Disclosure to Promote the Right To Information

Whereas the Parliament of India has set out to provide a practical regime of right to information for citizens to secure access to information under the control of public authorities, in order to promote transparency and accountability in the working of every public authority, and whereas the attached publication of the Bureau of Indian Standards is of particular interest to the public, particularly disadvantaged communities and those engaged in the pursuit of education and knowledge, the attached public safety standard is made available to promote the timely dissemination of this information in an accurate manner to the public.

इंटरनेट मानक

“!ान $ एक न' भारत का +नम-ण”Satyanarayan Gangaram Pitroda

“Invent a New India Using Knowledge”

“प0रा1 को छोड न' 5 तरफ”Jawaharlal Nehru

“Step Out From the Old to the New”

“जान1 का अ+धकार, जी1 का अ+धकार”Mazdoor Kisan Shakti Sangathan

“The Right to Information, The Right to Live”

“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता है”Bhartṛhari—Nītiśatakam

“Knowledge is such a treasure which cannot be stolen”

“Invent a New India Using Knowledge”

है”ह”ह

IS 874 (1992): Dextrose monohydrate [FAD 2: Sugar Industry]

IS 874: 1882

itfij~~ ¥i1;f)~I~e - fqfWfisc( ~T ~;r-er~ )Indian Standard

DEXTROSE MONOHYDRATE - SPECIFICATION( Third Revision )

UDC 664'162

e SIS 1992

BUREAU OF INDIAN STANDARDSMANAK BHAl'AN t 9 BAHADUR SHAH ZAPAR. MAR.G

NEW DELHI 110002

A.l'rlI1992 Price Gro-, 5

xxxxxx2008

AMENDMENT NO. 1 JULY 2002TO

IS 874: 1992 DEXTROSE MONOHYDRATE ­SPECIFICATION

(Third Revision)

( Page 2, clause 5.2.2 ) - Substitute the following for the existmg clause

• 5.2.2 BIS Certtficanon Markmg

The product may also be marked With the Standard Mark

5.2.2.1 The use of the Standard Mark IS governed by the provisrons of Bureau ofIndian Standards Act. 1986 and the Rules and Regulations made thereunder Thedetails of condrtions under which the licence for the use of Standard Mark maybe granted to manufacturers or producers. may be obtained from the Bureau ofIndian Standards t

(FAD 2)Reprography VOlt 81~ New Delhi India

AMENDMENT NO. 2 JUNE 2011 TO

IS 874 : 1992 DEXTROSE MONOHYDRATE ― SPECIFICATION

(Third Revision) [Page 2, clause 5.2.1(e)] — Substitute ‘Net quantity’ for ‘Net mass’. [Page 2, clause 5.2.1(f)] — Substitute the following for the existing:

‘Any other requirements as given under the Standards of Weights and Measures (Packaged Commodities) Rules, 1977 and the Prevention of Food Adulteration Act, 1955 and the Rules framed thereunder.’

(FAD 2)

Reprography Unit, BIS, New Delhi, Indi

Edible Starches and Starch Products Secuonal Committee, FADe 17

FOREWORD

Th« Indian Standard ( Third Revision ) was adopted by the Bureau of Indian Standards, after thedraft finalized by the Edible Starches and Starch Products Sectional Committee had beenapproved by the Food and Agriculture DIVISIon Council

ThIS standard was first published In 19~6 Its first revision was brought out In 1965 In which thehmit for «JrM me "as charged, the hmits for lead and copper substituted for heavy metals andthe requiremer ts for chloride, sulphates, less soluble sugars, solubrhty and dextrms deleted

In this revisron addinonal requirement for PUrity, specific volume, total solids content and othermetallic rmpuntres, namely, tm, ZInc,mercury ard cadmrum have been Included

ThIS standard covers requirements for dextrose monohydrate SUItable for use 10 the foodprocessing Industry The requirements for dextrose monohydrate used for pharmaceutrcal purposesare stipulated In the ( lP ) Indian Pharmacopoeia and are, therefore, not covered In the provisionsof thrs specrficatron,

In the preparation of this standard due consideratron has been given to the provisrons of thePrevention of Food Adulteranons Act, 1954 and the Rules framed thereunder and the Standards ofWel~hts and Measures (Packaged Commodnres ) Rules, 1977 However, this standard IS subjectto the restricnons Imposed under these, wherever, applicable

For the purpose of decidmg whether a particular requirement of this standard IS complied WIth.the fin ..JI value, observed or calculated, expressing the result of a test or analysis, shall be roundedoff In accordance w th IS 2 1960 'Rules for rounding off numerical values ( revised )'. Thenumber of sigrnficant places retained In the rounded off value should be the same as that of thespecified value ID this standard

IS 874: 1992

Indian Standard

DEXTROSE MONOHYDRATE - SPECIFICATION( Third Revision)

1 SCOPE

1.1 This standard prescribes the requirementsand the methods of samphng and test fordextrose monohydrate SUitable for use In thefood processing Industry.

1.2 This standard does not apply to dextrosemonohydrate meant for pharmaceuticalpurposes.2, REFERENCESThe Indian Standards hsted In Annex A arenecessary adjuncts to this standard

3 TERMINOLOGY3.0 For the purpose of this standard, thefollowing definitions shall apply.

3.1 Dextrose Monohydrate

A dextro-rotatory monosacchande having theformula C.H lIO. H10.

3.2 Optical Rotation

The angle through which the plane ofpolanzatron IS turned when a layer of the liquidsubstance, one decimetre In thickness and at atemperature of 25°C, IS examined under sodiumlight.

4 REQUIREMENTS

4.1 DeseriptloD

The materiel shall be punfied and crystallizedd-glucose contammg one molecule of water oferystallrzation. It shall be white or hght creamIn colour The material shall be a crystallmeor granular, odourless powder readily soluble1ft water With a characteristic sweet taste freefrom foreign flavour.

NOTE - The appearance, taste and odour shall bedetermined by .ensory tests

4.2 Freedom from Colourlnl MatterThe material shall be free from any addedcolouring matter.

4.3 Freedom from. ForellD Matter

The material shall be free from dirt, otherextraneous matter, Insects, rodent of othercontamination.

4.4 LOll o. D'118.

When tested by the method prescribed InAnnox B the loss OD drying shall be not less

than 7 5 percent and not more than 9 5 percentby mass4.5 Speclftc Rotation

The specific rotation of solution containing onegram of the material, previously drred at 105°Cfor 6 hours, With 002 ml of ammoniumhydroxide solution In each J0 ml of water shallbe not less than +52 5° and not more than+ 53 3°, when tested by the method prescribedIn Annex C

4.6 Specific Volume

The specific volume of the material shall not bemore than 160 ml/IOO g when tested by themethod given In Annex D

4.7 The material shall also comply With therequirements given In Table 1

Table 1 Requirements for DextroseMonohydrate

81 Characteristic Requlre- Method of Test.No. meat Ref to

r----A--~

Annex Othero(Thll StandardsStandard

(I) (2) (3) (4) (S)1) D-glucose content ( on 99 S AppendIX B

dry basis). percent ofby mass, Min (S 873.1974

II) Total solids content, 90 Bpercent by mass,Mzn

JU) Ash, sulphated ( on 01 7 ofdry basls ), percent IS 4706by mas" Max ( Part 2):

1978IV) ACidity To F

sausfythe test

v) Sulphur dioxide, mgl 70 It of1e"Max IS 4706

( Part 2) :J978

VI) Arsemc ( as As ), 1 1 0ma/k., Max

VII) Copper ( as Cu ). mg' 2 Hkat Max

vbi) Lead (as Pb ), mal OS Jkl, Max

IX) ZIDC, milk., Max SO0 15 ofIS 6287 :1985

xl TID, ma/kg, Max 2500 16 ofIS 6287 :1985

xi) Mercury I mg/k. t 10 ItMax

xu) Cadmium, ml/kl. 1 S LMax

IS 874 : 19'2

5 PACKING AND MARKING

S.1 PaddDI

The material shall be packed in clean, highdensity polyethylene (HDPE) or polylinedhigh density polywoven bags or biaxiallyoriented polypropylene ( BOPP) or hessian orother textile bags which may be either paper,polyethylene or cotton lined or in suitablemulti-walled paper bags or in lined corrugatedfibreboard containers or in solid fibreboardcontainers or in leverlid tin plate containers.

5.2 Marking

5.2.1 Each container shall be suitably marked/printed with indelible insoluble ink so as to givethe following information:

a) Name of the material;

b) Indication of source of manufacture;

c) Batch or code number;

d) Date of manufacture;

e) Net mass; and

f) A ny other details required under theStandards of Weights and Measures

(Packaged Commodlt;~s) Rules, 1977/Prevention of Food Adulteration Rules,

5.2.2 The containers maya1so be marked withStandar d Mark.

6 SAMPLING

Representative samples of the material shalt bedrawn and conformity of the material to therequirements of this specification shan bedetermined by the method prescribed inAnnex M.

7 TESTS

7.1 The tests shall be carried out as prescribedin 4.4, 4.5, 4.6 and col 4 and S of Table 1.

7.2 Quality of Reasents

Unless specified otherwise, pure chemicals shallbe employed in tests and distilled water( set IS 1070 : 1977 ) shall be used where the useof water as a reagent is intended.

NOTE - 'Pure chemicals' shall mean chemicalstbat do not contain impurities which affect theresults of analysis.

ANNEX A( Clause 2 )

LIST OF REFERRED INDIAN STANDARDS

Rectified spirit ( revised )

Water for general laboratoryuse ( second revision )

IS No.

(second 4706( Part 2 ) : 1978

IS No.

266 : 1977

323 : 1959

873 : 1974

1070 : 1977

Title

Sulphuric acidrevision)

Liquid glucoserevision)

( first 4905 : 1968

6287 : 1985

Title

Methods of test for ediblestarches and starch products:Part 2 Chemical methods( first revision)

Methods for randomsampling

Methods for sampling andanalysis for sugar sonfectio­nery (first revision)

Made of aluminium sheet of thickness 0'50 mm,SS rom in diameter an dIS mm in height with atight-fitting cover. The dish shall have apolished surface.

8-1 APPARATUS

8-1.1 Moisture Dish

ANNEX B( Clause 4.4 )

DETERMINATION OF LOSS ON DRYING

B-2 PROCEDURE

B-2.1 Weigh accurately about S g of thematerial into the tared moisture dish fitted withthe cover. Uncover the dish and dry thematerial in an oven at IOSoC for 4 hours.Replace the cover of the dish, cool in a desicca­tor and weigh. Repeat drying the material in

2

100 (M1 - M,)(M1 - Ai)--

the dish at hourly Intervals, cooling and weighingunnl the loss In mass between two successivewerghrngs IS less than one milhgram. Recordthe lowest mass

B-3 CALCULATION

8-3.1 Loss on drying,percent by mass

IS 874: 19f2

where

M 1 = mass, In g, of the dish with thematenal before drying.

AI,. = mass, In g, of the dish with thematerial after drying, and

M = mass, In g, of the empty dish..

ANNEX C( Clause 4.5 )

DETERMINATION OF SPECIFIC ROTATION

100 CI

'XC

c.i REAGENT

C-t.l Ammonium Hydroxide Solution - rd 090

C-l PROCEDURE

C-l.1 Preparltlon or Solation of the Material

Dry a convenient quantity of the material at105°C for 6 hours In an air-oven and cool It In adesiccator Weigh accurately 10 g of the drredmatenal mto a IOO-ml volumetric flask, dissolveIn a small quantity of water, add 0 2 ml ofammonium hydroxide solution, make up thevolume with water and mix.

C-1.1 Determine the optical rotation of the

solution wrthm 30 minutes from the time It wasdissolved usmg a suitable type of polanmeterand sodium light for all observations.

C-] CALCULATION

C-3.1 Specific rotation of the materral

where

ex = optical rotation In degrees,

I = thickness, In decimetre, of the layerexamined, and

c = mass, In g, of the substance containedIn 100 ml of solution at 25°C

n-i APPARATUS

ANNEX D( Clause 4.6 )

DETERMINATION OF SPECIFIC VOLUME

D..2 PROCEDURE

0-1.1 Cylinder Funnel Assembly

Place a 250 ml graduated cylinder, having agraduated section 24 to 26 ern In length, on ahorrzontal surface Suspend a funnel, having astem 30 mm In length and 70 rom outsidediameter 10 a vertrcal posrnon by means of aring support on a rIng stand, with stem centredmside cylmder 6 em above 250 - ml mark.

NOTE - If cylinder and funnel of abovedrmensrons are not available, Use any 250 mlcylinder and glass funnel havma dimensions nearestto above and keep the same assembly for differentdetermmanons

D-l.2 Balance

Suitable torsion or top Ioadmg balance. Capacity2 kg with 0·1 g accuracy.

D-2. t Accurately weigh about 100 g of thesample and with the aid of a spoon or spatula,carefully add sample to the funnel until thecomplete sample IS transferred In the cylinder.Level the top surface of material 10 the cylinderby ultmg the cylmder, If necessary. Readvolume In ml of the material from graduationson the cylinder.

D-3 CALCULATION

ySpecific volume, ml{lOO g = M X 100

where

Y = volume of sample observed (seeD-1.1); and

M = mass of sample, In g, taken for thetest

3

IS 174: 1"2

ANNEX E[ Table 1, Sl No. (ii) ]

DETERMINATION OF TOTAL SOLIDS CONTENT

E-l The total solids can be calculated as followsafter determmmg the loss on dryIng (see 8-3.1 ).

Total sohds content, _ 100 - 108s on dryiDIpercent, mlm - ( 8-3.1 ).

ANNEX F[ Table 1, Sl No. (IV) ]

DETERMINATION OF ACIDITY

1'.1 REAGENTS

F-I.I Pbellol,bthaleln ludicator Solation

o2 percent ( m]v ) DIssolve 0 2 g of phenol­phthalein ID 60 ml of rectified spmt (,ee IS 323 :1959 ) and add sufflcren! quantity of water toproduce 100 mi.

F-l.2 StaDdard Sodium Hydroxide Solatl08­002 N

'-2 PROCEDURE

1"-2.1 Weigh accurately about 5 g of thematenal mto a conical flask and dissolve It InSO ml of water free from carbon dioxide gas.TItrate the content of the conical flask withstandard sodium hydroxide solution usingphenolphthalein solution as mdicator

F-3 CALCULATION

F-3.1 ACIdIty, as ml of 0 02 N standard sodiumhydroxide solution required to neutrahze , g of

the material 250 'YN==M-

where

Y = volume, In ml, of standard sodiumhydroxide solution required to neutra­lize the quantity of the material takenfor the test,

N = normality of standard sodium hydroxidesolution; and

M == mass, In g, of the [matenal taken forthe test.

F-4 REPORT

F..4.1 The matenal shall be deemed to havesatisfied the requirements of the test If theacrdrry, expressed as volume of 002 N standardsodium hydroxide solution required to neutra­lize 5 g of the matenal, does not exceed 1"0mlunder the conditrons of the test

ANNEXG[ Table 1, Sl No. (VI) ]

TEST FOR ARSENIC

e-I The method as given In Appendix D ofIS 873 )974 shall be adopted With the followingmodification

In D-3.11nstead of 'brommated hydrochloricacid' use 'stannated hydrochloric acid',

ANNEXH[ Table 1, Sl No. (vii) ]

TEST FOR COPPER

H-I The method as given In Appendix E ofIS 873 ]974 shall be adopted WIth the followingmodificanon

4

In F-2.1 Instead of '30 ml standard solution'use '2 ml standard solution'.

IS .74: 1992

ANNEX J[ Table 1, 51 No. (viii) ]

TEST FOR LEAD

J·t The method as given in Appendix F ofIS 873 : 1974 shall be adopted with the followingmodification:

In F-2.1 instead of •S·O ml of dilute leadsolution' use ·0·5 ml dilute lead solution'.

ANNEX K[ Table 1, Sl No. (xi) ]

TEST FOR MERCURY

8

A

oo~

K-1 APPARATUS

K-l PRINCIPLE

K-l.l Sample is digested with nitric acid( RNO,) and sulphuric acid (HtSOt) underreftux in a special apparatus. Mercury isisolated by dithizone extraction, copper is remov­ed and mercury is estimated by photometricmeasurement of mercury dithizonate.

)[·2.1 Speela. DilestiOD Apparatus

(see Fig. 1). The apparatus is made frompyrex glass with standard taper joints through­out. Unit A is a modified Soxhlet extractor,of S em outer diameter and 200 ml capacity,without an inner siphon tube but equippedwith a stopcock on the tube leading to digestionflask, D. With the stopcock open, the apparatusis in reflux position; when closed, the unit servesas a trap for condensed water and acids. Thetop of .If is attached to a Friedrich's condenser,3S em long. The bottom of if is attached tothe centre neck of a 2..neck standard taper 24/40round-bottom SOO-ml flask, D. Necks are 3 cmapart to provide clearance. The second neck isused for attaching a 7S-ml dropping funnel B.

1'-3 REAGENTS

1'-3.1 Mercury Standard Solution

1[-3.1.1 Stock Solution

1 mgfml; prepared from dry, recrystallizedmercuric chloride ( Hgel. ) ( 67·7 mg/50 ml ).

K-3.1.1 Workin, Solution

2 p.g/ml is convenient. Prepare from stocksolution and store in pyrex bottles. Add hydro­chloric acid ( Hel ) in a proportion of 8 ml/litreto all standards before diluting to final volume.

)[-3.2 Chloroform (CHel,)

Distil from hot water-bath, collecting distillatein absolute alcohol in the proportion of 10 mlalcohol to 1 litre distillate. Intermittently shakereceiver during distillatioD.

FIG. 1 SPECIAL DIGESTION ApPARATUS PORDETERMINATION OP MERCURY RESIDUES

1(..3.3 Ditbi1.oneSolution

Dissolve about 1 g commercial reagent in50-75 ml chloroform and filter if insolublematerial remains. Extract in a separator withfour 100 ml portions of metal-free (redistilled)NH,OH (1 :99) (dithizone passes into theaqueous phase to give an orange solution ).Filter aqueous extracts into a large seapratorthrough a cotton plug inserted in the Item of

s

IS 874:: 1992

the funnel. Acidify slightly with dilute ,Heland extract dithizone with two or three 20 mlportions of CHela. Combine extracts' in sepa­rator and wash 2 or 3 times with water. DrainCHela into a beaker and evaporate with gentleheating on a steam bath, avoiding sputtering asthe solution goes to dryness. Remove lasttraces of moisture by heating for I hour atabout 50°C in vacuum. Store dry reagent inthe dark in a tightly stoppered bottle. Preparestock solution in redistilled CHela ( luO mgtlitre is convenient) and store in a refrigerator.Prepare dilutions as needed.

K-3.4 Sodium Thlosulphate Solution

l '5 percent prepared daily.

K-3.5 Sodium Hypochlorite Solution (NaOCI )

Preferably 5 percent available chlorine reagent.The reagent varies in available chlorine content.Determine the strength. Store in refrigeratorwhen not in use and determine titer monthly.( Certain preparations or hypochlorite intendedfor household use contain traces of Hg. Ifthese preparations are used, determine blank.Reagent containing more than 0'1 ,..,g Hg/mlshould not be used. )

K-3.6 Dilute Acetic Acid

30 percent ( v/v )

1'-3.7 Hydroxylamine Hydrochloride Solution( UINOH.HCI )

20 percent ( mlv ), Extract with dilute dithizoneuntil CHCla layer remains green, remove excessdithizone with CHela and filter.

K-4 PREPARATION OF SAMPLE

I-4.t Place weighed sample in digestion flaskwith 6 glass beads. Add 20 ml UNO. to thesample, swirl flask, and let it stand for half anhour in digestion assembly before heating. Add25 ml water and heat cautiously with smallrotating flame until the initial vigorous reactionis over and foaming ceases. [Original reactionmust not proceed violently or the evolvednitrogen peroxide ( NO. ) will carry vapours ofdigest mechanically through the condenser andcause Joss of Hg]. After initial reaction iscomplete, apply heat so that digest just refluxes,If the mixture darkens, add NHOa dropwisethrough the funnel as needed. Continue reflux­ing for half an hour or until the digest does notchange consistency ~ and cool.

K-4.2 Slowly add 20 ml of cold nitric acid­sulphuric acid mixture (1: 1 ) [ Use 100 ml ofacid mixture for about S g (dry mass) ofsample]. Heat with a small ftame, subsequentlyadding nitric acid dropwise as needed to dispeldarkening of the digest. Continue heating untilthe fibrous material is apparently digested. Turnthe stopcock of the soxhlet unit to trap water

and acids, and continue heating. Let the digestbecome dark brown ( not black) before addingfurther increments of nitric acid. (Fats andwaxes cannot be totally digested by hot acidsunder reflux. Therefore, no attempt should bemade to effect complete digestion in thisstep.) When all except fat and wax is in solu­tion, let digest cool. and. cautiously drain waterand acids into main digest. Cool and pour two25-ml portions of water through condenser andintermediate unit. Remove reaction flask, chillunder cold water or by surrounding with ice tosolidify fats and waxes, and filter off insolublematter on small plug of glass wool. Rinsereaction flask and filter pad successively withtwo 10-ml portions of water. Remove soxhletunit and wash it and flask with hot water toremove insoluble material. Pour hot waterthrough condenser to remove volatile fats andoils. Discard all washings.

K-4.3 Connect flask containing filtered samplesolution to assembled apparatus, heat andcollect water and acids in trap. Complete diges­tions, using small additions of nitric acid asneeded. In final stages of digestion, adjust flameuntil digest reaches incipient boiling (solutionsimmers) and acid vapours do not rise beyondlower half of condenser. Continue heating15 minutes after last addition of nitric acid.Digest should now be colourless or pale yellow.Let digest cool, drain trapped liquids carefullyinto reaction flask, and add two 50-ml portionsof water through condenser. Reflux solutionuntil all NO, is expelled from apparatus. Add5 ml 40 percent mjv urea solution and refluxfor 15 minutes. Digest should be colourless orpale yellow.

1:-5 ISOLATION OF MERCURY

K-5.1 Titrate I ml of prepared sample solution( K-4.3 ) with standard alkali. Add a calculatedamount of concentrated ammonia to reduceacidity to 1'0 N; swirl flask during addition ofthe ammonia to avoid local excess ( solutionshould never be ammoniacal to avoid formationof mercury complexes ).

K-5.2 Transfer sample solution to a 500-mlseparator. Add 10 ml of 4 mg/litre dithizoneand shake vigorously for 1 minute. (If thecharacteristic green colour of dithizone is visiblein the chloroform layer, indicating excess ofdithizone, the amount of mercury is withinO'5 ,..,g.) Let the layers separate and drainchloroform layers quickly to a second separatorcontaining 25 ml of 0'1 N Hydrochloric Acidand 5 ml H.NOH.HCI solution. (Small amountof oxidizing material may still be present. Onlong contact with dithizone solution, oxidizingsubstances may destroy dithizone reagent andprevent extraction of mercury. )

X-5.3 Repeat extraction of sample solution withtwo S-ml portions of dithizone solution. trans­ferriag CHela layer successively to second

6

IS 874 : J991

proceed With colorimetnc determination ofmercury as 10 K-7, converting absorbance (A)measured at 490 om to p.g mercury from theworkrng curve

K-7 PREPARATION OF STANDARD CURVE

K-7.1 The followmg table IS useful In preparmgthe standard curve and for estabhshrng appro­prrate mercury range In sample solutions whenl-cm cell is used

K-8 PRECAUTIONS

K-8.1 The cntical step IS drgestion of thesample, which must be almost complete, other­wise the residual organic matter may combineWith mercury and prevent or hmder extracuonWIth dithrzone The oxrdrsmg rnaterial In digestmust also be destroyed otherwise the duhizoncreagent IS decomposed and mere.. ury I~ notquantrtatively extracted Because of volatilityof mercury components careful heating ofdrgevt dur mg sample preparation I'; requiredACIdIty of final sample solution ( after partialneutrahzanon WIth arnmoma ) before extractionshould be about 1 N and not more than I 2 NDo not use sihcone grease In stopcocks

K-7.2 Prepare a working curve of requiredrange, star ting WIth the blank and extending tonnal standard of the range, with 4 intermediateIncrements Add appropriate amounts of mercuryto ~O ml 0 1 N H'Cl In a separator Add 5 mlH 2NOH HCI reagent and 5 ml CHela and shakevigorously for 1 minute Let the layers separate,drain off CHela and discard, being careful toremove as completely as possible all droplets ofCHela Add 3 rnl of 30 percent aceuc acid andan appropriate volume of drth izone solution,shake vigorously for one mmute, and let thelayers separate ( acid aids In stablizmg mercuricdithizonate ) Insert cotton plug Into the stemof the separator and collect dithrzone extract( discardmg the first ml ) In test tube for transferto appropriate cell Make photometer readingsat 490 nm (sInce both dilute dithtzonc andmercunc drthrzonate are somewhat unstable)read Immediately Plot A against ,.,.g mercury

VolumeDtthizone

(ml)(3)

5

2540

DtthtzoneConcentrauon( mg/Irtre )

(2)

6

10

10

(I)

0- 10

0- 50

0-100

Mercury Range,.,.g

K-6 DETERMINATION

K-6.1 10 the thi rd separator, add 3 ml of30 percent aceuc acid and an appropriatevolume and concentration of dithizone solutionas Indicated In the table (see K-7.1) and

separator If first extraction Indicates morethan 5 p.g Hg, add stronger concentrations ofdrthizone, as Indicated by table under K-7.t,untrl after 1 minute of vigorous shaking, CHClalayer contains drthrzone In marked excess DrainCHela layer Into second separator containingo 1 N Hel and again extract sample soluuonIO-rot portrons of 4 mg/Iitre drthrzone volunon,with two drainmg each successive extract In tosecond separator

K-5.4 Shake the contents of secon d separatorvigorously for 1 mmute and drain CHCIa layerInto a third separator contammg 50 ml of 0 I NH'Cl (ShakIng drthizone extract with diluteacid In second separator removes entrainedorganic matter With brological materials orthose of high protein content, aqueous layer ISusually hght yellow because of nitrated organiccompounds Small amounts are carried Intothe third separator where they are destroyed bychlorine ) Extract solution In second separatorwith 1-2 ml CHCla and transfer organic layer tothird separator

1'-5.5 To the contents of the thud separator add2 ml sodium thiosulphate solution, shakevigorously for 1 minute, let layers separate,drain off CHCla as completely as possible, anddiscard (Copper If present IS removed asdlthlzonate) Extract again with 1-2 ml CHCla,drain carefully, and discard Add 3 5 ml NaOelreagent ( or enough solution of different titer tofurnish 175 mg of available chlorme ) to decom­pose mercury thiosulphate complex and oxidrzeexcess thiosulphate, and shake vigorously for1 minute Add 5 ml H2N OH H'Cl reagent frompipette, taking care to wet both stopper andneck of separator Shake vigorously forI mmute Hold the mouth of the separator Infront of the cur vent and blowout any remain­mg gaseous chlorme Stopper separator andshake vigorously for 1 minute It IS impera­tive that all hypochlorite be reduced Traceamounts remammg would OXIdize dithizone,subsequently added, to a yellow oxidized formwhich would be measured In a photometer asmercury Extract the solut Ion With 2-3 ml ofCHCIs, drain off the organic layer carefully,and discard FInal aqueous solution should becolourless

7

IS 874: 1992

ANNEX L[ Table 1, 81 No. (xii) ]

METHOD FOR DETERMINATION OF CADMIUM

L-O Sample is digested with HNO., H.SO" andH.O.. All reactive metals are extracted fromsolution, after adjustment to about pH 9, withdithizone-Cbl'Cl, Cadmium is removed bystripping CHC)a solution with dilute Hel anddetermined by Atomic Absorption Spectro­photometry at 228'8 nm,

L-l REAGENTS

L-l.1 Nitric Acid ( HNOa )

Low in lead and cadmium.

L-l.2 Hydroaen Peroxide ( H 20 . ) - 50 percent.

L-l.3 Citric Acid

Monohydrate fine crystal.

L-l.4 Thymol Blue Indicator

Triturate 0'1 g indicator in agate mortar with4'3 ml 0'05 N NaOH. Dilute to 200 ml withH.O.

L-l.5 Dltbizone Solutions

Concentrated solution - 1 mg/ml. Prepare220 ml in CHCI,. Prepare fresh daily.

L-l.6 Cadmium Standard SolutioDl

L-l.6.1 Stock Solution

1'0 mgl ml. Dissolve 1 000 g cadmium, inJ6S ml Hel in I I volumetric flask. Dilute tovolume with H.O.

L-l.6.2 Intermedtate Solution

10 flog/rot. Dilute 10 ml stock solution with 2 NHel to 1 1. Prepare just before use.

L-1.6.3 Working Solution!

Dilute 0, 1,5, 10 and 20 ml intermediate solutionto 100 ml with 2 N HCI (0, 0'1, 0'5. 1'0, and2'0 pog Cd! rot respectively).

L-2 APPARATUS

L-2.1 Atomic Absorption Spectrophotometer

With hollow-cathode cadmium lamp and 10 cmburner head for air-CIH. flame; wavelength228'8 nm, range 0-2'0 pog/ml.

L-2.2 Glassware

Thoroughly washed with S'O N HNOa andrinsed with water. Beakers and watchglassesto be covered during all operations.

L-3 PROCEDURE

L-3.1 Digestion

Weigh 50'0 g sample into 1'5 I beaker, Addseveral boiling chips or beads, and cover. Care­fully add 25 ml HNO,. cover, and warm gentlywith flame to initiate reaction. When reactionsubsides, add 25 ml HNOa, warm again, andcontinue until 100 ml HNO. has been added.( Alternatively, add 100 ml HNO, all at once,with caution, add let stand at room temperatureovernight.) Heat until most nitrous oxidefumes have evolved; control excessive frothingby cooling or quenching with H.O from washbottle. Only some cellulose an d fatty rna terialsif any, remain undissolved.To remove any fat visible in hot solution,proceed as follows: Cool beaker in ice, anddecant clear, aqueous solution from coagulatedoils and solids through glass wool pad into I 1beaker. Add 100 ml HaO to I'S I beaker withfat, heat, swirl vigorously to rinse fat, chill, andfilter as before. Wash funnel and glass woolpad with about 20 ml H,O.

Add 20 ml H,SO, to sample, dilute to about300 ml with H.O, and evaporate over flameuntil charring begins. When charring becomesextensive, cautiously add SO percent H.01 ,

I ml at a time. Let reaction subside beforeadding next portion of oxidant, and never addgreater than 1 rot at a time. Continue additionsof H.O. until solution is colourless, Heatvigorously to SOa fumes, adding more HIO.as required to remove char_Heat vigorously toexpel excess HzO.. Cool colourless digest toroom temperature.

Prepare reagent blank of 100 ml HNOa, 20 mlR.SO., and same amounts of H 20 as added tosample. Cautiously add same amounts of 50 per­cent HIO t , as above, and remove all HNO.from blank. Carry out blank through sameoperations as sample.

L..3.2 Extraction

Add 2 g citric acid to cooled digest andcautiously dilute to about 25 ml with H.O.Add 1 ml thymol blue indicator and adjust toabout pH 8'8 by slowly adding NH,OH whilecooling in ice bath, until solution changes fromyellowish green to greenish blue. Transferquantitatively to 250 ml separator, using RIO,and dilute to about 150 ml.

Cool solution, and extract with two S-ml portionsconcentrated dithizone solution, shaking 1-2minutes each time. Continue extraction withS ml portions of dilute dithizone solution until

8

IS .74: 1992

last S ml portion of dithlzone extract shows nocbanae In colour. Combine drthizone extractsm 125 ml seperator; wash with 50 ml H.O, andtransfer solvent to another 125 mt separator.Extract HtO, wash with S ml CHela and addthts to drthizcne extracts. Add SO mlo 2 N Hel to combined dnhizone extracts,abake vigorously for I minute, and let layersseparate, discard dithizone layer Wash aqueoussolunon with 5 ml CHela and discard GHCI•.Quantitatively transfer aqueous solution to400 ml beaker, add boihng ChIpS, and evaporatecarefully to dryness Carefully rinse downaides of beaker wIth 10-20 ml H,O and agarnevaporate to dryness

L-3.3 Set Instrument to previously establishedoptimum eondmons, usmg au acetylene oxrdiz­Ing flame and 228 8 nm resonant wavelensth.DIssolve dry residue 111 S 0 ml 2 N Hel anddetermine A. of sample and standard solutionsagamst 2 N Hel as blank Flush burner withR.O between readings. Use scale expansioncontrols to obtain 4-10 X expansion, as con­venient. Determine cadmium from curve of Aagainst lAgCd/ml:

ppm Cd - ( prg Cd/ml) x (mt 2N HCIIgsample)

For concentration > 2 0 lAg Cd/ml, dilute,solution with 2 N no

ANNEX M( Clause 6.1 )

SAMPLING OF DEXTROSE MONOHYDRATE

M-3.1 Preparation of IndiTidoal Samples

M-2.1 The number" of containers to be selectedfrom the lot shall depend on the size of the lotN and shall be as given In Table 2.

Table 2 Number of Container. to beSelected for Samp1inl

M-2.3 The containers shall be selected fromthe lot at random In order to ensure therandomness of selection, procedures given InIS 4905 1968 may be followed

M-3 TEST SAMPLES AND REFEREESAMPLES

In the case of smaJl contamers, empty out thecontents of each selected container on a sheetof paper and mix thoroughly Cone andquarter as often as necessary nll a quantity ofthe material not less than 500 g I~ left. In thecase large containers, draw With an approprratesamphng Instrument small but equal quantmesof the material from top. middle and bottomportions of each selected con tal ner so as to geta total quantity of the material not less thanSOO g From this, take about 250 g of thematerial and divide It Into three equal partsEach part so obtained shall constitute an In­drvrdual sample representing the contarner andshall be transferred tmmediately to thoroughlyclean and dry containers, sealed air-tight and

No 01 CoDtalDento be Selected

n(2)3457

10

Lot Size

N(1)

3 to IS16to 4041 to 6566 to 110Over 110

M-2 SCALE OF SAMPLING

M-2.1 Lot

All the containers 10 a SIngle consignment ofthe matenal drawn from the same batch ofmanufacturer shall constitute a lot If aconsignment IS declared to or IS known to consistof dIfferent batches of manufacture, the con­tamers belonging to the same batch shall begrouped together and each groupshall constrtutea separate lot.

M.2.1.1 Samples shall be tested from each lotfor ascertaimng conformrty of the material tothe requirements of the specificanon

M-l GENERAL REQUIREMENTS OFSAMPLING

M-l.0 In drawing, preparing, stormg andhandling samples, the followmg precautions anddrrectrons shall be observed

M-l.l Samphng Instrument shall be clean anddry when used.

M-l.~ Precautions shall be taken to draw thesamples In a manner so as to protect the samples,the material bemg sampled, the samphngInstruments and the containers for samplesfrom adventrnous contammanon

M-l.3 The samples shall be placed In clean anddry glass containers.

M-l.4 The sample containers shall be sealed,arr-nght after filling and marked with full detarlsof sampling, date of manufacture, name of themanufacturer and other Important particularsof the consignment

M-l.5 Samples shall be stored In such a mannerthat the conditrons of storage do not undulyaffect the quality of the material.

Q

IS 874: 1992

labelled wrth the particulars gwen under M·l.4.The Individual samples so obtained shall bedivided Into three sets In such a way that eachset has a sample representing each selectedcontainer. One of these set shall be marked forthe purchaser, one for the vendor and the thirdfor the referee

M-3.2 Preparation of Composite Sample

Out of the rnaterra1from each selected containerremammg after the Individual sample has beentaken, equal quantrties of the matenal shall betaken and mixed together so as to form acomposite sample weighing not Jess than 600 gThis composite sample shall be divrded Intothree equal parts and transferred to clean drycontainers made of glass and labelled WIth theparticulars given In M-l.4 One of these com­posite samples shall be for the purchaser, one forthe vendor and the third for the referee

M..3 3 Referee S.mple

Referee sample shall consist of a set ofmd ividual samples (M..3.1) and a compositesample ( M..3.2 ) marked for this purpose andshall bear the seals of the purchaser and thevendor These shall be kept at a place agreedbetween the two

M·4 NUMBER OF TESTS

M·...! Tests for description, loss on drying.specific volume, D-glucose content, total solldaand specific rotation shall be conducted on eacbof the samples constituting a set of mdivrdualtest samples ( M-3.l )

M·~.2 Tests for the remammg charactensnes,namely, sulphated ash, acidity t sulphur dioxide.arsemc, lead, copper, Zinc, tin, mercury andcadmium, shall be conducted on the compositesample as prepared under M..3.2

M·! CRITERIA FOR CONFORMITY

M-S.1 The lot shall be considered to havesansfied the requirements for descnption, losson drying and specific rotation If each of themdrvidual test samples tested as In M·...)sansfies the relevant requirements

M-5.2 The lot shan be considered to havesatisfied the requirements for remainingcharacteristics If all the test results as obtainedon the composite sample (M..4.Z) satisfy therequirements for these charactenstics

M-S 3 The lot shan be considered to havesatisfied all the requirements of thrs specrflcanonIf It passes In M-S.1 and M-5.2

10

Standard Mark

The use of the Standard Mark is governed by the provisions of the Bureau of IndianStandards Act, 1986 and the Rules and Regulations made thereunder. The Standard Mark onproducts covered by an Indian Standard conveys the assurance that they have been producedto comply with the requirements of that standard under a well defined system of inspection,testing and quality control which is devised and supervised by BIS and operated by the pro ..ducer, Standard marked products are also continuously checked by BIS for conformity tothat standard as a further safeguard. Details of conditions under which a licence for the useof the Standard Mark may be granted to manufacturers or producers may be obtained fromthe Bureau of Indian Standards.

Bareau of Indian Standara

BIS is a statutory institution established under the B 4"2'" o/Indi"n StandardJ ~CI, 1986 to promoteharmonious development of the activities of standardlzatlon, m'.lrklnl and quality certification ofgoods and attending to connected matters in the country.

Copyright

BIS has the copyright of all its publications. No part of these publications may be reproduced inany form without the prior permission in writing of BIS. This does not preclude the free use, inthe course of implementing the standard, of necessary details, such as symbols and sizes, type orgrade designations. Enquiries relating to copyright be addressed to the Director (Publications ), BIS.

Re.islon or Indian Standards

Indian Standards are reviewed periodically and revised, when necessary and amendments, if any,are issued from time to time. Users of Indian Standards should ascertain that they are inpossession of the latest amendments or edition. Comments on this Indian Standard may be sentto BIS givinS the following reference :

Doc: No. FAD 17/33 (4052)

Amendments Issued Since Pablieation

Amend No. Date of Issue Text Affected

BUREAU OF INDIAN STANDARDS

378662

53 38 43

2350216

632 92 95

Telegrams: Manaksanstha( Common to all Offices)

Telephone

{331 01 31331 13 75

Headquarters:

Manak Bhavan, 9 Bahadur Shah Zafar Marg, New Delhi 110002Telephones: 331 01 31, 331 13 75

Reaional Offices :

Central: Manak Bhavan, 9 Bahadur Shah zafar MarsNEW DELHI 110002

Eastern: 1/14 C.I.T. Scheme VII M, V.I.P. Road, ManiktolaCALCUTTA 700054

Northern: seo 445-446, Sector 35-C, CHANDIGARH 160036

Southern: C.I.T. Campus, IV Cross Road, MADRAS 600113

Western: Manakalaya, E9 MIDC, Marol, Andheri (East)BOMBAY 400093

Branches: AHMADABAD. BANGALORE. BHOPAL. BHUBANESHWAR.COIMBATORB. FARIDABAD. GHAZIABAD. GUWAHATI.HYDERABAD. JAIPUR. KANPUR. LUCKNOW. PATNA.THIRUVANANTHAPURAM.

Printed at Swatantra Bbarat Press, DelhI, IDdia