydroxide solution 8.5% RDeionised water R


METTLER TOLEDO DL77/DL70ESMETTLER TOLEDO DL58/55

1. Conproportionation of bromate and bromide in anacidic medium to bromine.

BrO3- + 5Br- + 6H+ → 3Br2 + 3 H20

2. After saponification of the ester with NaOH, oxidationof the hydroxyl groups to ketone, as well as theelectrophilic bromination of the benzol ring with bromine,takes place.3. Excess bromine is reduced by iodide under theformation of iodine

Br2 + 2I- → I2 + 2Br-

4. Iodine is reduced with thiosulphate to iodide.I + 2S O 2- → 2I- + S O 2-

250 mL Glass titration beakerRondo60 Sample changer

METTLER TOLEDO


Waste disposal

Ph. Eur. 1997; Monograph"Methyl-4-hydroxybenzoate"

Sample preparation

Methyl-4-hydroxybenzoate, C8H8O3Sample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DM140-SCIndication

Content Determination of Methyl-4-hydroxybenzoate

Weigh 72.0 to 82.0 mg methyl-4-hydroxy-benzoate in a 100 mL round-bottomed flask. Add25 mL sodium hydroxide solution 8.5% to thesample flask as well as to an additional two flasksfor the blank determination. Reflux for 30 minutes ina hot waterbath.Cool the solutions and transfer into a 250 mLtitration beaker, rinsing twice with deionised water.Add 50 mL 0.1N potassium bromate solution, 0.63g potassium bromide and 40 mL acetic acid 98%.Allow to cool for 3 minutes. Finally, add 10 mLhydrochloric acid 37%, wrap the titration beakerwith aluminium foil and start the titrationimmediately.

A Rondo60 sample changer is used for thecompletely automated analysis. If the titration isdone manually on the titration stand, an additional 5mL chloroform must be added to each titrationbeaker before titrating.

Remarks

R(%) = (x-Q[2])• M/(10 •m•6)

Q [2]= Thiosulphate consumption in mmolx = Mean value of the blank determination inmmolM = Molar mass Methyl-4-hydroxybenzoatem = Sample size in g6 = Equivalent number

Calculation

Method for the bromatometric determination of Methyl-4-hydroxybenzoate


L. Pludra

Author

Structure

109


ET1 0.0000 358.2 0:05 8.5700 347.1 -1.3 0:19 12.8540 335.9 -2.6 0:28

ET2 15.0000 323.0 -6.0 0:36 15.5000 316.5 -12.9 0:42 15.8040 310.2 -21.0 0:47 16.0100 303.1 -34.3 0:53 16.1340 295.6 -60.4 0:58 16.2140 286.9 -109.4 1:04 16.2960 248.9 -462.7 1:14

EQP1 16.3780 210.2 -472.1 1:36 16.4600 201.0 -112.7 1:46 16.5420 196.1 -58.9 1:53




Method: G075 Methyl-4-hydroxybenzoate Date: 20-12-1999 10:50


RESULTS


1/1 982094 50.0 mL R1 = 5.053 mmol Blank

1/2 982094 50.0 mL R1 = 5.049 mmol Blank

1/3 982094 50.0 mL R1 = 5.050 mmol Blank

2/1 982094 0.0852 g R2 = 101.27 % C8H8O3

2/2 982094 0.0774 g R2 = 99.86 % C8H8O3

2/3 982094 0.0785 g R2 = 99.81 % C8H8O3

2/4 982094 0.0821 g R2 = 99.64 % C8H8O3

2/5 982094 0.0816 g R2 = 99.62 % C8H8O3

2/6 982094 0.0794 g R2 = 99.94 % C8H8O3

STATISTICS





STATISTICS





Titration curve

Results

110

Method: G075 Methyl-4-hydroxybenzoate Version: 20-12-1999 10:50

Title Method ID . . . . . . . . . . . . . G075 Title . . . . . . . . . . . . . . .Methyl-4-hydroxybenzoate Date/time . . . . . . . . . . . . . 20-Dec-1999 10:50 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . Stand 1 Entry type . . . . . . . . . . . . . Fixed volume U Volume [mL] . . . . . . . . . . . 50.0 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 0.0 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Dispense Titrant . . . . . . . . . . . . . . KJ 16,6% Concentration [mol/L] . . . . . . . 1.0 Volume [mL] . . . . . . . . . . . . 15 Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 30 Titration Titrant . . . . . . . . . . . . . . Na2S2O3 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DM140-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 45.0 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 6.0 Limits dV . . . . . . . . . . Relative dV(min) [%dosVol] . . . . . 0.5 dV(max) [%buVol] . . . . . 2.5 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.25 dt [s] . . . . . . . . . . . . 5.0 t(min) [s] . . . . . . . . . . 5.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 250.0 Maximum volume [mL] . . . . . . . 55.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . Blank Formula . . . . . . . . . . . . . . R1=Q Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . mmol Decimal places . . . . . . . . . . . 3 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes

Method Sample Number samples . . . . . . . . . . . 6 Titration stand . . . . . . . . . . Stand 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.072 Upper limit [g] . . . . . . . . . 0.088 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 152.1 Equivalent number z . . . . . . . . 6 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 30 Time [s] . . . . . . . . . . . . . . 600 Dispense Titrant . . . . . . . . . . . . . . KJ 16,6% Concentration [mol/L] . . . . . . . 1.0 Volume [mL] . . . . . . . . . . . . 15 Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . Na2S2O3 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DM140-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 15.0 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 6.0 Limits dV . . . . . . . . . . Relative dV(min) [%dosVol] . . . . . 0.5 dV(max) [%buVol] . . . . . 2.5 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.25 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 5.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 150.0 Maximum volume [mL] . . . . . . . 20.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . C8H8O3 Formula . . . . . . . . . . . . . . R2=(x-Q[2])*C/m Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R2 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes

111

M166

Phenol is well resorbed by the skin and mucous membranes and is effective against vegetative forms ofbacteria as well as some fungi and viruses.

PhenolM = 94.1 g/mol

Chloroform RDeionised water RPotassium iodide solution 16.6% R



1. Conproportionation of bromate and bromide in anacidic medium to bromine.

BrO3- + 5Br- + 6H+ → 3Br2 + 3 H20

2. Oxidation of phenol with excess bromine to2,4,4,6-Tetrabromo-2,5-cyclohexadien-1-one

3. Excess bromine is reduced by iodide under theformation of iodine.

Br2 + 2I- → I2 + 2Br-

4. Iodine is reduced with thiosuphate to iodide.I2 + 2S2O3

2- → 2I- + S4O62-


METTLER TOLEDO


Waste disposal

DAC 1986, 3. Lieferung 88;Monographie "Verflüssigtes Phenol"(German)

Sample preparation

Phenol, C6H6OSample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DM140-SCIndication

Content Determination of Phenol in Liquified Phenol

Weigh a sample of 0.12 to 0.3 g liquified phenol,accurately to 0.1 mg, in a 100 mL volumetric flaskand fill up to the mark with deionised water. Transfer25 mL of the solution in the flask into a 100 mLtitration beaker and add 0.5 g potassium bromideand 15 mL hydrochloric acid 7%.

The method corresponds essentially with the Ph. Eur.1997 monograph "Phenol".A Rondo60 sample changer is used for thecompletely automated analysis. If the titration isdone manually on the titration stand, an additional 5mL chloroform must be added to each titrationbeaker before titrating.

Remarks

R(%) = (QDISP-Q)• M•4/(10 •m•6)QDISP = Total amount of dispensed Bromate inmmolQ = Thiosulphate consumption in mmolM = Molar mass Phenolm = Sample size in g6 = Equivalent number4 = Factor from the aliquotation of the sample sol.

Calculation

Method for the bromatometric determination of Phenol


L. Pludra

Author

Structure

112


ET1 0.0000 -295.0 0:12 8.5710 -283.1 1.4 0:34 12.8560 -277.6 1.3 1:13

ET2 15.0000 -274.5 1.5 1:22 15.2000 -274.1 1.8 1:26 15.4000 -273.9 1.1 1:31 15.6000 -273.5 2.1 1:36 15.8000 -273.3 0.7 1:40 16.0000 -273.2 0.7 1:45

// // // // 21.0000 -260.0 8.8 5:24 21.2000 -257.1 14.7 5:32 21.3930 -244.0 67.8 5:49

EQP1 21.4260 -232.0 362.7 6:32 21.4460 -228.8 164.5 7:01 21.4660 -227.4 70.0 7:07




Method: G011 Cont. liquified Phenol Date: 22-09-1999 13:05

User: Kuntze/Rechenb. Measured: 22-09-1999 13:28

RESULTS


1/1 992464 0.1221 g R1 = 92.85 % C6H6O

1/2 992464 0.1211 g R1 = 93.22 % C6H6O

1/3 992464 0.1224 g R1 = 92.24 % C6H6O

1/4 992464 0.1234 g R1 = 91.53 % C6H6O

1/5 992464 0.1207 g R1 = 93.51 % C6H6O

1/6 992464 0.1216 g R1 = 92.69 % C6H6O

STATISTICS


Mean value x = 92.67 % C6H6O

Standard deviation s = 0.709040 % C6H6O


Titration curve

Results

113

Method: G011 Cont. liquified Phenol Version: 22-09-1999 13:05

Title Method ID . . . . . . . . . . . . . G011 Title . . . . . . . . . . . . . . . Cont. liquified Phenol Date/time . . . . . . . . . . . . . 22-Sep-1999 13:05 Sample Number samples . . . . . . . . . . . 4 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.12 Upper limit [g] . . . . . . . . . 0.13 ID1 . . . . . . . . . . . . . . . . Test-Nr. Molar mass M . . . . . . . . . . . . 94.1 Equivalent number z . . . . . . . . 6 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 5 Dispense Titrant . . . . . . . . . . . . . . KBrO3 Concentration [mol/L] . . . . . . . 0.1 Volume [mL] . . . . . . . . . . . . 20 Stir Speed [%] . . . . . . . . . . . . . 70 Time [s] . . . . . . . . . . . . . . 300 Dispense Titrant . . . . . . . . . . . . . . KJ 16,6% Concentration [mol/L] . . . . . . . 1.0 Volume [mL] . . . . . . . . . . . . 5 Rinse Auxiliary reagent . . . . . . . . . CHCl3 Volume [mL] . . . . . . . . . . . . 15.0 Stir Speed [%] . . . . . . . . . . . . . 75 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . Na2S2O3 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DM140-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 0.3 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.25 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 5.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 250.0 Maximum volume [mL] . . . . . . . 6.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . C6H6O Formula . . . . . . . . . . . . . . R=(QDISP-Q)*C*4/m Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 3 Rinse Auxiliary reagent . . . . . . . . . CHCl3 Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer Short-form method . . . . . . . . . Yes All results . . . . . . . . . . . . Yes

Method

114

M167

Ascorbic acid (Vitamin C) is used for the prophylaxis and treatment of scurvy, pre-scurvy andMöller-Barlowscher Disease.

Ascorbic AcidM = 176.1 g/mol

Deionised water RSulphuric acid 5% R

c(I2) = 0,05 mol/L


Oxidation of ascorbic acid byelementary iodine in an acidicmedium.


METTLER TOLEDO

Halogen free organic solvents waste.

Waste disposal

Ph. Eur. 1997; Monograph "AscorbicAcid"

Sample preparation

Ascorbic Acid, C6H8O6Sample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DM140-SCIndication

Content Determination of Ascorbic Acid (Vitamin C)

Weigh a sample of 0.14 to 0.16 g ascorbic acid,accurately to 0.1 mg, in a 100 mL titration beakerand dissolve in 10 mL sulphuric acid 5%. Add 40mL deionised water.


Remarks

R(%) = (Q • M/(10 •m)) + H20

Q = Titrant consumption in mmolM = Molar mass Ascorbic Acidm = Sample size in gH20 = % Loss on drying of Ascorbic Acid

Calculation

Method for the iodometric determination of Ascorbic Acid

Standard Ascorbic Acid

L. Pludra

Author

Structure

115


ET1 0.0000 324.9 0:32 8.5700 311.8 -1.5 0:42 12.8540 296.4 -3.6 0:46

ET2 15.0000 235.6 -28.3 1:19 15.1500 233.7 -12.6 1:34 15.3300 232.4 -7.4 1:55 15.5300 231.8 -2.8 2:20 15.7300 230.9 -4.6 2:48 15.9300 232.1 6.0 3:19 16.1300 233.7 8.1 3:49 16.3300 234.7 4.9 4:20 16.5300 237.9 16.1 4:50 16.7300 240.3 11.9 5:21 16.9300 244.6 21.7 5:52

EQP1 17.1300 331.2 432.9 5:59 17.1400 332.2 98.0 6:04 17.1500 333.1 84.0 6:08




Method: G085 Cont. Ascorbic acid Date: 21-12-1999 11:22


RESULTS


1/1 990034 0.1489 g R1 = 99.76 % C6H8O6

1/2 990034 0.1475 g R1 = 99.76 % C6H8O6

1/3 990034 0.1473 g R1 = 99.46 % C6H8O6

1/4 990034 0.1454 g R1 = 99.20 % C6H8O6

1/5 990034 0.1501 g R1 = 99.40 % C6H8O6

1/6 990034 0.1524 g R1 = 99.37 % C6H8O6

STATISTICS

Number of results n = 6




Titration curve

Results

116

Method: G085 Cont. Ascorbic acid Version: 21-12-1999 11:22

Title Method ID . . . . . . . . . . . . . G085 Title . . . . . . . . . . . . . . . Cont. Ascorbic Acid Date/time . . . . . . . . . . . . . 21-Dec-1999 10:53 Sample Number samples . . . . . . . . . . . 6 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.14 Upper limit [g] . . . . . . . . . 0.16 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 176.1 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 75 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . I2 Concentration [mol/L] . . . . . . . 0.05 Sensor . . . . . . . . . . . . . . . DM140-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 15 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 3.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 400.0 Maximum volume [mL] . . . . . . . 25.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Rinse Auxiliary reagent . . . . . . . . . Water Volume [mL] . . . . . . . . . . . . 20.0 Calculation Result name . . . . . . . . . . . . C6H8O6 Formula . . . . . . . . . . . . . . R1=(Q*C/m)+H20 Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes

Method

117

M168

Palmitoyl ascorbic acid, also known as ascorbyl palmitate, is an anti-oxidant.

Palmitoyl Ascorbic AcidM = 414.5 g/mol

Methanol RDeionised water R

c(I2) = 0,05 mol/L


Oxidation of palmitoyl ascorbic acidby iodine in an acidic medium.


METTLER TOLEDO


Waste disposal

Ph. Eur. 1997; Monograph"Palmitoyl Ascorbic Acid"

Sample preparation

Palmitoyl Ascorbic Acid, C22H38O7Sample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DM140-SCIndication

Content Determination of Palmitoyl Ascorbic Acid

Weigh a sample of 0.15 to 0.17 g palmitoylascorbic acid, accurately to 0.1 mg, in a 100 mLtitration beaker and dissolve in 40 mL methanol.


Remarks

R(%) = (Q • M/(10 •m)) + H20

Q = Titrant consumption in mmolM = Molar mass Ascorbyl Palmitatem = Sample size in gH20 = % Loss on drying of Ascorbyl Palmitate

Calculation

Method for the iodometric determination of Palmitoyl Ascorbic Acid

Standard Ascorbic acid

L. Pludra

Author

Structure

118


ET1 0.0000 143.6 0:03 0.5700 162.0 32.3 0:12 0.8540 167.6 20.0 0:18

ET2 1.0000 170.2 17.7 0:23 1.2000 172.7 12.3 0:28 1.4000 175.0 11.6 0:32

\\ \\ \\ \\ 6.2000 229.9 51.1 3:20 6.3060 236.1 58.8 3:43 6.4260 243.7 63.0 4:10 6.5440 254.0 87.8 4:40 6.6140 262.1 116.0 5:11 6.6680 268.9 125.7 5:41 6.7260 278.2 159.3 6:12 6.7660 284.1 148.7 6:42 6.8220 326.1 748.7 7:12 6.8420 318.4 -381.5 7:43

EQP1 6.8820 355.8 934.5 7:50 6.9020 362.9 357.0 7:53 6.9220 367.8 245.0 7:57

\\ \\ \\ \\



Onkel Tuka DL70 Quality Control laboratory

Method: G081 Cont. Ascorbyl palmitate Date: 06-07-1999 9:58

User: Ch. Dzionara Measured: 06-07-1999 15:24

RESULTS


1/1 991568 0.1662 g R1 = 99.515 %

1/2 991568 0.1714 g R1 = 99.717 %

1/3 991568 0.1655 g R1 = 99.721 %

1/4 991568 0.1672 g R1 = 99.905 %

1/5 991568 0.1622 g R1 = 99.272 %

1/6 991568 0.1608 g R1 = 99.308 %

STATISTICS


Mean value x = 99.573 %

Standard deviation s = 0.25200 %


Titration curve

Results

119

Method: G081 Cont. Ascorbyl palmitate

Version: 06-07-1999 9:58

Title Method ID . . . . . . . . . . . . . G081 Title . . . . . . . . . . . . . . . Cont. Ascorbylpalmitate Date/time . . . . . . . . . . . . . 06-Jul-1999 9:58 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.15 Upper limit [g] . . . . . . . . . 0.17 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 414.5 Equivalent number z . . . . . . . . 2 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 75 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . 1/2 I2 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DM140-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 5.0 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 3.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 400.0 Maximum volume [mL] . . . . . . . 10.0 Evaluation procedure . . . . . . Standard Steepest jump only . . . . . . . Yes Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Rinse Auxiliary reagent . . . . . . . . . H2O Volume [mL] . . . . . . . . . . . . 20.0 Calculation Result name . . . . . . . . . . . . Content Formula . . . . . . . . . . . . . . R=(Q*C/m)+H20 Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 3 Record Output unit . . . . . . . . . . . . Printer+Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer Short-form method . . . . . . . . . Yes All results . . . . . . . . . . . . Yes

Method

120

M169

Calcium stearate is used as an auxiliary reagent in the preparation of tablets and capsules.

CalciumM = 40.08 g/mol

1-Butanol RAmmonium chloride buffer solutionpH 10 R (1 mL 10 mM HgEDTA)0.1M Na2-EDTAEthanol, anhydrous RAmmonia solution 26%

c(ZnSO4) = 0.1 mol/L

METTLER TOLEDO DL77/DL70ESMETTLER TOLEDODL58/55/53/50Graphix

Complexation of calcium byNa2-EDTA in an alkaline medium.The detection of the equivalencepoint takes place with a mercuryindicator electrode whose potentialis dependent on the concentration offree mercury ions.


METTLER TOLEDO

Halogen-free organic solvents waste, zinccontaining.

Waste disposal

Ph. Eur. 1997; Monograph "CalciumStearate"

Sample preparation

Calcium stearate, C36H70O4CaSample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DM141-SC (amalgamated)Indication

Content Determination of Calcium in Calcium Stearate

Weigh a sample of 0.49 to 0.51 g calcium stearate,accurately to 0.1 mg, in a 100 mL titration beaker.Add 50 mL of a solution of equal volumes 1-butanoland anhydrous ethanol. Pipette into the sample 5mL ammonium solution 26%, 3 mL ammoniumchloride buffer solution pH10 and 30 mL 0.1MNa2-EDTA. Place the titration beaker in an ultrasonicbath at 45 - 50 °C, and leave for approximately fiveminutes until the sample is completely dissolved.Prepare two blank determination samples in thesame way.


Remarks

R(%) = (x-Q) • M • F/(10 • m)Q = Titrant consumption in mmolx = Mean value of the blank determination inmmolF = 100/(100-H20) Formula for the loss ondrying of Calcium StearateM = Molar mass Calciumm = Sample size in g

Calculation

Method for the complexometric determination of calcium in Calcium Stearate

Standard EDTA-Dihydrate (vgl. M539)

L. Pludra

Author

Structure

121


ET1 0.0000 -303.9 1:24 16.0000 -277.4 1.7 5:54 24.0000 -272.5 0.6 6:45

ET2 28.0000 -268.0 1.1 6:57 28.2000 -267.5 2.1 7:02 28.4000 -267.3 1.1 7:07 28.6000 -266.9 2.1 7:12 28.8000 -266.6 1.4 7:17 29.0000 -266.1 2.5 7:23 29.2000 -265.7 2.1 7:38 29.4000 -264.9 3.9 7:43 29.6000 -263.8 5.6 7:50 29.8000 -261.4 12.3 7:59 30.0000 -247.7 68.2 8:29

EQP1 30.0320 -243.9 118.1 9:06 30.0550 -242.1 79.1 9:18 30.1010 -240.0 47.2 9:31




Method: G046 Ca cont. in Ca-Stearate Date: 29-10-1999 10:03

User: Kuntze/Karasch Measured: 29-10-1999 11:24

RESULTS


1/1 992389 30.0 mL R1 = 3.003 mmol Blank

1/2 992389 30.0 mL R1 = 3.003 mmol Blank

2/1 992389 0.4985 g R2 = 7.072 % Ca

2/2 992389 0.4993 g R2 = 7.075 % Ca

2/3 992389 0.5000 g R2 = 7.071 % Ca

2/4 992389 0.4946 g R2 = 7.067 % Ca

2/5 992389 0.4999 g R2 = 7.067 % Ca

2/6 992389 0.4949 g R2 = 7.060 % Ca

STATISTICS




Rel. Standard deviation srel = 0.019 %

STATISTICS


Mean value x = 7.069 % Ca

Standard deviation s = 0.005371 % Ca

Rel. Standard deviation srel = 0.076 %

Titration curve

Results

122

Method: G046 Cont. Ca in Ca-Stearate Version: 29-10-1999 10:03

Title Method ID . . . . . . . . . . . . . G046 Title . . . . . . . . . . . . . . . Cont. Ca inCa-Stearate Date/time . . . . . . . . . . . . . 05-Nov-1999 8:52 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Fixed volume U Volume [mL] . . . . . . . . . . . 30.0 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 1 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 75 Time [s] . . . . . . . . . . . . . . 15 Titration Titrant . . . . . . . . . . . . . . ZnSO4 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DM141-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 28 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 4.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.2 dt [s] . . . . . . . . . . . . 2.0 t(min) [s] . . . . . . . . . . 4.0 t(max) [s] . . . . . . . . . . 45.0 Threshold . . . . . . . . . . . . 50.0 Maximum volume [mL] . . . . . . . 32.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Steepest jump only . . . . . . . Yes Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . Blank det. Formula . . . . . . . . . . . . . . R1=Q Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . mmol Decimal places . . . . . . . . . . . 3 Rinse Auxiliary reagent . . . . . . . . . Water Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes

Method Sample Number samples . . . . . . . . . . . 4 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.49 Upper limit [g] . . . . . . . . . 0.51 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 40.08 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 75 Time [s] . . . . . . . . . . . . . . 15 Titration Titrant . . . . . . . . . . . . . . ZnSO4 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DM141-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 15 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 4.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.2 dt [s] . . . . . . . . . . . . 2.0 t(min) [s] . . . . . . . . . . 4.0 t(max) [s] . . . . . . . . . . 45.0 Threshold . . . . . . . . . . . . 50.0 Maximum volume [mL] . . . . . . . 25.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Steepest jump only . . . . . . . Yes Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . Ca Formula . . . . . . . . . . . . . . R2=((x-Q[2])*C/m) Constant . . . . . . . . . . . . . . C=M*10/(z*(100-H20)) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 3 Rinse Auxiliary reagent . . . . . . . . . Water Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R2 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer+Computer All results . . . . . . . . . . . . Yes

123

M170

Magnesium stearate is used as an auxiliary reagent in the preparation of tablets and capsules.

MagnesiumM = 24.31 g/mol

1-Butanol RAmmonium chloride buffer solutionpH 10 R (1mL 10 mM HgEDTA)0.1M Na2-EDTAEthanol, anhydrous RAmmonia solution 26%



Complexation of magnesium byNa2-EDTA in an alkaline medium.The detection of the equivalencepoint takes place with a mercuryindicator electrode whose potentialis dependent on the concentration offree mercury ions.


METTLER TOLEDO

Halogen-free organic solvents waste, zinccontaining.

Waste disposal

Ph. Eur. 1997; Monograph"Magnesium Stearate"

Sample preparation

Magnesium stearate, C36H70O4MgSample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DM141-SC (amalgamated)Indication

Content Determination of Magnesium in Magnesium Stearate

Weigh a sample of 0.74 to 0.76 g magnesiumstearate, accurately to 0.1 mg, in a 100 mL titrationbeaker and add 50 mL of a mixture of equalvolumes 1-butanol and anhydrous ethanol. Pipetteinto the sample 5 mL ammonium solution 26%, 3mL ammonium chloride buffer solution pH10 and30 mL 0.1M Na2-EDTA. Place the titration beaker inan ultrasonic bath at 45 - 50 °C, and leave forapproximately five minutes until the sample iscompletely dissolved.Prepare three blank determination samples in thesame way.


Remarks

R(%) = (x-Q) • M • F/(10 • m)Q = Titrant consumption in mmolx = Mean value of the blank determination inmmolF = 100/(100-H20) Formula for the loss ondrying of Magnesium StearateM = Molar mass Magnesiumm = Sample size in g

Calculation

Method for the complexometric determination of magnesium in Magnesium Stearate

Standard EDTA-Dihydrate (M539)

L. Pludra

Author

Structure

124


ET1 0.0000 -286.0 0:02 1.1420 -284.0 1.8 0:07 1.7130 -282.7 2.3 0:10

ET2 2.0000 -282.0 2.2 0:13 2.5000 -281.3 1.5 0:17 3.0000 -280.6 1.4 0:21

\\ \\ \\ \\ 14.0000 -264.7 2.9 2:20 14.5000 -263.1 3.2 2:25 15.0000 -261.0 4.3 2:29 15.5000 -258.2 5.6 2:34 16.0000 -251.9 12.6 2:42

EQP1 16.2550 -232.7 75.2 2:56 16.2910 -230.8 52.5 3:00 16.3630 -228.1 37.9 3:07

\\ \\ \\ \\



Onkel Tuka Quality Control Laboratory

Method: G061 Cont. Magnesium stearate Date: 29-10-1999 10:02

User: Kuntze/Karasch Measured: 29-10-1999 13:19

RESULTS


1/1 992563 30.0 mL R1 = 3.003 mmol Blank

1/2 992563 30.0 mL R1 = 3.003 mmol Blank

2/1 992563 0.7426 g R2 = 4.636 % Magnesium

2/2 992563 0.7447 g R2 = 4.639 % Magnesium

2/3 992563 0.7554 g R2 = 4.631 % Magnesium

2/4 992563 0.7522 g R2 = 4.635 % Magnesium

2/5 992563 0.7505 g R2 = 4.630 % Magnesium

2/6 992563 0.7441 g R2 = 4.622 % Magnesium

STATISTICS





STATISTICS


Mean value x = 4.632 % Magnesium

Standard deviation s = 0.006120 % Magnesium


Titration curve

Results

125

Method: G061 Cont. Magnesium stearate Version: 29-10-1999 10:02

Title Method ID . . . . . . . . . . . . . G061 Title . . . . . . . . . . . . . . . Cont. Magnesiumstearate Date/time . . . . . . . . . . . . . 29-Oct-1999 10:02 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Fixed volume U Volume [mL] . . . . . . . . . . . 30.0 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 0.0 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . ZnSO4 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DM141-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 28.0 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 5.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.5 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.25 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 2.0 t(max) [s] . . . . . . . . . . 20.0 Threshold . . . . . . . . . . . . 40.0 Maximum volume [mL] . . . . . . . 32.0 Evaluation procedure . . . . . . Standard Steepest jump only . . . . . . . Yes Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . Blank Formula . . . . . . . . . . . . . . R=Q Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . mmol Decimal places . . . . . . . . . . . 3 Rinse Auxiliary reagent . . . . . . . . . Water Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes

Method Sample Number samples . . . . . . . . . . . 4 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.74 Upper limit [g] . . . . . . . . . 0.76 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 24.31 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . ZnSO4 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DM141-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 2.0 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 5.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.5 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.25 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 2.0 t(max) [s] . . . . . . . . . . 20.0 Threshold . . . . . . . . . . . . 50.0 Maximum volume [mL] . . . . . . . 20.0 Evaluation procedure . . . . . . Standard Steepest jump only . . . . . . . Yes Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . Magnesium Formula . . . . . . . . . . . . . . R2=((x-Q[2])*C2/m) Constant . . . . . . . . . . . . . . C2=M*10/(z*(100-H20)) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 3 Rinse Auxiliary reagent . . . . . . . . . Water Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R2 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer+Computer All results . . . . . . . . . . . . Yes

126

M171

Solid fat is predominantly used as the main ingredient for rectal and vaginal preparations. It is well toleratedand provides a very good release of the active agent from the base after melting.

1-MonoglycerideM = 358.56 g/mol

Potassium iodide solution RDeionised water RPeriodate acetic acid reagent R:0.446 g sodium periodate in 2.5mL 25% sulphuric acid, diluted to100 mL with acetic acid 98% RCitric acid solution 2%

c(Na2S2O3) = 0.1 mol/L


1. Chemical reactionH2COH-HCOH-H2CO-CO-R + IO4

- →HCO-CH2O-CO-R + H2CO + IO3

- + H2O2. Conproportionation of periodate, iodate andiodide respectively, in an acidic medium to iodine

IO4- + 7I- + 8H+ → 4I2 + 4H20

IO3- + 5I- + 6H+ → 3I2 + 3H20

3. Iodine is reduced to iodide with thiosulphate.I2 + 2S2O3

2- → 2I- + S4O62-

250 mL Glass titration beaker

METTLER TOLEDO


Waste disposal

Ph. Eur. 1997; Monograph "SolidFat"

Sample preparation

Solid Fat, C21H42O4Sample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DM140-SCIndication

Content Determination of 1-Monoglycerides in Solid Fat

Weigh a sample of 9.90 to 10.10 g solid fat anddissolve in 50 mL chloroform. Transfer to aseparating funnel and extract three times with 25 mLcitric acid solution 2% R (m/V).The standard solutions are prepared from theseparated organic phase. Place 25 mL of thesample solution in a 250 mL titration beaker. Add25 mL periodate acetic acid reagent, carefullyswirling, and allow to stand covered for 30 min. Add100 mL deionised water.At the same time, prepare three 250 mL titrationbeakers with 50 mL chloroform and 25 mLperiodate acetic acid solution for a blankdetermination.

The dried and ground residue is used for the contentdetermination. The blank samples are prepared inthe same way as the solid fat samples.

Remarks

R(%) = (x-Q[2])• M•4/(10 •m•4)

Q [2]= Thiosulphate consumption in mmolx = Mean value of the blank determin. in mmolM = Molar mass 1-Monoglyceridem = Sample size in g4 = Factor from the aliquotation of the samplesolution4 = Equivalent number

Calculation

Method for the iodometric determination of 1-Monoglycerides in solid fat

Standard Potassium iodate (M526)

L. Pludra

Author

Structure

127


ET1 0.0000 393.5 0:03 14.2840 376.2 -1.2 0:20 21.4260 366.7 -1.3 0:58

ET2 25.0000 360.1 -1.8 1:05 27.0000 355.2 -2.5 1:10 29.0000 348.6 -3.3 1:15 30.9040 337.7 -5.7 1:21 31.8940 325.7 -12.2 1:26 32.3220 312.3 -31.2 1:31 32.4800 298.8 -85.9 1:36 32.5360 285.5 -237.5 1:43 32.5560 270.3 -759.5 1:50

EQP1 32.5760 215.2 -2750.9 2:16 32.5960 205.2 -504.0 2:24 32.6160 201.2 -199.5 2:28




Method: G008 1-Monoglycerides in fat Date: 21-12-1999 13:49


RESULTS


1/1 990674 25.0 mL R1 = 4.114 mmol Blank

1/2 990674 25.0 mL R1 = 4.114 mmol Blank

1/3 990674 25.0 mL R1 = 4.115 mmol Blank

2/1 990674 10.0284 g R2 = 2.95 % C21H42O4

2/2 990674 10.0034 g R2 = 2.96 % C21H42O4

2/3 990674 10.0937 g R2 = 2.92 % C21H42O4

2/4 990674 9.901299 g R2 = 2.99 % C21H42O4

2/5 990674 10.0746 g R2 = 2.93 % C21H42O4

2/6 990674 10.0134 g R2 = 2.96 % C21H42O4

STATISTICS





STATISTICS





Titration curve

Results

128

Method: G008 1-Monoglycerides in fat Version: 21-12-1999 13:49

Title Method ID . . . . . . . . . . . . . G008 Title . . . . . . . . . . . . . . . 1-Monoglycerides infat Date/time . . . . . . . . . . . . . 21-Dec-1999 13:49 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . Stand 1 Entry type . . . . . . . . . . . . . Fixed volume U Volume [mL] . . . . . . . . . . . 25.0 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 100.0 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 65 Time [s] . . . . . . . . . . . . . . 5 Dispense Titrant . . . . . . . . . . . . . . KJ 16,6% Concentration [mol/L] . . . . . . . 1.0 Volume [mL] . . . . . . . . . . . . 10 Stir Speed [%] . . . . . . . . . . . . . 65 Time [s] . . . . . . . . . . . . . . 30 Titration Titrant . . . . . . . . . . . . . . Na2S2O3 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DM140-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 40.0 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 250.0 Maximum volume [mL] . . . . . . . 50.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . Blank det. Formula . . . . . . . . . . . . . . R1=Q Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . mmol Decimal places . . . . . . . . . . . 3 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes

Method Sample Number samples . . . . . . . . . . . 6 Titration stand . . . . . . . . . . Stand 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 9.9 Upper limit [g] . . . . . . . . . 10.1 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 358.56 Equivalent number z . . . . . . . . 4 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 65 Time [s] . . . . . . . . . . . . . . 5 Dispense Titrant . . . . . . . . . . . . . . KJ 16,6% Concentration [mol/L] . . . . . . . 1.0 Volume [mL] . . . . . . . . . . . . 10 Stir Speed [%] . . . . . . . . . . . . . 65 Time [s] . . . . . . . . . . . . . . 30 Titration Titrant . . . . . . . . . . . . . . Na2S2O3 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DM140-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 25.0 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 2.0 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 250.0 Maximum volume [mL] . . . . . . . 45.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . C21H42O4 Formula . . . . . . . . . . . . . . R2=(x-Q[2])*C*4/m Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R2 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes

129

M172

Glycerol is used as an active ingredient in cases of slow digestion, constipation and increased intracranialpressure. As a medicinal drug aid, it is used as a component for ointments, suppositories, ear drops, liquidsoaps and gels.

GlycerolM = 92.1 g/mol

Deionised water REthylene glycol solution 50% RSodium periodate solution 2.14%

c(NaOH) = 0.1 mol/L


1. Chemical reactionH2COH-HCOH-H2COH + 2IO4

- → HCOOH + 2H2CO+ 2IO3

- + H2O2. The excess of periodate reacts with ethyleneglycole. Formaldehyde is formed.

3. Formic acid (cf. reaction 1) is titrated withsodium hydroxide .

HCOOH + NaOH → NaHCO2 + H2O

Titration beaker ME-101974

METTLER TOLEDO


Waste disposal

Ph. Eur. 1997; Monograph "Glycerol85%"

Sample preparation

Glycerol 85%, C3H8O3Sample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG111-SCIndication

Content Determination of Glycerol 85%

Weigh a sample of 0.09 to 0.11 g glycelrol,accurately to 0.05 mg, in a 150 mL brown glasstitration beaker and add 45 mL deionised water.Then add 25 mL sodium periodate solution 2.14 %(m/V), close the beaker and allow to stand in a darkplace for 15 min. Add 5 mL ethylene glycol solution50 % (m/V) and allow to stand covered in a darkplace for a further 20 minutes.For the blank determination, add all the auxilliaryreagents to the beaker and allow to stand in a darkplace for 20 minutes before titrating.

Remarks

R(%) = (Q[2]-x) • M/(10 •m)

Q = Titrant consumption in mmolx = Mean value of the blank determination inmmolM = Molar mass Glycerolm = Sample size in g

Calculation

Method for the alcalimetric determination of Glycerol


L. Pludra

Author

Structure

130


ET1 0.0000 235.2 0:02 3.4280 204.1 -9.1 0:13 5.1420 188.3 -9.2 0:20

ET2 6.0000 180.5 -9.1 0:25 6.3000 177.6 -9.6 0:29 6.6000 174.7 -9.6 0:32 6.9000 171.4 -11.2 0:35

\\ \\ \\ \\ 10.0550 91.9 -93.7 1:50 10.1430 78.7 -149.5 1:57 10.2010 65.0 -236.5 2:05 10.2520 47.0 -354.1 2:15 10.3030 19.9 -531.2 2:27

EQP1 10.3550 -70.6 -1740.5 2:47 10.4070 -150.8 -1542.7 3:08 10.4590 -169.3 -355.4 3:17




Method: G054 Cont. Glycerol 85% Date: 14-12-1999 8:39


RESULTS


1/1 993061 25.0 mL R1 = 0.00502 mmol Blank

1/2 993061 25.0 mL R1 = 0.00523 mmol Blank

1/3 993061 25.0 mL R1 = 0.00518 mmol Blank

2/1 993061 0.111 g R2 = 85.70 % C3H8O3

2/2 993061 0.1086 g R2 = 85.74 % C3H8O3

2/3 993061 0.1057 g R2 = 85.63 % C3H8O3

2/4 993061 0.1048 g R2 = 85.94 % C3H8O3

2/5 993061 0.1065 g R2 = 85.90 % C3H8O3

2/6 993061 0.0964 g R2 = 85.86 % C3H8O3

STATISTICS





STATISTICS





Titration curve

Results

131

Method: G054 Cont. Glycerol 85% Version: 14-12-1999 8:39

Title Method ID . . . . . . . . . . . . . G054 Title . . . . . . . . . . . . . . . Cont. Glycerol 85% Date/time . . . . . . . . . . . . . 14-Dec-1999 8:39 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . Stand 1 Entry type . . . . . . . . . . . . . Fixed volume U Volume [mL] . . . . . . . . . . . 25.0 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 100.0 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 60 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . NaOH Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG111-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.01 dV(max) [mL] . . . . . . . 0.1 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 150.0 Maximum volume [mL] . . . . . . . 1.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . Blank det. Formula . . . . . . . . . . . . . . R=Q Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . mmol Decimal places . . . . . . . . . . . 5 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes

Method Sample Number samples . . . . . . . . . . . 6 Titration stand . . . . . . . . . . Stand 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.09 Upper limit [g] . . . . . . . . . 0.11 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 92.1 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 65 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . NaOH Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG111-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 6.0 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 12.0 Limits dV . . . . . . . . . . Relative dV(min) [%dosVol] . . . . . 0.5 dV(max) [%buVol] . . . . . 3.0 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 1.0 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 2.0 t(max) [s] . . . . . . . . . . 20.0 Threshold . . . . . . . . . . . . 200.0 Maximum volume [mL] . . . . . . . 20.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . C3H8O3 Formula . . . . . . . . . . . . . . R2=(Q[2]-x)*C2/m Constant . . . . . . . . . . . . . . C2=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R2 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes

132

M173

This is an auxiliary reagent which is used as a water-in-oil emulsifier and is the consistency giving factor inointments and creams. It can also be used as a lubricant in the production of tablets as well as an additivein controlled release preparations.

Glycerol MonostearateM = 358.56 g/mol

Dichloromethane R,Acetic acid 98% RPotassium iodide solution RDeionised water RPeriodate acetic acid reagent R:0.446 g sodium periodate in 2.5 mL 25%sulphuric acid, diluted to 100 mL with acetic acid98% R

c(Na2S2O3) = 0,1 mol/L


1. Chemical reactionH2COH-HCOH-H2CO-CO-R + IO4

- →HCO-CH2O-CO-R + H2CO + IO3


IIO4- + 7I- + 8H+ → 4I2 + 4H20

IO3- + 5I- + 6H+ → 3I2 + 3H20


2- → 2I- + S4O62-


METTLER TOLEDO


Waste disposal


Sample preparation

Glycerol Monostearate, C21H42O4Sample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DM140-SCIndication

Content Determination of Glycerol Monostearate 40-50%

Weigh a sample of 0.390 to 0.410 g glycerolmonostereate and dissolve in 50 mL dichloro-methane. Separate in a separating funnel with 25mL deionised water. Repeat a further three times. Ifan emulsion begins to form, add a few drops ofacetic acid 98%.Collect the water phase for the determination of freeglycerol.Filter the organic phase through cottonwool into a100 ml volumetric flask and fill up to the mark withdichloromethane. Take 50 mL of this solution andtransfer into a 250 mL titration beaker. Add 25 mLperiodate acetic acid reagent, swirling carefully.Cover the beaker and allow to stand for 30 minutes.Finally add 100 mL deionised water.

The samples for the determination of free glyceroland the content determination are prepared at thesame time. For the blank determination measure 50mL dichloromethane and 25 mL periodate aceticacid reagent, and prepare in exactly the samemanner as for the content determination.

Remarks

R(%) = (x-Q[2])• M•2/(10 •m•2)

Q [2]= Thiosulphate consumption in mmolx = Mean value of the blank determin. in mmolM = Molar mass Glycerol Monostearatem = Sample size in g2 = Factor from the aliquotation of the samplesolution2 = Equivalent number

Calculation

Method for the iodometric determination of Glycerol Monostearate


L. Pludra

Author

Structure

133


ET1 0 398,6 320 377,4 -1,1 27

ET2 30 364,5 -1,3 68// // // //38 354,7 -2 7638,5 353,6 -2,2 8039 352,2 -2,8 8439,5 350,7 -2,9 8840 348,9 -3,5 9140,5 346,9 -4,1 9541 344,6 -4,6 9941,5 341,9 -5,5 10342 338,7 -6,4 10742,5 334,4 -8,5 11143 328 -12,7 11543,472 317,5 -22,2 14743,722 303,4 -56,6 15243,81 289,7 -155,9 15743,84 277,4 -408,3 161

EQP1 43,86 232,3 -2253,9 18243,88 218 -717,6 19443,9 211,4 -329 204




Method: G006 Glycerol monostearate 40-50% Date: 15-12-1999 13:56


RESULTS


1/1 993268 25.0 mL R1 = 4.164 mmol Blank

1/2 993268 25.0 mL R1 = 4.169 mmol Blank

1/3 993268 25.0 mL R1 = 4.161 mmol Blank

2/1 993268 0.3945 g R2 = 35.64 % C21H42O4

2/2 993268 0.3993 g R2 = 34.42 % C21H42O4

2/3 993268 0.4060 g R2 = 35.03 % C21H42O4

2/4 993268 0.3970 g R2 = 34.67 % C21H42O4

2/5 993268 0.3943 g R2 = 35.49 % C21H42O4

2/6 993268 0.3944 g R2 = 32.82 % C21H42O4

STATISTICS





STATISTICS





Titration curve

Results

134

Method: G006 Glycerol monostearate 40-50% Version: 15-12-1999 13:56

Title Method ID . . . . . . . . . . . . . G006 Title . . . . . . . . . . . . . Glycerol monostearate40-50% Date/time . . . . . . . . . . . . . 15-Dec-1999 13:56 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . Stand 1 Entry type . . . . . . . . . . . . . Fixed volume U Volume [mL] . . . . . . . . . . . 25.0 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 100.0 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 75 Time [s] . . . . . . . . . . . . . . 10 Dispense Titrant . . . . . . . . . . . . . . KJ 16,6% Concentration [mol/L] . . . . . . . 1.0 Volume [mL] . . . . . . . . . . . . 12 Stir Speed [%] . . . . . . . . . . . . . 75 Time [s] . . . . . . . . . . . . . . 60 Titration Titrant . . . . . . . . . . . . . . Na2S2O3 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DM140-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 30 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 250.0 Maximum volume [mL] . . . . . . . 55.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . Blank det. Formula . . . . . . . . . . . . . . R1=Q Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . mmol Decimal places . . . . . . . . . . . 3 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes

Method Sample Number samples . . . . . . . . . . . 6 Titration stand . . . . . . . . . . Stand 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.39 Upper limit [g] . . . . . . . . . 0.41 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 358.56 Equivalent number z . . . . . . . . 2 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 75 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . Na2S2O3 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DM140-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 30 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.5 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 250.0 Maximum volume [mL] . . . . . . . 60.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . C21H42O4 Formula . . . . . . . . . . . . . . R2=(x-Q[2])*C*2/m Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R2 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes

135

M174

This is an auxiliary reagent which is used as a water-in-oil emulsifier and is the consistency giving factor inointments and creams. It can also be used as a lubricant in the production of tablets as well as an additivein controlled release preparations.

GlycerolM = 92.09 g/mol

Deionised water RPotassium iodide solution RPeriodate acetic acid reagent R

c(Na2S2O3) = 0.1 mol/L


1. Chemical ReactionH2COH-HCOH-H2COH + 2IO4

- → HCOOH + 2H2CO+ 2IO3


IO4- + 7I- + 8H+ → 4I2 + 4H20

IO3- + 5I- + 6H+ → 3I2 + 3H20


2- → 2I- + S4O62-


METTLER TOLEDO


Waste disposal


Sample preparation

Glycerol MonostearateSample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DM140-SCIndication

Content Determination of Free Glycerol in Glycerol Monostearate 40-50%

Filter the water phase previously collected in thecontent determination of glycerol monostearate40-50%, through a pleated filter into a 100 mLvolumetric flask. Rinse the filter with 5 mL deionisedwater and fill the flask up to the mark. Pipette 50 mLof the sample solution into a 250 mL titrationbeaker. Add 25 mL periodate acetic acid reagent,swirling carefully. Cover the beaker and allow tostand for 30 minutes. Add 100 mL deionised water.

The samples for the determination of free glyceroland the content determination are prepared at thesame time. For the blank determination measure 50mL dichloromethane and 25 mL periodate aceticacid reagent, and prepare in exactly the samemanner as for the content determination.

Remarks

R(%) = (x-Q[2])• M•2/(10 •m•4)

Q [2]= Thiosulphate consumption in mmolx = Mean value of the blank determin. in mmolM = Molar mass Glycerol Monostearatem = Sample size in g2 = Factor from the aliquotation of the samplesolution4 = Equivalent number

Calculation

Method for the determination of free glycerol in Glycerol Monostearate


L. Pludra

Author

Structure

136


ET1 0 398,6 320 377,4 -1,1 2730 364,5 -1,3 68

ET2 35 354,7 -2 7635,5 353,6 -2,2 8036 352,2 -2,8 8436,5 350,7 -2,9 8837 348,9 -3,5 9137,5 346,9 -4,1 9538 344,6 -4,6 9938,5 341,9 -5,5 10339 338,7 -6,4 10739,5 334,4 -8,5 11140 328 -12,7 11540,472 317,5 -22,2 14740,722 303,4 -56,6 15240,81 289,7 -155,9 15740,84 277,4 -408,3 161

EQP1 40,86 232,3 -2253,9 18240,88 218 -717,6 19440,9 211,4 -329 204



Onkel Tuka Quality Control Laboratory

Method: G007 Cont. free Glycerol Date: 15-12-1999 15:03


RESULTS


1/1 993268 25.0 mL R1 = 4.138 mmol Blank

1/2 993268 25.0 mL R1 = 4.138 mmol Blank

1/3 993268 25.0 mL R1 = 4.137 mmol Blank

2/1 993268 0.3945 g R2 = 3.44 % C3H8O3

2/2 993268 0.3993 g R2 = 3.67 % C3H8O3

2/3 993268 0.4060 g R2 = 3.38 % C3H8O3

2/4 993268 0.3970 g R2 = 3.59 % C3H8O3

2/5 993268 0.3943 g R2 = 3.58 % C3H8O3

2/6 993268 0.3944 g R2 = 3.67 % C3H8O3

STATISTICS





STATISTICS





Titration curve

Results

137

Method: G007 Cont. free Glycerol Version: 15-12-1999 15:03

Title Method ID . . . . . . . . . . . . . G007 Title . . . . . . . . . . . . . . . Cont. free Glycerol Date/time . . . . . . . . . . . . . 15-Dec-1999 15:03 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . Stand 1 Entry type . . . . . . . . . . . . . Fixed volume U Volume [mL] . . . . . . . . . . . 25.0 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 100.0 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 75 Time [s] . . . . . . . . . . . . . . 10 Dispense Titrant . . . . . . . . . . . . . . KJ 16,6% Concentration [mol/L] . . . . . . . 1.0 Volume [mL] . . . . . . . . . . . . 12 Stir Speed [%] . . . . . . . . . . . . . 75 Time [s] . . . . . . . . . . . . . . 60 Titration Titrant . . . . . . . . . . . . . . Na2S2O3 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DM140-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 35 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.5 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 250.0 Maximum volume [mL] . . . . . . . 45.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . Blank det. Formula . . . . . . . . . . . . . . R1=Q Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . mmol Decimal places . . . . . . . . . . . 3 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes

Method Sample Number samples . . . . . . . . . . . 6 Titration stand . . . . . . . . . . Stand 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.39 Upper limit [g] . . . . . . . . . 0.41 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 92.09 Equivalent number z . . . . . . . . 4 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 75 Time [s] . . . . . . . . . . . . . . 10 Dispense Titrant . . . . . . . . . . . . . . KJ 16,6% Concentration [mol/L] . . . . . . . 1.0 Volume [mL] . . . . . . . . . . . . 12 Stir Speed [%] . . . . . . . . . . . . . 75 Time [s] . . . . . . . . . . . . . . 30 Titration Titrant . . . . . . . . . . . . . . Na2S2O3 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DM140-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 25 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.5 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 250.0 Maximum volume [mL] . . . . . . . 45.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . C3H8O3 Formula . . . . . . . . . . . . . . R2=(x-Q[2])*C*2/m Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R2 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes

138

M175

In emergency medicine, Na2-EDTA allows a fast reduction of the blood plasma calcium level, such as in thecase of hypercalceamia. It is also widely used to treat eye injuries from lime water and kidney stones.

Na2-EDTA-DihydrateM=372.2 g/mol

Hydrochloric acid 7% RXylenol orange trituration RMetheneamine solution 40 % (m/V)RDeionised water


METTLER TOLEDO DL77/DL70ES

The content of Na2-EDTA isdetermined by a complexometrictitration of zinc sulphate usingxylenol orange for photometricdetection.


METTLER TOLEDO


Waste disposal

Ph. Eur. 1997; Monograph "EdetateDisodium"

Sample preparation

Na2-EDTA, C10H14N2Na2O8Sample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DP550Indication

Content Determination of Ethylenediamine Disodiumacetate (Na2-EDTA)

Weigh a sample of 0.490 to 0.510 g Na2-EDTA,accurately to 0.1 mg, into a titration beaker anddissolve in 40 mL deionised water. Addapproximately 50 mg xylenol orange trituration, 5mL metheneamine solution 40% (m/V) and 2 mLhydrochloric acid 7%.

If the titration is performed on the sample changer, abeaker with deionised water must be placed on thetitration stand. Once the method has been started,the probe must be dipped into it and the potential setto 1000 ± 5 mV within 30 seconds.

Remarks

R(%) = (QDISP+Q)• M•/(10 •m)

QDISP = Total amount of dispensed Zinc Sulphatein mmolQ = Titrant consumption in mmolM = Molar mass Na2-EDTAm = Sample size in g

Calculation

Method for the photometric content determination of Ethylenediamine Disodiumacetate

Standard EDTA-Dihydrate (M539)

L. Pludra

Author

Structure

139


ET1 0.0000 324.9 0:32 8.5700 311.8 -1.5 0:42 12.8540 296.4 -3.6 0:46

ET2 15.0000 235.6 -28.3 1:19 15.1500 233.7 -12.6 1:34 15.3300 232.4 -7.4 1:55 15.5300 231.8 -2.8 2:20 15.7300 230.9 -4.6 2:48 15.9300 232.1 6.0 3:19 16.1300 233.7 8.1 3:49 16.3300 234.7 4.9 4:20 16.5300 237.9 16.1 4:50 16.7300 240.3 11.9 5:21 16.9300 244.6 21.7 5:52

EQP1 17.1300 331.2 432.9 5:59 17.1400 332.2 98.0 6:04 17.1500 333.1 84.0 6:08




Method: G005 Cont. Sodium edetate Date: 02-12-1999 13:05


RESULTS


1/1 990783 0.5028 g R1 = 99.71 % Na-EDTA.2H2O

1/2 990783 0.5068 g R1 = 99.66 % Na-EDTA.2H2O

1/3 990783 0.5001 g R1 = 99.60 % Na-EDTA.2H2O

1/4 990783 0.4939 g R1 = 99.68 % Na-EDTA.2H2O

1/5 990783 0.5006 g R1 = 99.70 % Na-EDTA.2H2O

1/6 990783 0.4957 g R1 = 99.73 % Na-EDTA.2H2O

STATISTICS


Mean value x = 99.68 % Na-EDTA.2H2O

Standard deviation s = 0.045276 % Na-EDTA.2H2O


Titration curve

Results

140

Method: G005 Cont. Sodium edetate Version: 02-12-1999 13:05

Title Method ID . . . . . . . . . . . . . G005 Title . . . . . . . . . . . . . . . Cont. Sodium edetate Date/time . . . . . . . . . . . . . 02-Dec-1999 13:05 Instruction Attach titration beaker containing 60 mL deion. water to the Rondo60 or titration stand 1! Instruction Set the sensor to a value of 1000 +- 5 mV within 30 s. Sample Number samples . . . . . . . . . . . 1 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Fixed volume U Volume [mL] . . . . . . . . . . . 50.0 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 100.0 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 65 Time [s] . . . . . . . . . . . . . . 1 Measure Sensor . . . . . . . . . . . . . . . DP550 Unit of meas. . . . . . . . . . . . mV dE [mV] . . . . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . . . . 1.0 t(min) mode . . . . . . . . . . . . Fix t(min) [s] . . . . . . . . . . . 30.0 t(max) [s] . . . . . . . . . . . . . 30.0 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.49 Upper limit [g] . . . . . . . . . 0.51 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 372.2 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 65 Time [s] . . . . . . . . . . . . . . 1 Dispense Titrant . . . . . . . . . . . . . . ZnSO4 Concentration [mol/L] . . . . . . . 0.1 Volume [mL] . . . . . . . . . . . . 12 Stir Speed [%] . . . . . . . . . . . . . 65 Time [s] . . . . . . . . . . . . . . 1 Titration Titrant . . . . . . . . . . . . . . ZnSO4 Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DP550 Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 4.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.01 dV(max) [mL] . . . . . . . 0.1 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 2.0 dt [s] . . . . . . . . . . . . 2.0 t(min) [s] . . . . . . . . . . 15.0 t(max) [s] . . . . . . . . . . 120.0 Threshold . . . . . . . . . . . . 2000.0 Maximum volume [mL] . . . . . . . 5.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Rinse Auxiliary reagent . . . . . . . . . Water Volume [mL] . . . . . . . . . . . . 20.0 Calculation Result name . . . . . . . . . . . . Na-EDTA*2H2O Formula . . . . . . . . . . . . . . R=(Q+QDISP)*C/m Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes

Method

141

M176

Ibuprofen is an anti-inflammatory and fever reducing agent whose potency in vivo is approximately 2.5 to 3times stronger than acetylsalisylic acid. As an anti-rheumatic, it also has the fewest side-effects compared toother non-steroidal anti-rheumatics.

IbuprofenM=206.3 g/mol

50 mL Methanol

c(NaOH) = 0,1 mol/L


Deprotonation of the carboxylgroups



METTLER TOLEDO


Waste disposal

Ph. Eur. 1997, Suppl. 2000Monograph "Ibuprofen"

Sample preparation

Ibuprofen, C13H18O2Sample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG111-SCIndication

Content Determination of Ibuprofen

Weigh a sample of 0.170 to 0.190 g Ibuprofen,accurately to 0.1 mg, into a titration beaker. Add50 mL Methanol R and dissolve.

The previously determined loss on drying content issaved as the auxilliary value H20. According to Ph.Eur. 1997, a blank titration must be performed witheach 50 mL methanol R.

Remarks

R(%) = ((Q[2]-x) • M/(10 •m)) + H20

Q = Titrant consumption in mmolx = Mean value of the blank determination inmmolM = Molar mass Ibuprofenm = Sample size in gH20 = % Loss on drying of Ibuprofen

Calculation

Method for the alkalimetric determination of Ibuprofen

Standard Potassium Hydrogen Phthalate(M521)

L. Pludra

Author

Structure

142


ET1 0.0000 162.3 0:19 4.0000 26.2 -34.0 0:33 6.0000 8.8 -8.7 0:42

ET2 7.0000 -4.2 -13.0 0:49 7.1000 -5.7 -15.4 0:52 7.2000 -7.6 -18.9 0:55 7.3000 -9.4 -17.5 0:57 7.4000 -11.7 -23.1 1:00 7.5000 -14.2 -25.2 1:03 7.6000 -16.8 -25.9 1:07 7.7000 -20.0 -31.5 1:11 7.8000 -23.6 -36.4 1:15 7.9000 -28.1 -44.8 1:20 8.0000 -33.5 -53.9 1:24 8.1000 -40.3 -68.6 1:30 8.2000 -50.6 -102.9 1:35 8.2870 -65.0 -165.7 1:42 8.3390 -79.8 -284.0 1:49 8.3680 -94.0 -490.0 1:55 8.3850 -106.1 -712.3 2:02 8.3970 -118.3 -1015.0 2:09

EQP1 8.4070 -132.8 -1449.1 2:18 8.4170 -143.8 -1106.0 2:25 8.4320 -158.1 -947.3 2:32




Method: G060 Cont. Ibuprofen Date: 11-11-1999 14:08


RESULTS


1/1 50.0 mL R1 = 0.005 mmol Blank

1/2 50.0 mL R1 = 0.09 mmol Blank

1/3 50.0 mL R1 = 0.005 mmol Blank

2/1 0.1734 g R2 = 99.81 % C13H18O2

2/2 0.1773 g R2 = 99.79 % C13H18O2

2/3 0.1815 g R2 = 99.67 % C13H18O2

2/4 0.1752 g R2 = 99.90 % C13H18O2

2/5 0.1728 g R2 = 99.86 % C13H18O2

2/6 0.1847 g R2 = 99.95 % C13H18O2

STATISTICS





STATISTICS




Rel. standard deviation rel = 0.097 %

Titration curve

Results

143

Method: G060 Cont. Ibuprufen Version: 11-11-1999 14:08

Title Method ID . . . . . . . . . . . . . G060 Title . . . . . . . . . . . . . . . Cont. Ibuprufen Date/time . . . . . . . . . . . . . 11-Nov-1999 14:08 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Fixed volume U Volume [mL] . . . . . . . . . . . 50.0 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 100.0 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . NaOH Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG111-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.01 dV(max) [mL] . . . . . . . 0.1 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 10.0 Maximum volume [mL] . . . . . . . 1.0 Evaluation procedure . . . . . . Standard Steepest jump only . . . . . . . Yes Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . Blank Formula . . . . . . . . . . . . . . R1=Q Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . mmol Decimal places . . . . . . . . . . . 3 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Rinse Auxiliary reagent . . . . . . . . . Methanol Volume [mL] . . . . . . . . . . . . 10.0 Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes

Method Sample Number samples . . . . . . . . . . . 4 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.17 Upper limit [g] . . . . . . . . . 0.19 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 206.3 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . NaOH Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG111-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 7.0 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 12.0 Limits dV . . . . . . . . . . Relative dV(min) [%dosVol] . . . . .0.5 dV(max) [%buVol] . . . . . 2.5 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 1.0 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 2.0 t(max) [s] . . . . . . . . . . 20.0 Threshold . . . . . . . . . . . . 200.0 Maximum volume [mL] . . . . . . . 10.0 Evaluation procedure . . . . . . Standard Steepest jump only . . . . . . . Yes Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . C13H8O2 Formula . . . . . . . . . . . . . . R2=((Q[2]-x)*C2/m)+H20 Constant . . . . . . . . . . . . . . C2=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Rinse Auxiliary reagent . . . . . . . . . Methanol Volume [mL] . . . . . . . . . . . . 20.0 Statistics Ri (i=index) . . . . . . . . . . . . R2 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer+Computer All results . . . . . . . . . . . . Yes

144

M177

Sodium hydroxide is used as a neutralising agent in the production process.

Sodium HydroxideM = 40.0 g/mol

Deionised water R

c(HCl) = 0.5 mol/l


1. Equivalence pointNaOH + HCl → NaCl + H2ONa2CO3 + HCl → NaHCO3 + NaCl + H2O

2. Equivalence pointNaHCO3 + HCl → NaCl + CO2 + H2O


METTLER TOLEDO


Waste disposal

Ph. Eur. 1997; Monograph "SodiumHydroxide"

Sample preparation

Sodium HydroxideSample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DG111-SCIndication

Total Alkali and Carbonate Content of Sodium Hydroxide

Weigh a sample of 0.90 to 1.100 g SodiumHydroxide, accurately to 0.1 mg, into a 100 mLtitration beaker. Add 40 mL deionised water anddissolve.

The titration should ideally show only oneequivalence point for the total alkali content,however, a second equivalence point may arise froma carbonate impurity. According to thepharmacopoeia, this content has to be determinedtogether with the total alkali content.

Remarks

R1(%) = (Q1 +Q2)• M/(10 •m)

Q1 = Titrant consumption to the first EQPM = Molar mass Sodium Hydroxidem = Sample size in g

R2(%) = Q2• 105.98/(10 •m)Q2 = Titrant consumption to the second EQP105.98 = Molar mass Sodium Carbonate

Calculation

Method for the acidimetric determination of the total alkali and carbonate content in Sodium Hydroxide

Standard THAM Tris-hydroxymethylaminomethane (vgl. Appl. M524)

L. Pludra

Author

Structure

145


ET1 0.0000 -399.4 0:03 17.1420 -387.7 0.7 1:11 25.7130 -378.6 1.1 2:01

ET2 30.0000 -373.3 1.2 2:13 30.5000 -372.0 2.7 2:46 31.0000 -371.3 1.3 2:51 // // // // 53.4190 -199.6 470.9 7:43 53.4390 -189.3 511.0 7:48 53.4590 -175.4 696.5 7:56 53.4790 -152.5 1148.0 8:08

EQP1 53.4990 -109.1 2166.8 8:33 53.5190 -99.4 486.5 8:38 53.5390 -85.5 696.5 8:43 53.5590 -26.9 2925.9 9:13

EQP2 53.5790 81.5 5421.3 9:44 53.5990 147.7 3310.9 9:59 53.6190 165.4 885.5 10:04 53.6390 177.1 584.5 10:09 // // // //




Method: G094 Total alkaline cont. Date: 20-12-1999 10:31


RESULTS


1/1 961124 0.9839 g R1 = 99.26 % Total alkali

R2 = 0.00 % Na2CO3

1/2 961124 1.0825 g R1 = 99.44 % Total alkali

R2 = 0.44 % Na2CO3

1/3 961124 0.9555 g R1 = 98.51 % Total alkali

R2 = 0.63 % Na2CO3

1/4 961124 1.0508 g R1 = 99.25 % Total alkali

R2 = 0.52 % Na2CO3

1/5 961124 0.9975 g R1 = 98.47 % Total alkali

R2 = 0.47 % Na2CO3

1/6 961124 1.0675 g R1 = 99.13 % Total alkali

R2 = 0.46 % Na2CO3

STATISTICS


Mean value x = 99.01 % Total alkali

Standard deviation s = 0.413723 % Total alkali


STATISTICS


Mean value x = 0.42 % Na2CO3

Standard deviation s = 0.216639 % Na2CO3


Titration curve

Results

146

Method: G094 Total alkaline cont.

Version: 20-12-1999 10:31

Title Method ID . . . . . . . . . . . . . G094 Title . . . . . . . . . . . . . . . Total alkaline cont. Date/time . . . . . . . . . . . . . 18-Mai-1999 16:30 Sample Number samples . . . . . . . . . . . 4 Titration stand . . . . . . . . . . ST20 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.9 Upper limit [g] . . . . . . . . . 1.1 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 40 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 30 Titration Titrant . . . . . . . . . . . . . . HCl Concentration [mol/L] . . . . . . . 0.5 Sensor . . . . . . . . . . . . . . . DG111-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 30 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.5 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 1.0 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . .300.0 Maximum volume [mL] . . . . . . . 55.0 Evaluation procedure . . . . . . Standard Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Result name . . . . . . . . . . . . Total alkali Formula . . . . . . . . . . . . . . R1=(Q1+Q2)*C/m Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Calculation Result name . . . . . . . . . . . . Na2CO3 Formula . . . . . . . . . . . . . . R2=Q2*C2/m Constant . . . . . . . . . . . . . . C2=10.598 Result unit . . . . . . . . . . . . % Decimal places . . . . . . . . . . . 2 Rinse Auxiliary reagent . . . . . . . . . Water Volume [mL] . . . . . . . . . . . . 20.0 Record Output unit . . . . . . . . . . . . Computer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R2 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Record Output unit . . . . . . . . . . . . Printer+Computer All results . . . . . . . . . . . . Yes

Method

147

M178

2-Aminophenol is a starting material used in the production of pharmaceuticals, hair dyes, andazo-dyestuffs. It is also used as a photographic developer, antioxidant, and as a polymerization inhibitor forunsaturated bonds.

2-AminophenolM = 109,13 g/mol

20% HBrDeionised water

c(NaNO2) = 0.2 mol/L

METTLER TOLEDO DL70ES/DL77METTLER TOLEDODL58/55/53/DL50Graphix

Under acidic conditions, nitrousacid is added to the aminophenol,which is converted to a diazoniumsalt.

R-NH2 + HNO2 + HBr →[R-N≡N+]Br- + 2H2O

Titration beaker ME-10197

METTLER TOLEDO

Neutralize to break up the diazonium salt.Never allow the diazonium salt to dry- explosive!

Waste disposal

Sample preparation

2-Aminophenol C6H7NOSample

Substance

Chemicals

Titrant

Instruments

Results

Literature

Chemistry

Accessories

DM 140-SCIndication

Content Determination of 2-Aminophenol

0.16 to 0.20 g of 2-Aminophenol is weighed into abeaker. 20 mL of deionised water and 10 mL of20% HBr are added.

The maximum volume titrant added is kept small,and no predispense is used. If too much nitrous acidis added at once, it decomposes before any reactionwith 2-aminophenol. HCl can be used instead ofHBr, but this reaction is slower and must be done atlow temperature (typically 4°C).

Remarks

R(%) = (Q • M)/ 10• m

Q = titrant consumption in mmolm = sample size in gM = molar mass 2-Aminophenol

Calculation

Method for the determination of 2-Aminophenol content by diazotization

Standard Sulfanilic Acid (M544)

M. Biber

Author

Structure

148


ET1 0.0000 340.5 0:03 0.0200 349.0 423.3 0:07 0.0400 357.7 436.2 0:10

0.0600 364.9 358.6 0:13 0.0880 377.4 447.4 0:17 0.1080 386.8 465.3 0:20 0.1280 388.3 77.5 0:34 0.1480 387.8 -25.8 0:47 0.1880 389.2 35.5 1:02 0.2680 392.3 38.8 1:18 0.4580 397.5 26.5 1:28 0.6580 400.1 13.9 1:58 0.8580 402.4 11.3 2:16 1.0580 403.4 5.2 2:35

1.2580 404.7 6.5 2:53 // // // // 8.0540 478.4 81.0 17:04

8.1420 494.9 187.3 17:35 8.1690 491.3 -131.6 18:06 8.2230 516.2 460.7 18:36 8.2430 517.6 71.1 19:07 8.2630 533.2 781.9 19:37

EQP1 8.2830 585.8 2630.0 20:07 8.3030 637.2 2568.7 20:18 8.3239 656.5 966.1 20:23


METTLER DL58 Titrator V3.1 Mettler Toledo GmbH Analytical

Market Support Laboratory

Method: 747 Cont. 2Aminophenol Date: 08-08-2000 8:21

User: MB Measured: 08-08-2000 8:21

RESULTS


1/1 2Aminophen 0.171 g R1 = 98.929 % C6H7NO






STATISTICS


Mean value x = 98.448 % C6H7NO

Standard deviation s = 0.0591069 % C6H7NO


Titration curve

Results

149

Methode: 747 Cont. 2Aminophenol Version: 8-8-2000 8;21

Title Method ID . . . . . . . . . . . . . 747 Title . . . . . . . . . . . . . . . Cont. 2Aminophenol Date/time . . . . . . . . . . . . . 08/08/2000 8:21 Sample Sample ID . . . . . . . . . . . . . 2Aminophen Entry type . . . . . . . . . . . . . Weight Lower limit [g] . . . . . . . . . 0.15 Upper limit [g] . . . . . . . . . 0.35 Molar mass M . . . . . . . . . . . . 109.13 Equivalent number z . . . . . . . . 1 Titration stand . . . . . . . . . . Stand 1 Temperature sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 45 Time [s] . . . . . . . . . . . . . . 30 EQP titration Titrant/Sensor Titrant . . . . . . . . . . . . . NaNO2 Concentration [mol/L] . . . . . . 0.2 Sensor . . . . . . . . . . . . . DM140 Unit of meas. . . . . . . . . . . mV Predispensing . . . . . . . . . . . No Titrant addition . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . 8.0 dV(min) [mL] . . . . . . . . . . 0.02 dV(max) [mL] . . . . . . . . . . 0.2 Measure mode . . . . . . . . . . . . Equilibrium controlled dE [mV] . . . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . . 30.0 Recognition Threshold . . . . . . . . . . . . 500.0 Steepest jump only . . . . . . . Yes Range . . . . . . . . . . . . . . Yes Limit A [mV,pH,...] . . . . . 400 Limit B [mV,pH,...] . . . . . 800 Tendency . . . . . . . . . . . . None Termination at maximum volume [mL] . . . . . 20.0 at potential . . . . . . . . . . No at slope . . . . . . . . . . . . No after number EQPs . . . . . . . . Yes n = . . . . . . . . . . . . . 1 comb. termination conditions . . No Evaluation Procedure . . . . . . . . . . . . Standard Potential 1 . . . . . . . . . . . No Potential 2 . . . . . . . . . . . No Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Formula . . . . . . . . . . . . . . R=Q*C/m Constant . . . . . . . . . . . . . . C=M/(10*z) Decimal places . . . . . . . . . . . 3 Result unit . . . . . . . . . . . . % Result name . . . . . . . . . . . . Statistics . . . . . . . . . . . . . Yes Report Output . . . . . . . . . . . . . . . Computer Results . . . . . . . . . . . . . . Yes All results . . . . . . . . . . . . Yes Raw results . . . . . . . . . . . . No Table of measured values . . . . . . Yes Sample data . . . . . . . . . . . . No E - V curve . . . . . . . . . . . . Yes dE/dV - V curve . . . . . . . . . . No d2E/dV2 - V curve . . . . . . . . . No log dE/dV - V curve . . . . . . . . No E - t curve . . . . . . . . . . . . No V - t curve . . . . . . . . . . . . No dV/dt - t curve . . . . . . . . . . No

Method

150

The methods in this brochure represent selected, possible application examples. These have been tested with allpossible care with the analytical instruments mentioned in the brochure. The experiments were conducted and theresulting data evaluated based on our current state of knowledge.

However, the applications do not absolve you from personally testing their suitability for your intended methods,instruments and purposes. As the use and transfer of an application example are beyond our control, we cannotaccept responsibility therefore.

When chemicals and solvents are used, the general safety rules and the directions of the manufacturer mustbe observed.

Mettler-Toledo GmbHAnalyticalCH-8603 Schwerzenbach, SwitzerlandTelefon (01) 806 77 11, Fax (01) 806 73 50Internet: http://www.mt.com

Subject to technical changes© 09/04 Mettler-Toledo GmbH, ME-51710071Printed in Switzerland on 100% chlorine-freepaper, for the sake of our environment.

For all other countries:Mettler-Toledo GmbHPO Box, VI-400, CH-8606 Greifensee, SwitzerlandTel. (01) 944 22 11, Fax (01) 944 31 70

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