IS 15121: Animal Feeding Stuffs - Determination of the Contents of Calcium, Copper, Iron, Magnesium, Manganses, Potassium, Sodium, and Zinc - Method Using Atomic Absorption Spectrometry

14 Pages·2002·1.3 MB·English

by  Bureau of Indian Standards

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IS 15121 (2002): Animal Feeding Stuffs - Determination of
the Contents of Calcium, Copper, Iron, Magnesium,
Manganses, Potassium, Sodium, and Zinc - Method Using
Atomic Absorption Spectrometry [FAD 5: Livestock Feeds,
Equipment and Systems]
“!ान $ एक न’ भारत का +नम-ण”
Satyanarayan Gangaram Pitroda
““IInnvveenntt aa NNeeww IInnddiiaa UUssiinngg KKnnoowwlleeddggee””
“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता हहहहै””ै”
Bhartṛhari—Nītiśatakam
“Knowledge is such a treasure which cannot be stolen”

IS 15121 :2002
ISO 6869:2000
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Indian Standard
ANIMAL FEEDING STUFFS — DETERMINATION OF
THE CONTENTS OF CALCIUM, COPPER, IRON,
MAGNESIUM, MANGANESE, POTASSIUM, SODIUM
AND ZINC — METHOD USING ATOMIC ABSORPTION
SPECTROMETRY
ICS 65.120

@ BIS 2002
BUREAU OF INDIAN STANDARDS
MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DEL HI 110002
April 2002 Price Group 4
Livestock Feeds Sectional Committee, FAD 5
NATIONAL FOREWORD
This Indian Standard which is identical with ISO 6869:2000 ‘Animal feeding stuffs — Determination
of the contents of calcium, copper, iron, magnesium, manganese, potassium, sodium and zinc —
Method using atomic absorption spectrometry’ issued bythe International Organization forStandardization
( ISO ) was adopted by the Bureau of Indian Standards on the recommendation of the Livestock
Feeds Sectional Committee and approval of the Food and Agriculture Division Council.
In the adopted standard, certain terminology and conventions are not identical to those used in Indian
Standards. Attention is drawn specially to the following:
a) Wherever the words ‘International Standard’ appear referring to this standard, they should be
read as ‘Indian Standard’.
b) Comma ( ,) has been used as a decimal marker while in Indian Standards, the current practice
is to use a point ( . ) as the decimal marker.
In this standard, the following International Standards are referred to. Read intheir respective place,
the following:
International Standard Corresponding Indian Standard Degree of Equivalence
ISO 6498 Animal feeding stuffs — IS 14831 : 2000 Animal feeding Identical
Preparation of test sample stuffs — Preparation of test sample
ISO 3696:1987 Water for analytical Is 1070 : 1992 Reagent grade Equivalent
laboratory use — Specification water ( third revision )
and test methods
In reporting the results of a test or analysis made in accordance with this standard, ifthe final value,
observed or calculated, isto be rounded off, itshall be done inaccordance with IS 2:1960 ‘Rules for
rounding off numerical values ( revised )’.
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IS 15121 :2002
ISO 6869:2000 ,i~’
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Indian Standard “,,
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ANIMAL FEEDING STUFFS — DETERMINATION OF
THE CONTENTS OF CALCIUM, COPPER, IRON,
i:
MAGNESIUM, MANGANESE, POTASSIUM, SODIUM .“,J
1’
AND ZINC — METHOD USING ATOMIC ABSORPTION 1I
SPECTROMETRY
1 Scope
This international Standard specifies an atomic absomtion .sDectrometricmethod for the determination of the
contents of calcium (Ca), copper (Cu), iron(Fe), magnesium (Mg), manganese (Mn), potassium (K), sodium (Na)
and zinc (Zn) inanimal feeding stuffs.
The method isapplicable toallanimal feeding stuffs. .“-Id
The limitofdetermination forthe elements concerned isasfollows:
.’
Kand Na 500 mg/kg;
Ca and Mg 50 mg/kg;
Cu, Fe, Mn and Zn 5 mg/kg.
2 Normative references
The followingnormative documents containprovisionswhich, throughreference inthistext, constitute provisionsof -----
this International Standard. For dated references, subsequent amendments to, or revisions of, any of these
publicationsdo notapply. However, parties toagreements based onthis International Standard are encouraged to
investigate the possibilityof applying the most recent editions of the normative documents indicated below. For
undated references, the latest editio n of the normative documents referred to applies. Members of ISO and IEC

maintain registersofcurrentlyvalid International Standards.

ISO 3696:1987, Water for analytical laboratory use — Specification and test methods.
ISO 6498, Animal feeding stuffs — Preparation of test samples.
3 Principle
A test portion isdissolved in hydrochloricacid, ifnecessary after ashing ina muffle furnace at (550 ~ 15) “C. Any
silica compounds present are removed by precipitation and filtration. The precipitate is dissolved in hydrochloric
acid and diluted to the desired volume, then aspirated into the air-acetylene flame of the atomic absorption
spectrometer.
The absorbance of each element is measured by comparison with the absorbance of calibration solutionsfor the
same element.
4 Reagents and materials
Use onlyreagents ofrecognized analytical grade.
4.1 Water, complyingwithat leastgrade 3 inaccordance with ISO 3696.
IS 15121 :2002
ISO 6869:2000
4.2 Concentrated hydrochloric acid, c(HCI) = 12 mol/1(p = 1,19 g/ml).
4.3 Hydrochloric acid, c(HCI) =6 mol/1.
4.4 Dilute hydrochloric acid, c(HCI) =0,6 mol/1.
4.5 Lanthanum nitrate solution.
Dissolve 133 gof La(N03)3.6H20 in1Iitreofwater (4.1).
Another lanthanum saltmay be used ifthe lanthanum contentofthe prepared solutionisthe same.
4.6 Caesium chloride solution.
Dissolve 100 gofCSCI in1Iitreofwater (4.1).
Another caesium salt maybe used ifthe caesium contentofthe obtained solutionisthe same.
4.7 Stock solution of Cu, Fe, Mn and Zn.
Mix 100 mlofwater (4.1) and 125 mlofconcentrated hydrochloricacid (4.2) ina 1Iitrevolumetricflask.
Weigh outthe following:
— 392,9 mg ofCopper(n)Sulfatepentahydrate (CuS04”5H@);
— 702,2 mg ofammonium iron(n)sulfate hexahydrate [(NH4)2S04.FeS04 ”6H20];
— 307,7 mgofmanganese sulfate monohydrate (MnS04”H20);
— 439,8 mg ofzinc sulfate heptahydrate (ZnS04.7H20).
Transfer the weighed saltstothe volumetricflaskand dissolvethem inwater (4.1). Dilute tothe mark withwater.

The contents ofCu, Fe, Mn and Zn of thisstocksolutionare each 100 pg/ml.

NOTE Ready-preparedcommerciallyavailablesolutionsmaybeused.
4.8 Standard solution of Cu, Fe, Mn and Zn.
Dilute20,0 mlofthe stocksolution(4.7) withwater (4.1) to 100 mlina volumetricflask.
The contentsofCu, Fe, Mn and Zn ofthissolutionare each 20 pg/ml.
Prepare the solutionfresh onthe day ofuse.
4.9 Stock solution of Ca, K, Mg and Na.
Weigh outthefollowing:
— 1,907 gofpotassium chloride(KCI);
— 2,028 gofmagnesium sulfate heptahydrate (MgS04”7H20);
— 2,542 gofsodium chloride(NaCl).
Transfer the weighed saltstoa 1Iitrevolumetricflask.
IS 15121 :2002
1
ISO 6869:2000
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Add 50 mlof hydrochloricacid (4.3) toa beaker. Weigh intothe beaker 2,497 gofcalcium carbonate (CaC03). 1.
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CAUTION: Beware of the development of carbon dioxide.
Boil for 5 min on an electric hot plate (5.4). Cool and transfer the solution to the volumetric flask containing the
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weighed saltsofK, Mg and Na. Dissolvethe saltsand dilutetothe mark withdilutehydrochloricacid (4.4). :,:!
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The contentsofCa, Kand Na ofthissolutionare each 1mg/ml;the content ofMg ofthe solutionis200 Kg/ml. .!
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NOTE Ready-preparedcommerciallyavailablesolutionsmaybeused.
4.10 Standard solution of Ca, K, Mg and Na.
Dilute25,0 mlofstocksolution(4.9) withdilutehydrochloricacid (4.4) to250 ml ina volumetric flask.
The contentsofCa, Kand Na ofthissolutionare each 100 ~g/ml;the content ofMg ofthe solutionis20 ~g/ml.
Prepare the solutionfresh inthe week ofuseand storeitina polyethylene bottle.
4.11 Lanthanum/caesium blank solution
Add 5 ml of lanthanum nitrate solution(4.5), 5 ml of caesium chloride solution (4.6) and 5 ml of hydrochloricacid
(4.3) toa 100 mlvolumetricflask. Dilutetothe markwithwater (4.1).
5 Apparatus
Rinse all volumetric ware, including the pipettes used for preparing calibration solutions, with dilute hydrochloric
acid (4.4) before use.
Ifdedicated incineration dishes and glassware are used, itisnotnecessary to boilwith hydrochloricacideach time
--
before use. --”
Usual laboratoryapparatus and, inparticular,thefollowing,
,

5.1 Analytical balance, capable ofweighingtothe nearest 0,1 mg.

5.2 Incineration dishes of platinum, quartz or porcelain, free from potassium and sodium, with a smooth
unetched inner surface, upper internaldiameter 4 cm to6cm, lower internaldiameter 2 cm to 2,5 cm, and a height
ofabout 5cm. Before use, boilwithhydrochloricacid(4.3).
5.3 Glassware ofhard borosilicateglass.
Before use, boilwithhydrochloricacid (4.3) and rinsewithwater.
5.4 Electric hot plate orgas burner.
5.5 Boiling water bath.
5.6 Electric muffle furnace, capable ofbeingmaintained at (550 &15) “C,
$.7 Atomic absorption spectrometer (see ISO 6956 [6]), suitableformeasuring atthe wavelengths specified in
8.6.1 and 8.7.1, provided with an air-acetylene flame and a facility for correction for, or measurement of,
background absorption.
5.8 Hollow cathode lamps or electrode-less discharge lamps, for the determination of Ca, Cu, Fe, K, Mg,
Mm Na orZn.
5.9 Filter paper whichdoes notrelease minerals.

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IS 15121 :2002
ISO 6869:2000
6 Sampling
Sampling is not part of the method specified in this International Standard. A recommended sampling method is
given inISO 6497 [5].
It is important that the laboratory receive a sample which is truly representative and has not been damaged or
changed duringtransportorstorage.
Store the sample sothat deterioration and otherchanges incompositionare prevented.
7 Preparation of test sample
Prepare the testsample inaccordance withISO 6498.
8 Procedure
8.1 Detection of presence of organic matter
Heat aspatula withsome test sample inaflame.
Ifthetest sample meltswithoutsmoke, littleorganic matter ispresent.
Ifthe testsample changes incolourand meltingdoes notoccur,the test sample contains organic matter.
8.2 Test potiton
Depending on the expected content, weigh 1gto5g ofthe prepared test sample (clause 7), to the nearest 1mg,
intoan incinerationdish(5.2).
Ifthe testsample contains organicmatter (see 8.1), proceed inaccordance with8.3.
Ifthe testsample contains littleornoorganicmatter (see 8.1), proceed inaccordance with8.4.

8.3 Dry ashing
Heat the incineration dish on a hot plate or over a gas burner (5.4) until the test portion has been completely
carbonized. Avoid burningthe test portion.
Transfer the dishtothe mufflefurnace (5.6) which has already been at a temperature of 550 “Cfor 15 min. Ashthe
sample for3 hat thistemperature.
Allow the sample to cool down then moisten the contents of the dish with 2 ml of water. If many carbon particles
are present, drythe dishover the water bath (5.5).
Ashforanother 2 hinthe mufflefurnace setat550 “C.
Allowtocooldown then add 2 mlofwater.
8.4 Decomposition
While swirling, add 10 ml of hydrochloric acid (4.3), first dropwise until effervescence (possible development of
carbon dioxide) has ceased, then faster. Swirl and heat the contents ofthe dishuntilalmost dry.Wbiledrying,take
care toavoid lossbysplattering.

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IS 15121 :2002 ‘,.
ISO 6869:2000
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Dissolve the residue by heating with 5ml of hydrochloric acid (4.3) and transfer the solution quantitatively with
some 5 mlportionsofwater toa 50 mlvolumetricflask.
Allowtocool, then dilutetothe mark withwater and mix.Allowthe particlestosettle and filter(see 5.9) the solution
f.
ifitisnotclear after 4 h.
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8.5 Blank solution
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Prepare for each measuring series a blank solution by carrying out the procedure according to 8.2, 8.3 and 8.4
withoutthe test sample.
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8.6 Determination of copper, iron, manganese and zinc
8.6.1 Measuring conditions
Adjust the atomic absorption spectrometer (5.7) in accordance with the manufacturer’s instructions. Optimize the
response ofthe instrumentfor measurement withthe air-acetylene flame. Forthe determination of Cu, Fe, Mn and
Zn setthefollowingwavelengths:
Cu: 324,8 nm;
Fe: 248,3 nm;
Mn: 279,5 nm;
Zn: 213,8 nm.
8.6.2 Preparation of calibration curve
Prepare a series of appropriate calibration solutionsbydilutingthe standard solution (4.8) with dilute hydrochloric
acid (4.4).
Measure the absorbance of the hydrochloricacid (4.4). Measure the absorbance of the calibration solutions and
subtractthe absorbance measured fo rthe hydrochloricacid (4.4).

Draw a calibration cuwe by plottingthe corrected absorbance against the respective contents of Cu, Fe, Mn and
Zn.
8.6.3 Measurement of test solution
Measure parallel to the calibration solutions, under identical circumstances, the absorbance of the test solution
(8.4) and the blank solution(8.5). Subtract the latterabsorbance fromthefirstabsorbance.
If necessary, dilute a quantity ofthe test solutionand blank solutionwith dilute hydrochloricacid (4.4) to obtain an
absorbance inthe linear partofthe calibrationcurve.
Proceed inaccordance withclause 9.

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