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”

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“Knowledge is such a treasure which cannot be stolen”

“Invent a New India Using Knowledge”

है”ह”ह

IS 8249 (1994): Zinc sulphate heptahydrate, agriculturalgrade [FAD 7: Soil Quality and Gertilizers]

REAFFIRMED~6. .. ... IS 8249 : 1994

\11(-\ ~14 1fACf)

m ~G~ ctIN Vs - fqfwfisc

( q~~n tjwt~1eftJI )

Indian Standard

ZINC SULPHA'IE HEPTAHYDRATE,AGRICULTURAL GRADE - SPECIFICATION

( First Revision )First Reprint JANUARY IlJY6

<0 815 1994

BURE,\V OF INDIAN STANDARDSMANAK BHAVAN, 9 BAHADUR SHAH lAFAR MARO

NEW DELHI 110002·f

AMENDMENT NO. 1 FEBRUARY 2001TO

IS 8249: 1994 ZINC SULPHATE HEPTAHYDRATE,AGRICULTUR~LGRADE - SPECIFICATION

(First Revision)

( Page 1, clause 3.1 ) - Substitute the following for the existing:

'The material shall be in the form of crystals consisting essentially ofZnS04.7H20!

( Page 5, Annex B ) - Substitute the following for the existing:

ANNEXB[ Table 1, 51No .(ii ) ]

DETERMINATION OF MAGNESI lIM

B-1 Two methods have been specified EDTA method and Atomic AbsorptionSpectroscopic method. The Atomic Absorption Spectroscopic metbod shall betaken as referee method.

B-Z EDTA METHOD

B-%.1 Reagents

B·Z.I.l Dilute Suphuric Acid - approximately 5 N.

B-Z.l.1 Dilute Nitric Acid - approximately 10 percent (vlv).

B-Z.I.3 Sodium SUlphide Solution - 10 percent.

B·Z.l.4 Eriochrome Black T Indicator - Dissolve 0.1 g of Eriochrome black Tin 25 ml of methyl alcohol.

B-Z.l.S Diammonium Hydrogen Phosphate - 10 percent (vlv).

B-%.1.6 Ammonium Hydroxide -Ammonium Chloride Buffer Solution

Mix 350 ml of ammonium bydroxide (20 percent, m/m) with 34 g of ammoniumchloride. Dilute with water and make up tbe volume to 1 000 mi. (The pH of tilesolution should be not more tban 10.)

B-Z.I.7 Standard Magnesium Solution - 0.01 M.

Group 3 1

Amend No.1 to IS 814' : 1.94

B-Z.1.7.1 Weigb 2.464 0 g of magnesium sulphate (MgS04.7H20) and dissolveit in water. Make up tbe volume to one litre ..

R·Z.I.8 Ethylenediamine Tetreaceuue (EDTA) Solution

Dissolve 3.72 g of disodium ethylenediamine tetra acetate dihydrate in water andmake up the volume to one litre.

B-Z.I.8.1 Standardization 01EDTA solution

Take 10 ml of standard magnesium solution in a conical flask. Add 20 ml ofwater, 1 ml of Eriochrome black T indicator and 25 ml of ammonium hydroxideammonium chloride buffer solution. Heat to 40 to SOoC and then titrate withEDTA solution, maintaining the tempenture between 40 and soGe until thecolour changes from wine red to distinct blue. Calculate the molarity of EDTAsolution as follows:

Mola rity of EDTA solution.10Mt

VIwhere

Ml =molarity of standard magnesium solution, and

Vt =volume in ml of EDTA solution used for titratioD.

B-2.! Procedure

B-2.Z.1 Weigh accurately about S g of the sample, dissolve in water and add1 mJ of-dilute sulphuric Icid. Filter the solution and make up to 2SO mI withwater in I volumetric flask. Take SO mI of tbe above solution ill. beaker, beat,pass bydrogen sulphide gas or add sodium sulpbide solutioD and eaule completeprecipitation. Filter, bot aDd keep the filtnte for the determination of magnesiumas given in 8-2.2.1. Boil tbe residue with dilute nitric acid and filter if necessary.To tbe filtered solution add dilute sulphuric acid, evaporate, dilute and filter. Usetbe filtrate for the determination of copper Ind the residue for tbe determinationof lead.

1J.1.Z.Z Take the filtrate obtailllCd in B-Z.%.l after precipitation -of sulphides,add a few drops of concennated nitric acid, boil and cool and then add solidammonium chloride (about 2 g), boil and cool, add ammoniuDI hydroxide tillstrong smell of ammonia comes Ind filter the precipitate tbrougb sinteredcrucible. Take the filtrate and add dilute sulphuric Icid till the solution is acidic(test with methyl IU), belt the solution to boil and add excess of diammonium

2

Amend No.1 to IS 8149 : 1994

hydrogen phosphate with continuous stirring. Add 10 percent ammonia solutionwitb continuous stirring till the solution is just alkaline (test with methyl red);while precipitate of zinc ammonium phosphate will be formed (the optimum pHfor precipitation is 6 to 7). Allow it to stand for 3 to 4 hours, tben filter throughfilter paper (Wbatman No. 40 or equivalent). Collect the filtrate in I volumetricflask and make up the volume (say to 100 ml), take a suitable aliquot (say 10ml)for the determination of magnesium. Add 20 011 of water, 1 ml of eriochromeblack T indicator and 20 ml of ammonium hydroxide..ammonium chloride buffersolution. Heat to 40 to 50°C and titrate with standard EDTA solution,maintaining the temperature between 40 to 50°C until the colour changes fromwine red to distinct blue.

8-1.3 Calculation

1 ml ero.oi M EDTA =0.243 2 mg of 'Mg'

v x 0.243 2Magnesium (as Mg), percent by mass = S

where

V = volume of 0.01 M EDTA solution used for titration.

8-2.3.1 The calculation factor S is derived presuming tblt 5 g of material istaken for test in 0-%.%.1 Ind the filtrate obtained in B-%.Z.% is 100 ml out ofwbich 10 ml is titrated.

B·3 ATOMIC ABSORPTION SPECTROSCOPIC METHOD

B-3.1 Reagents

B-3.1.1 Strontium Chloride

Dissolve 7.5 g of strontium chloride (SrCl2.6H20) in one litre of glass distilledwater.

B-3.1.Z Standard Magnesium Solution

Weigh 0.507 g of magnesium sulphate (MgS04. 7H20) on I clean watch glassand transfer it to one litre flask tbrough the funnel giving several washings towatch glass and tbe funnel with gllSS di4Jtilled or demineralized Wlter. This is50 ppm Mg solution. Dilute 10 ml of SO ppm solution of Mg to 100 ml to get5 ppm sta ndard Mg solution.

3

Amend No.1 to IS 8%49 : 1994

B-3.1.3 Preparation ofWorking Standards

Pipette tbe following volume of S ppm standard Mg solution in 50 ml numberedvolumetric flasks. Add 10 ml of strontium chloride solution to each flask andmake up the volume to SOmi.

Stopper the flask and shake them well. Prepare fresh standards every fortnight.

Flask No. Volume of5 ppm Volume 01 Concentration ofmg Solution taken Strontium Magnesium alter

(ml) Chlo,ideAdded Making the( ml) Volume to 50 ml

(ppm)

1 0.0 10.0 0.02 2.0 10.0 0.23 4.0 10.0 0.44 6.0 10.0 0.65 8.0 10.0 0.86 to.o 10.0 1.0

B-J.Z Procedure

8-3.%.1 Pipette 20 ml of a solution which was prepared for the determination ofzinc by dissolving 0.25 g of the fertilizer sample in one litre flask. Add 10 ml ofstrontium chloride, Make up the volume to SOml,

8-3.1.1 Flame the standards Ind the samples on Itomie Ibsorption spectroscopicpbotometer at the wavelength of 285.5 mJ1(Mg line of the lastrument).

B-3.3 Calculations

Prepare a standard curve of known concentntions of Mg solutiolUJ by plottingtbe absorbance value on V-axis against tbeir respective concentntion values onX-axis. Percentage magnesium in tbe zinc fertilizer will correspond to theconcentration values calculated from the standard curve.

4

Amend No. 1 to IS 8Z49 : 1994

Example:

Mass of the fertilizerVolume madeFurther dilutionReading of the sample from absorption spectrophotometerCorresponding concentration of Mg from standard curveagainst YabsorbancePercentage magnesium in the fertilizer

a 0.25 g::z 1000 ml= 2.5 times= y= X

= X

( Page 6, Annex C ) - Substitute tbe following for the existing:

ANNEX C[ Table 1, 51 No. (iii) ]

DETERMINATION OF COPPER

e-l Two methods have been specified chemical method (Diethyldithiocarbamate method or biquinoline method) or Atomic absorptionspectroscopic method.

c-a CHEMICAL METHOD

c-z.i PROCEDURE

Make up the filtrate in 8-1.1.1 for the detennination of copper, to 200 ml withwater in a volumetric flask. Take a suitable aliquot of the solution containing notmore than 0.05 mg of copper. Determine copper by dietbyl ditbiocarblmatemethod or by biquinoline method as prescribed in IS 7212.

C·3 ATOMIC ABSORPTION SPECTROPHOTOMETRIC METHOD

C ...3.1 Reagents

C·3.1.1 Standard Copper Solution

Weigb 0.196 5 g of copper sulphate (CuS04. 5H20) on I clean watch g..ss Indtransfer it to one litre flask through tbe funnel giving seven) washings to Witchglass and the funnel witb glass distilled Wiler. Add one ml of 10 percentsulphuric acid and make up the volume up to the mark. Stopper the Olsk andshake the solution well. This is SO ppm Cu solution and sbould be stored in aclean bottle for further use. Dilute 10 ml of SO ppm solution of copper to 100 mlto get 5 ppm standard copper solution.

s

Amend No.1 to IS 8Z49 : 1994

C-3.1.Z Glass distilled or mineralized acidified water ofpH 2.5 ± 0.5.

e·3.1.3 Preparation of Working Standards

Pipette the following volume of 5ppm standard copper solution in 50 mlnumbered volumetric flasks and make the volume with acidified water.

Flask No. Volume of5 ppm Concentration ofCopperStandards Cu Solution taken after Makillg the Volume to

(ml) 50ml(ppm)

1 0.0 0.02 2.0 0.23 4.0 0.44 6.0 0.65 8.0 0.86 10.0 1.0

Stopper tbe flasks and shake them well. Prepare fresh standards every fortnight.

C·3.2 Procedure

C-J.2.1 The solution which was prepared for the determination or zinc bydissolving 0.25g of the fertilizer sample in one litre flask should be used for tbedetermination of copper.

C-J.2.1 Flame the standards and the samples on an atomic absorptionspectrophotometer at a waYclcngtb of 324.8 mfA. (Cu line of the instrument).

C-3.J Cakulatlons

Prepare the standard curve of known concentrations of copper solutions byplotting the absorbance values on Y-axis against tbeir respective concentrationvalues on X-axis. Calculate tbe percentage copper in the zinc fertilizer bymultiplying tbe copper concentration value calculated from the standard curveby 0.4.

6

Amend No.1 to IS 8149 : 1994

Example:

Mass of the fertilizer samples a 0.25 gVolume made =1 000 mlReading of the sample from atomic absorption spectrophotometer :z YCorresponding concentration of copper from standard curve =X ppm

against YabsrobancePercentage copper in the fertilizer =0.4 X

( Page 6, Annex D ) - Substitute the following for the existing:

ANNEX D[ Table 1, Sl No. (iv) ]

DETERMINATION OF LEAD

D-l Two methods have been specified dithiozone method and atomic absorptionspectrophotometric method. The atomic absorption spectrophotometric methodshall be taken 8S referee method.

D-Z DITHIOZ()NE METHOD

D-Z.1 ProcedurE

Dissolve the residue received in 8-2.2.1 for determination of lead in dilute nitricacid, and make up to a known volume with water in I volumetric flask. Take asuitable aliquot of the solution and determine lead by tbe calorimetric methodusing dithiozone as prescribed in IS 7017.

D-] ATOMIC ABSORPTION SPECTROPHOTOMETRIC METHOD

1)-3.1 Reagents

0-3.1.1 Standard Lead Solutions

Weigh 0.159 9 g of lead nitrate [Pb(N03)2] on a clean watch glass and transfer itto one litre flask through tbe funnel giving several washings to watcb glass andfunnel with glass distilled or demineralized water. Add 10 ml of concentrateddistilled nitric acid and make the volume up to the mark. Stopper the flask Indshake the solution well. This is 100 ppm lead solution and should be stored in aclean bottle for further use. Dilute 10 ml of 100 ppm solution of lead to 100 mlwith 1 percent nitric acid solution to get 10 ppm standard lead solution.

7

Amend No. 1 to IS 8149 : 1994

0.3.1.% One Percent Nuric Acid Solution

Dilute 10 ml of concentrated distilled nitric acid to one litre with glass distilledwater.

D-3.1.3 Twenty Percent Zinc Sulphate Solution

Weigh 20 g of zinc sulpahte (ZnS04.7H20) and dilute to tOO mI Witb 1 percentnitric acid solution.

D-3.1.4 Preparation ofWorlcingStandards

Pipette the following volume of 10 ppm standard lead solution in SO mInumbered volumetric flasks. Add 5 ml of 20 percent zinc sulphate solution toeach flask and make the volume with 1 percent nitric acid solution.

Flask No. Volume of10 ppm Volume 0120% .Concentration ofLead Solution lake" Zinc Sulphate Lead after Making

(ml) Solution Added the Volume to(ml) 50ml(ppm)

1 0.0 S.O 0.02 2.0 S.O 0.43 4.0 S.O 0.84 6.0 S.O 1.25 8.0 S.O 1.66 10.0 S.O 2.0

Stopper tbe flasks and sbake them well.

D-3.1 Procedure

0.3.%.1 Preparation of Zinc Sulphate Fertilizer Samples - Weigh 1 g of 'thematerial on I clean watch glass and transfer to SO mI volumetric flask throughtbe funnel giving washings with 1 percent nitric acid solution. Dissolve thematerial Ind make up the volume with 1 percent nitric Icid solution. Samplesshould be prepared in duplicate.

D-J.Z.z Flaming the Solutions

Flame the standards and the simples OD atomic absorption spectrophotometer 11

I wavelength of 217 mu(Lead line of tbe instrument).

8

Amend No. 1 to IS 814' : 19'4

0.3.3 Calculations

Prepare a standard curve of known concentrations of lead solutions by plottingtbe absorbance values on Y-axis against their respective lead concentntion onX-axis. Cakula1e the percentage lead in zinc fertilizer by multiplying leadconcentration value calculated from standard curve by 0.005.

(PCD20)

RepropapIaJ UBit, 81S.NewDelhi, ladia9

AMENDMENT NO. 2 MAY 2012 TO

IS 8249 : 1994 ZINC SULPHATE HEPTAHYDRATE, AGRICULTURAL GRADE — SPECIFICATION

( First Revision )

[Page 1, clause 4.2(d)] — Substitute ‘Gross and net quantity in kg;’ for ‘Gross and net mass in kg;’.

(FAD 7)

Reprography Unit, BIS, New Delhi, India

Fertilizers Sectional Committee, PCD 20

FOREWORD

This Indian Standard ( First Revision ) was adopted by the Bureau of Indian Standards, after thedraft finalized by the Fertilizers Sectional Committee had been approved by the Petroleum, Coaland Related Products Division Council.

In this revision, consideration has bee-n given to the need for maintaining co-ordination with thespecifications of the Fertilizer (Control) Order, 1957 and the Essential Commodities Act. 1955 ofGovernment of J»dia, therefore. three methods of test for determination of zinc have beenincluded. Any method can be used for routine analysis whereas method 3 is a referee method inthe event of any dispute.

This standard is subject to the provisions imposed under Fertilizer Control Order whereverapplicable.

For the purpose of deciding whether a particular requirement of this standard is complied with,the final value, observed or calculated, expressing the result of a test or analysis, shall be roundedoff in accordance with IS 2: 1960 'Rules for rounding off numerical values (revised)'. Thenumber of significant places retained in the rounded off value should be the same as that of thespecified value in this standard.

IS 8149 : 1994

Indian Standard

ZINC SULPHAT~ HEPTAHYDRATE,AGRICULTURAL GRADE-SPECIFICATION

( First Revision)

e following Indian Standards are necessary adjuncts: this standard :

.isstandard prescribes tbe requirements and metbodsrsampling and test for zinc sulphate beptabydrate,}"icultural grade.

REFERENCES

SCOPE

IS No.

()70: 1992

741 : 1970

985 : 1985

()92

Part 1) : 1985

?art 3) : 1985

?art 6) : 1985

)17 : 1973

212 : 1974

Title

Reagent grade water (third revision)

Method for determination ofpH(Reaffinned 1977)

Code of practice for handling andstorage of bagged fertilizers(Reaffirmed 1990)

Methods of sampling and test forfertilizers

Sampling (Reaffirmed 1990)

Part 3 Determination of phosphorus(first revision) (Reaffirmed 1990)

Part 6 Determination of moistureand impurities (first revision)(Reaffirmed 1990)

Method of colorimetric determinationof traces of heavy metals by dithizone(Reaffirmed 1991)

Methods of determination of copper(Reaffirlned 1988)

Table 1 Requirements ror Zinc SulphateBeptahydrate, AgrIcultural Grade

(Clauses 3.2, 6.2.2 to 6.2.4 and 1)

8. CbRadelisdc aeq.......eal Method of TestNo. (ReI to Aaa.z)

(1) (2) (3) (4)

i) Zioc (a Zn). percent 21.0 AnnexAby mass, Mill

if) Mapaium (as Mg), 0.5 Annex Bpercent by mass, Max

iii) Copper <as Cu), percent 0.1 ADnexCby mass,Max

iv) Lead (as Pb), percent 0.003 Annex Dby mass, MtVC

v) pH of S'percent (1ftIv) Not less than 4.0 Annex Esolution

vi) Matter insoluble in 1.0 Annex Fwater, percent bymass, Max

4 PA.CKING AND MARKING

4.1 Packing

The material shall be packed in the manner as agreedto between tbe purchaser and the supplier. Each bagshall be securely closed.

be above mentioned standards contain provisions..bich, througb reference in this text, constituteprovisions... this standard. At the time of publication, theIitions indicated were valid. All standards are subject) revision, and parties to agreements based on thistandard are encouraged to investigate the possibility" applying the most recent editions of the standardsidicated above.

REQUIREMENTS

.1 Description

'he material shall be dry, in the fonn of free-flowingowder or crystals consisting essentially of znSo~.7H20.

.% The material shall also comply with theequirernents given in Table 1.

1

4.% Marking

Eacb bagshall bear legibly the following information:

a) Name of tbe fertilizer;

b) Indication of the source of manufacture;

c) Percentage of zinc by BlaSS; and

d) Gross and net mass in kg;

e) Batch number, in code or otherwise. to enablethe lot of manufacture to be traced back fromrecords; and

t) Any other information IS required under FCO.•

4.2.1 The packages may also be marked with theStandard Mark.

4.3 DIS Cel1lftcatlon Marking

The product n18Y also be marked with Standard Mark.

4.3.1 The use of the Standard Mark is governed by tbeprovisions of Bureau of Indian Standards Act, 1986and the Rules and Regulations D18de thereunder. Thedetails of conditions under which tbe licence for theuse ofStandard Mark may be granted to manufacturersor producers may be obtained from the Bureau ofIndian Standards.

S HANDLING AND STORAGE

Factors to be taken in view in tbe bandJingand storageof the material shall be 8S prescribed in IS 5985: 1985.

6 SAMPLING

6.1 Representative samples of the material shall bedrawn as prescribed in IS 6092 (Part 1) : 1985.

6.2 Number orTests and Criteria for Conformity

6.2.1 Zinc shall be tested on each of the individualsamples.

6.2.2 The remaining characteristics given in Table 1shall be tested Oil ~he composite sample,

6.2.3 The Jot shall be considered to have satisfied tberequirement for zinc, if test results 011 each of theindividual samples meet the corresponding requirementgiven in Table 1.

6.Z.4 The lot shall be considered to have met tberemaining requirements given in Table 1 if each of thetest results on the composite sample satisfies thecorresponding requirement given in Table I.

6.3 The lot shall be declared as conforming 10 therequirements of the specification if6.2.3 and 6.2.4 arcsatisfied.

7 TEST METHODS

The test for the requirements listed under 3 shall becarried out according to methods prescribed in IS 6092(Part 2) : 1985, IS 6092 (Part 3) : 1985 and IS 6092(Part 6): 1985. Reference to relevant parts and clausesare given in ('01 4 of Table 1.

Unless specified otherwise, pure chemicals and distilledwater (see IS 1070 : 1<)92) shall he employed in tests.

NOTE -- . Pure chemicals' shall mean chemicals that do notcontain impurities which affect the results of analysis,

ANNEXA(Table 1)

MI:'rHODS OF TEST .'OR ZIN(~ SUl.,)'lL\l'fI4: Hf:IYfAHYDRAT.:.

AGRICUIJ'rIJRAI., GRAI)I·:

A-O DETERMINATION 0." ZINC

Three methods have been prescribed for determination)f zinc in zinc sulphate heptahydrate, agriculture grade,All tbe methods can be used for determination of zinc)0 routine basis. However in the event of any dispute,\1ethod 3 should be treated as a referee method.

"Ie/hod 1

-\-1 El'HYLEN..: IllAl\lINE l·.:'rRAA(:..~rrAl·.::EDTA) METHOD

\- J.O ()utIJne or thr Meth(Mt~('

~inc is titrated against ethylene diamine tctraacctatc"EDTA) solution. The initial separation of zinc fr0J11'mpuritics is done by zinc sulphide precipitation.

\-1.1 Reagents

1\-1.1.1 Dilute Sulphuric Acid - (1 : 1(0).

\-1.1.% Ammonium Sulphate - AR Grade.

2

A-I.l.3 Hydrochloric Acid - (1 : 1).

A-l.1.4 Sodium Hydroxide Solution -- 1 N.

1\-1.1.5 Metltv! Orange 111{.Iif~(Il(J" -- n.ns pvrccut.

A- J.1.6 Methyl Red Indicator

Dissolve O.t g of nu-thyl red in 50 1111 nfl'rhanol anddilute 10 100 ml with water.

A-I.I.8 EtlJr!"l!t' Diaminv Tctraacetate (EDTA)Solution - 0.0 I J\t1.

Dissolve 3.723 g of disodium ethylene diaminc tetraacetate dihydrate in distilled water nnd make up thevolume to I litre in alliin.' volumetric flask.

A-1.1.9 Zinc Ion Solution --0.1 hi.

Weigh about 1.63 g of i'iUl' shot or zinc Illct~1 (01'99:9percent purity) fl'ag(.)nt grade accurately. Dissolve 1:1

20 ml ofhydrochloric acid (1 : 1), keep it for few boursInd allow it to dissolve completely.

Neutralize the resultingsolution with sodium hydroxidesolution using methyl red indicator. Make up thevolume of the solution to exactly 250 mi.

A-I.I.tO Buffer Solutio" - pH 10.

Add 142mJ of concentrated ammonia solution (relativedensity 0.88 to 0.90) to 17.s g of ammonium chlorideAR grade and dilute to 250 ml with distilled water.

A-I.I.lt Eriochrome Black T Indicator

Dissolve 0.2 g ofdry stuff in 15 ml of triethanolamineand S m1 of absolute ethanol.

~-l.Z Procedure

A-l.%.l Standardization 01EDTA Solution

Dilute 2S ml of standard zinc ion solution to 100 mlwithdistiJled water, add 2 ml ofthe buffersolution anda few drops of the eriochrome black T indicator.Titrate with the EDTA solution until tbe colour changesfrom wine red to blue.

Calculate 1 ml EDTA equivalent to zinc as givenbelow:

Note tbe volume of EDTA consumed 88 VI ml.

1 ml of EDTA Mass of zinc weighed

(0.01 M) solution = in A - 1.1.9 in mg = M110 )( V

1

A-l.2.Z Weigh accurately 7.5 g of the sample anddissolve it in water. Make it up to 250 lUI. Pipette out2S ml of the made up solution in a conical flask. Add6 to 8 g ofammonium sulphate, stir until dissolved andacidify with dilute sulphuric acid adding 1 to 2 drops ofmethyl orange indicator. Fit tbe conical flask with 8

two boles RIbberstopper C8 rryingan inlet tube extendingto the bottom of the flask 8 nd 8 n outlet tube flash withbottom of tbe stopper. Pass a rapid stream of hydrogensulphide through tbe solution rapidly for half an hourat room temperature, Allow tbe precipitate to settle for15 minutes. Then liltertbrougb Whatman No. 42 FilterPaper. Wash the precipitate with water containing alittle hydrogen sulphide. Check the washing for completehardness removal,

A-l.Z.3 Dissolve the precipitate in 30 to 40 011 ofhydrochloric acid (1 : 1) and wash the filter paper witha little water. Boil the solution to remove hydrogensulphide (test tbe vapour witb moist lead acetate paper).When hydrogen sulphide is completely removed, cool,and neutralize with sodium hydroxide using methylred indicator. Make it up to SOO ml in a volumetricflask.

A-l.Z.4 Pipette SO ml of the made up solution in 8

conical flask. AddSto6mlofammonia buffersolutionand 8 to 10 drops of eriocbrome black T indicator.

3

188149: 1994

Titnte it with EpTA solution (0.01 M). Note thevolume of EDTA consumed as V

2•

A-I.J Calculation

Zinc <as Zn), percent by mass =

where

volume of EDTA solution (0.01 M)consumed;

mass in mgof zinc per ml of EDTA solution(0.01 M); and

M2 = mass in g of sample taken for test underA-l.2.2.

Method 2

A-2 MODIFIED ETHYLENE DIAMINETETRAACETATE (EDTA) METHODS (FCOALIGNED)

A-2.1 Reagents

A-2.1.1 Disodium Ethylenediamine Tetraacetate(EDTA)

Dissolve 3.72g of disodiumethylene eIi.mine tetraacetatedihydrate in distilled water and make up the volume to1 litre in a 1 litre volumetric flask.

A-2.1..1 Standard Zinc Solution

Weigh about 1.0g of zinc metal reagentgrade acaarately.Dissolve in 20 mJ of hydrochloric acid (1 : 1), keep itfor few hours and allow it to dissolve completely.Make up tbe volume of tbe solution to exactly1·000 mi.

A-2.1.J Ammonium Hydroxide - 20 percent (m/m).

A-Z.l.i/Ammonium Chloride -AR grade.

A-Z.l.s Sodium Cyanide - AR grade.

A-%.l.6 Sodium Chloride - AR grade.

NOTE - Sodium cyanide is very poisonous. ItShould be usedwith extreme care.

A-l.t.' Eriochrome Black TIndicator Mature

Mix thoroughly 1 g of eriochrome black T indicatorwith 100 g of sodium chloride.

A-Z.t.8 Formaldehyde-Acetic Acid Solution(4 Percent)

Dissolve 100 011 of formaldehyde 37-40 (m/v) percentin about 100 mIof distilled water. Add 40 ml glacialacetic acid and make volume to 1 litre with distilledwater.

A-J.t.9 Hydroxylamine Hydrochloride -AR Grade.

188249: 19M

A·Z.z Procedure

A-2.Z.1 Standardization ofEDTA Solution

Take 10 ml ofstandard zinc solution. Add about 0.1 gof ammonium chloride and 30 mI of ammoniumhydroxide solution (20 percent). Dilute it by addingabout 30 mldistilled water. Add. pinch of eriochromeblack T indicator mixture. It will fve red colour.Titrate it with EDTA solution to obtain clear blue endpoint. Note the volume of EDTA used as VI ml.

A-Z.2.2 Estimation 01ZincinSamples

Weigh accurately 1.0gofa given zincsulphate sampleand dissolve it in 100 mJ of distiUed water in avolumetric flask. Take 10 mJ of aliquot in beaker. Add0.1 g o~ bydrox>:lamine ~ydrochloride and 0.1 g ofammomum chlonde. Cautiously add small quantity ofsodium cyanide. White~cipita1e willappear.Continueadding sodium cyanide till whiteprecipitatedisappearswhile swirling tbe beaker with band.Add about O.S gexcess of sodium cyanide. Dilute it by adding about30 mJ of ammonium hydroxide (20 percent) and addabout 30 mI of distilled water.

Add • pinch of eriochrome black T indicator mixture.It will give red colour. Titnte with EDTA solution tillthere is a sharp change to violet colour. Note thevolume of EDTA used IS V2 mi. Add 20 ml offormaldehyde-acetic acid solution to' above titratedsolution and mix well. Red colour will reappear.Titrate it with EDTA solution to get blue end pointwithout red tinge. Note the volume of EDTA used insecond titration as V) ml.

A·2.3 CALCULAnON

10)( V3

)( MZinc (as Zn), percent by mass :: -----

VI

M = mass in g of piece of zinc metal taken forpreparation of standard zinc solution,

VI = volume ofEDTA solution (in mI) used for10 ml of standard zinc solution, and

VJ == volume ofEDTA solution (in mJ) used forsecond titration.

Method 3

A-3 ABSORPTION SPECTROPHOTOMETRICMETHOD (FCO ALIGNED)

A-3.t Reagents

Unless specified otherwise, pure chemicals and glassdistilled or demineralized water sball be used in tests.

NOTE - 'Pure chemicals' shall means chemicals lbal do DOlcoDtain impurities which .ffect aberaul. of aaalysis.

4

'Demineralized water'means thewaterobtained afterpasling distilled Wlter through a cation and a anioneX~banger resinsor. combinedcation-anionexchangeresiD.

A-3.I.l Standard ZincSolution

Weigh 0.439 8 g of zinc sulphate (ZnSO4.7~O) A.R.grade on a clear watch glass and transfer it to one litreflask through the funnel giving several washings towatch glass and funnel with glass distilJed ordemineralizedwater. Add one mlofl0percentsulfuricacid (A.R.grade) and make the volume up to the mark.Stopper the flask and shake the solution well. This is100 ppm zinc solution herelnaftercalled Standard A.This solution should be stored in a clean bottle forfurtber use. Dilute 10 ml of 100 ppm solution of zinc(Standard A) to 100 ml to get 10 ppm standard zincsolution designated asStandard B.

A·3.1.2 Glass Distilled or Minera:ised Water ofpH 2.5 +0.5

Dilute 1 mI of 10 percent sulphuric acid to one litrewith glass distilled or mineralized water wand adjustthe.pH to ~.5 ~th a pH !D~ter using ~SO. or NaOH.This solution IS called acidified water and 5 to 10 litresof this soluti~n should be prepared at a time.

A-3.2 PreparatioD of Working Standards

Pipette the following volume of Standard B in '50 mJnumberedvolumetric flasks and makethe volume withacidified water (see Table 2).

Table 2 PreparatloD olWorkJng Standards

Ji1uk No. VoIaIIIe ofStudard CODceatratJOD. B takea (ml) 01 ZlDC after

maida. volume 1050JIll (ppm)

1 0.0 0.02 1.0 0.23 2.0 0.44 3.0 0.6, 4.0 0.86 s.o 1.07 7.0 1.48 9.0 1.89 10.0 2.0

A·3.3 Procedure

A-3.3.1 Preparation of ZincSulphate Fertilizer Samples

Weigh0.25 goethe materialona clean watch glass andtransfer it to one litre volumetric flask through thefunnel giving repeated washings with glass distilledwater and dissolve tbe material by shaking well. Thenmake the volume up to mark with glass distilled waterand shake well.

Take5 mJ oftbe preparedsolution in 250ml volumetricflaskand makethevolumewitbacidified water.Sbake

y

X ppm20 (X)

O.25g1 000 rnJSO times

thesolution well and filter through Whatman No. 42filter paper in dry clean Ossb. The flasks sbould berinsed with a 10 to IS ml of the filtrate and thencontinue filtration.

A-3.3.2 Flaming the Solutions

Flame the standards and the filtered samples foratomicabsorptionspectrophotometer at a wavelengthof 213.8 nm (Zn line of tbe instrument).

A-3.4 CalculatloD

Prepare a standard curve of known concentrationsofzinc solution by plotting the absorbance values ofY-axis.Calculatethe percentage zincin zincfertilizerby multiplying zinc concentration value calculatedfrom standard curve by 20.

Example:

Mass of the fertilizersampleVolume madeFurtber dilutionReadingof the samples from

atomic absorptionCorresponding, concentration

value of zinc 'from stand'lrd curveagainst Y absorbance

Percentage zinc in the fertilizer

IS824' : 1994A-3.5 Precautlou

I) WeighingmustbedoneonaD electricbalance;

b) All the glass apparatus to be used should beneutral and Wished with dilute hydrochloricacid(1 : 4)and WiShed thoroughly withdistiDedand then with demineralised water;

c) The pipette should be rimed with the samesolution to be measured;

d) The outside .of the pipette should be wipedwith filter paper after taking out from thesolution to be measured;

e) After using the pipette, place them on a cleandry fillerpaper in Older 10pevent contamination;and

f) To start filtration,only a fewdropssbould beadded first in order to wet the filter paper andthen continue further filtration.

Stopper tbe flasks and shake them well. Prepare thestandardinduplicate.Thesameacidifiedwatershouldbe usedfor preparingthesolutionofunknown fertilizersamples. Fresh standards should be prepared everytime when a fresh lot of acidified water is prepared.

ANNEXB( Table 1 )

DETERMINATION OF MAGNESIUM

B-1 REAGENTS

8-1.1 Dilute Sulphuric Acid - approximately5 N.

B-l.2 Dilute Nitric Acid -approximately 10percent(vlv).

B-l.3 Sodium Sulphide Solution - 10 percent.

B-l.4 Erlochrome Black T Indicator

Dissolve 0.1 g of eriochrome black T in 2S mJ ofmethyl alcohol.

B-1.! Dlammonlum Hydrogen Phosphate - 10percent (m/m).

B-l.6 Ammonium Hydroxide - AmmoniumChloride Buffer Solution

Mix 350 IIII of ammonium hydroxide (20 percent,m/m) with 34 g of ammonium chloride. Dilute withwater and makeup the volume to 1 000 lUI. (ThepHofthe solution should be not more than 10).

D-l.7 Standard Magnesium Solution -0.01 M.

8-1.7.1 Weigh 2.464 0 g of magnesium sulphate(MgS0

4.7H

20)and dissolve it in water. Make up the

volume to one litre.

s

8-1.1 Ethylenediamine Tetrsaeetate (EDTA)Solution

Dissolve-3.72 g of disodium ethylenediamine tetraacetatedihydrateinwaterand makeup thevolumetoone litre.

8-1.8.1 Standardization ofEDTA Solution

Take 10 mJ of standard magnesium solution in aconical flask. Add 20 ml of water, 1 ml of eriochromeblackT indicatorand 2S mIof ammonium hydroxideammonium chloride buffer solution. Heat to 40 toSOOCand tben titrate witb EDTAsolution, maintainingthe temperature between 40 and SOOC until the colourchanges from wine red to distinct blue. Calculate themolarity of EDTA solution as follows :

10M.Molarity of EDTAsolution =

where

M1

= molarity of standard magnesium solution,and

VI = volume in ml of EDTA solution used fortitration.

181249: 19M

B-2 PROCEDURE

8-%.1 Weigh accurately about S g of the Simple,dissolve inwlterandadd 1mI ofdilute sulphuric acid.Filter the solution and mike up to 250 mJ with water ina volumetric Olsk. ·rate SO mIofthe above solution inI beaker, beat, pllS hydrogen sulphide gas or addsodium sulphide solution and ensure completeprecipitation. Filter bot and keep the filtrate for thedetermination of magnesium IS given in B-2.2.Boilthe residuewithdilute nitricacidandfilterifnecessary.To the filtered solution add dilute sulphuric acid,evaporate, dilute and filter. Use the filtrate for thedetermination of copper and the residue for thedetermination of lead.

8-2.2 Tlke the filtrate obtained in B-2.1 .fterpRdplition ofsulphides, add I fewdrops of concentratatnitric acid, boil I net cool and then addsolid ammoniumchloride (about 2 g), boil IDd cool, add ammoniumhydroxide till strong smell of ammonia comes andfilter the precipitate through sintered crucible. Takethe filtrateand adddilute sulphuricacid till thesolutionis acidic (test with methy red), heat tbe solution to boilInd add excess of diammonium hydrogen phosphatewiIh continuous stirring. Add 10 percent ammoniasolution withcontinuous stirring till the solution isjustalkaline (test with methyl red); white precipitate ofzincIDUllOnium phosphate wiD be fonned (theoptimum

pH forprecipitation is6 to7).Allowit tostandfor3 to4 bours,then filter through filter paper (WhItman No.40 or equiv~lent). Collect the filtrate in a volumetricOaskand makeupthevolume (sayto 100m1), and takea suitable aliquot (say 10 mI) for the determination ofmagnesium. Add 20 ml of water, 1 ml of eriocbromeblack T indicatorand 20 mI of ammonium hydroxide­ammonium chloride butTer' solution. Heat to 40 toSOOC and titrate with standard EDTA solution,maintainingthe temperature between40 to SOOC untilthe colour cbangts from wine red to distinct blue,

B-3 CALC1JLATION

1 ml of 0.01 M EDTA. 0.243 2 mg of 'Mg'

Vx 0.2432Magnesium (IS Mg). percent by mass =----

5

where

v =- volumeof 0.01 M EDTA solution used fortitration.

8-3.1 The calculation factor S is derived presumingthat S g of material is taken for test in 8-%.1 and thefiltrate obtained in B-Z.2is 100 mIout of which 10 mJis titrated.

ANNEXC( Table 1 )

D~~ATIONOFCOWER

c-r PROCEDURE

Makeup tbe filtrate reservedinB-2.1 fordeterminationof copper, to 200 mI with water in a volumetric flask.

Take a suitable aliquot of tbe solution containing notD10re than O.OS mg of copper. Determine copper bydiethyl dithiocarblmate method or by biquinoline methodas prescribedin IS 7212 : 1974.

ANNEXO( Table 1 )

DETERMINATION OF LEAD

0-1 PROCEDURE

Dissolve the ~idue reserved in B-2.1 fordeterminationof lead, in dilute nimc acid, and make up to 8 known

volume with water in 8 volumetric flask. Take asuitable aliquot of the solution and determine lead bytbe colorimetric method using dithizone as prescribedin IS 7017 : 1973.

ANNEXE( Table 1 )

DETERMINATION OFpH

Eel PROCEDURE

Dissolve S g of tbe material in fresbly boiled Ind

cooled water,dilute to 100ml and mix. Determine thefH valueoftbe solution with apH DIeter as prescribedIn IS 5741 : 1970. .

F-l REAGENT

ANNEX F

( Table 1 )DE1'..:RMINATION or MA'I-fER INSOI ..IJBt,E IN WA1~ER

at 110 :!: SoC to constant mass.

IS 8149 : 1994

1e"-1.1 Dilute Sulphuric Afid - 10 percent.

F-l.Z Procedure

Dissolve 25.0 g oftbe material in 125 n11 of water andadd 1 ml of dilute sulphuric acid. Heat the solution inboiling. Filter through a weighed and prepared Goochcrucible or sintered glass crucible (G No.4) and washthe residuethoroughly with bot water. Drythe crucible

7

F-l.3 Calculation

Matter insoluble in water = 4A

where

A =mass in g of the residue.

Bureau or Indian Standards

SIS is a statutory institution established under the Burta" of Inditul Standturb Act, 1986 to promoteharmonious development of the activities ofstandardization, markingand qualityceniftcation of goOdsand attending to connected matters in the country.

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Review of Indian Standards

Amendments are issued to standards as the need arises on the basis of comments. Standards are alsoreviewed periodically; a standard along with amendments is reaffirmed when such review indicates thatno changesare needed; if the review indicates that changesare needed, it is taken up for revision. Usersof Indian Standards should ascertain that they are in possession of the latest amendments or edition byreferring to the latest issueof 'BIS Handbook' and 'Standards Monthly Additions'.

This Indian Standard'has been developedfrom Doc : No. P( '() 20 ( 1193 )

Amendments Issued Since Publication

Amend No.

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Date of Issue

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