UGANDA STANDARD  
      US ISO 6869
First Edition
   2009 -09-04
 
Reference numbe r 
  US ISO 6869:2000
 © UNBS 200 9 
  
Animal feeding stuffs — Determination of the contents of 
calcium, copper, iron, magnesium, manganese, potassium, 
sodium and zinc — Method using atomic absorption 
spectrometry 
 US ISO 6869:2000  
 
© UNBS  2009 – All rights reserved Compliance with this standard does not, of itself confer immunity from legal obligations 
A Uganda Standard does not purport to include all necessary provisions of a contract. Users are 
responsible for its correct application  
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E-mail: unbs@infocom.co.ug
    US ISO 6869:2000  
© UNBS  2009 - All rights reserved National foreword 
Uganda National Bureau of Standards (UNBS) is a parastatal under the Ministry  of Tourism, Trade and 
Industry established by the Act of Parliament of 198 3, of the Laws of Uganda.  UNBS is mandated to co-
ordinate the elaboration of standards and is  
(a) a member of International Organisation for Standardisation (ISO) and  
(b) a contact point for the WHO/FAO Codex A limentarius Commission on Food Standards, and  
(c) the National Enquiry Point on TBT/SPS Agr eements of the World Trade Organisation (WTO). 
The work of preparing Uganda Standards is carried out through Technical Committees. A Technical 
Committee is established to deliberate on standards in a gi ven field or area and consists of representatives of 
consumers, traders, academician s, manufacturers, governme nt and other stakeholders. 
Draft Uganda Standards adopted by the Technical Committ ee are widely circulated to stakeholders and the 
general public for comments. The committee reviews the comments before recommending the draft standards 
for approval and declaration as Uganda Standards by the National Standards Council. 
This Uganda Standard, US 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, is identical with and  has been reproduced from an International Standard ISO
6869:2000,  Animal feeding stuffs — Determination of t he contents of calcium, copper, iron, magnesium,
manganese, potassium, sodium and zinc — Method  using atomic absorption spectrometry, and has been
adopted as a Uganda Standard . 
Wherever the words, "International Standard" a ppear, they should be replaced by "Uganda Standard." Reference number
ISO6869:2000(E)
©ISO2000INTERNATIONAL
STANDARDISO
6869
Firstedition
2000-12-01
Animal feedingstuffs— Determination
ofthe contents ofcalcium, copper, iron,
magnesium, manganese, potassium,
sodiumandzinc — Methodusing atomicabsorptionspectrometr
y
Aliments des animaux — Déterminationdes teneurs encalcium, cuivre, fer,
magnésium, manganèse, potassium, sodiumet zinc— Méthodeparspectrométried'absorption atomiqueISO 6869:2000(E)
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ii © ISO2000 –All rights reservedISO 6869:2000(E)
© ISO2000 –All rights reserved iiiContents
Foreword....................................................................................................................... ..............................................iv
1 Scope......................................................................................................................... .....................................1
2 Normativereferences........................................................................................................... .........................1
3 Principle..................................................................................................................... .....................................1
4 Reagents and materials.......................................................................................................... ......................1
5 Apparatus..................................................................................................................... ..................................3
6 Sampling...................................................................................................................... ...................................4
7 Preparation of test sample....................................................................................................... .....................4
8 Procedure..................................................................................................................... ..................................4
8.1 Detection of presenceof organicmatter.......................................................................................... ...........4
8.2 Test portion................................................................................................................. ...................................4
8.3 Dryashing................................................................................................................... ...................................4
8.4 Decomposition............................................................................................................... ................................4
8.5 Blanksolution............................................................................................................... .................................5
8.6 Determination of copper,iron,manganeseand zinc................................................................................. 5
8.7 Determination of calcium,magnesium,potassium and sodium..............................................................6
9 Expression of results........................................................................................................... .........................6
10 Precision.................................................................................................................... .....................................7
10.1 Interlaboratorytests....................................................................................................... ...............................7
10.2 Repeatability.............................................................................................................. .....................................7
10.3 Reproducibility............................................................................................................ ...................................8
11 Test report................................................................................................................... ...................................8
Annex A (informative) Resultsof interlaboratorytests...........................................................................................9
Bibliography................................................................................................................... ...........................................15ISO 6869:2000(E)
iv © ISO2000 –All rights reservedForeword
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO
member bodies). The work of preparing International Standards is normally carried out through ISO technical
committees. Each member body interested in a subject for which a technical committee has been established hasthe right to be represented on that committee. International organizations, governmental and non-governmental, inliaison with ISO, also take part in the work. ISO collaborates closely with the International ElectrotechnicalCommission(IEC) onall matters of electrotechnicalstandardization.
InternationalStandards are drafted in accordance with the rules givenintheISO/IEC Directives, Part3.
Draft International Standards adopted by the technical committees are circulated to the member bodies for voting.
Publicationas anInternationalStandardrequires approval byat least 75% of themember bodies casting a vote.
Attention is drawn to the possibility that some of the elements of this International Standard may be the subject of
patent rights. ISO shall not beheldresponsiblefor identifyinganyor allsuch patent rights.
International Standard ISO6869 was prepared by Technical Committee ISO/TC34, Food products , Subcommittee
SC 10,Animalfeedingstuffs .
Annex A of this International Standardis for informationonly.INTERNATIONAL STANDARD ISO 6869:2000(E)
© ISO2000 –All rights reserved 1Animalfeedingstuffs —Determinationofthe contents ofcalcium,
copper, iron, magnesium, manganese, potassium, sodium
andzinc —Methodusing atomic absorptionspectrometry
1 Scope
This International Standard specifies an atomic absorption spectrometric method for the determination of the
contents of calcium (Ca), copper (Cu), iron (Fe), magnesium (Mg), manganese (Mn), potassium (K), sodium (Na)
and zinc (Zn) in animalfeeding stuffs.
Themethodis applicableto allanimalfeedingstuffs.The limit of determination for the elements concerned is as follows:
KandNa 500mg/kg;
CaandMg 50mg/kg;
Cu,Fe, Mn and Zn 5mg/kg.
2 Normative references
The following normative documents contain provisions which, through reference in this text, constitute provisions of
this International Standard. For dated references, subsequent amendments to, or revisions of, any of thesepublications do not apply. However, parties to agreements based on this International Standard are encouraged toinvestigate the possibility of applying the most recent editions of the normative documents indicated below. Forundated references, the latest edition of the normative documents referred to applies. Members of ISO and IEC
maintain registers of currentlyvalid InternationalStandards.
ISO3696:1987, Water for analytical laboratory use —Specificationandtest methods.
ISO 6498, Animalfeedingstuffs —Preparation of test samples .
3P r i n c i p l e
A test portion is dissolved in hydrochloric acid, if necessary after ashing in a muffle furnace at (550 /Gb115)°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 absorptionspectrometer.
The absorbance of each element is measured by comparison with the absorbance of calibration solutions for the
sameelement.
4 Reagents andmaterials
Useonlyreagents of recognized analyticalgrade.
4.1 Water ,complying with at least grade3 inaccordance with ISO3696.ISO 6869:2000(E)
2 © ISO2000 –All rights reserved4.2 Concentrated hydrochloric acid ,c(HCl)=12mol/l( /G72=1,19g/ml ).
4.3 Hydrochloric acid ,c(HCl) =6mol/l.
4.4 Dilutehydrochloric acid ,c(HCl)=0,6mol/l.
4.5 Lanthanum nitratesolution .
Dissolve133g of La(NO 3)3·6H2Oi n1l i t r eo fw a t e r( 4 .1 ) .
Another lanthanum salt maybeused if the lanthanum content of thepreparedsolution is thesame.
4.6 Caesium chloridesolution .
Di ssolv e100gofCsCli n1l itreofw ater(4.1).Another caesium salt maybeusedif the caesium content of the obtainedsolution is thesame.
4.7 Stocksolution of Cu,Fe,Mn and Zn .
Mix 100mlof water (4.1) and 125ml of concentratedhydrochloric acid (4.2) ina 1 litre volumetric flask.
Weighout thefollowing:
/Gbe392,9mgof copper(II) sulfate pentahydrate(CuSO
4·5H2O);
/Gbe702,2mgof ammonium iron(II) sulfatehexahydrate[(NH 4)2SO4.FeSO4·6H2O];
/Gbe307,7mgof manganesesulfate monohydrate(MnSO 4·H2O);
/Gbe439,8mgof zinc sulfate heptahydrate(ZnSO 4·7H2O).
Transfer the weighedsalts tothe volumetric flask anddissolvethem in water (4.1). Dilute tothemark with water.
Thecontents of Cu, Fe, MnandZn of this stock solution areeach 100 /G6dg/ml.
NOTE Ready-preparedcommerciallyavailable solutions maybe used.
4.8 Standard solutionof Cu,Fe,MnandZn.
Dilute 20,0mlof thestock solution(4.7) with water (4.1) to 100ml in a volumetric flask.
Thecontents of Cu, Fe, MnandZn of this solution areeach20 /G6dg/ml.
Prepare the solutionfreshon the dayof use.
4.9 Stocksolution of Ca,K,Mg and Na.
Weighout thefollowing:
/Gbe1,907g of potassium chloride(KCl);
/Gbe2,028g of magnesium sulfateheptahydrate(MgSO 4·7H2O);
/Gbe2,542g of sodium chloride(NaCl).
Transfer the weighedsalts to a1litre volumetric flask.ISO 6869:2000(E)
© ISO2000 –All rights reserved 3Add 50ml of hydrochloric acid(4.3) to abeaker.Weighintothebeaker 2,497g of calcium carbonate(CaCO 3).
CAUTION: Bewareof thedevelopment of carbon dioxide.
Boil for 5min on an electric hot plate (5.4). Cool and transfer the solution to the volumetric flask containing the
weighed salts of K, Mg and Na. Dissolve the salts and dilute to the mark with dilute hydrochloric acid (4.4).
Thecontents of Ca, K andNaof this solutionare each1mg/ml; thecontent of Mgof thesolution is 200 /G6dg/ml.
NOTE Ready-preparedcommerciallyavailable solutions maybe used.
4.10 Standard solution of Ca,K,Mg and Na .
Dilute 25,0mlof stock solution(4.9) withdilute hydrochloric acid(4.4) to 250ml in avolumetric flask.
Thecontents of Ca, K andNaof this solutionare each100 /G6dg/ml; thecontent of Mg of thesolution is 20 /G6dg/ml.
Prepare the solutionfreshin the week of useand storeit ina polyethylene bottle.
4.11 Lanthanum/caesiumblank solution
Add 5ml of lanthanum nitrate solution (4.5), 5ml of caesium chloride solution (4.6) and 5ml of hydrochloric acid
(4.3) to a100mlvolumetric flask. Dilute tothemark with water (4.1).
5 Apparatus
Rinse all volumetric ware, including the pipettes used for preparing calibration solutions, with dilute hydrochloricacid(4.4) beforeuse.
If dedicated incineration dishes and glassware are used, it is not necessary to boil with hydrochloric acid each time
beforeuse.
Usual laboratoryapparatus and, in particular, thefollowing.
5.1 Analyticalbalance, capable of weighing tothenearest 0,1mg.
5.2 Incineration dishes of platinum, quartz or porcelain, free from potassium and sodium, with a smooth
unetched inner surface, upper internal diameter 4cm to 6cm, lower internal diameter 2cm to 2,5cm, and a height
of about 5cm. Beforeuse, boil withhydrochloric acid(4.3).
5.3 Glassware of hardborosilicate glass.
Beforeuse, boil with hydrochloric acid(4.3) andrinse with water.
5.4 Electrichot plate orgasburner.
5.5 Boiling waterbath.
5.6 Electricmufflefurnace , capableof being maintainedat (550 /Gb115)°C.
5.7 Atomic absorptionspectrometer (seeISO6956[6]), suitablefor measuringat the 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,
backgroundabsorption.
5.8 Hollow cathode lamps orelectrode-less discharge lamps , for the determination of Ca, Cu, Fe, K, Mg,
Mn, Naor Zn.
5.9 Filterpaper which does not release minerals.ISO 6869:2000(E)
4 © ISO2000 –All rights reserved6 Sampling
Sampling is not part of the method specified in this International Standard. A recommended sampling method is
given in ISO 6497 [5].
It is important that the laboratory receive a sample which is truly representative and has not been damaged or
changedduringtransport or storage.
Store thesamplesothat deteriorationand other changes in composition areprevented.
7 Preparationoftestsample
Prepare the test sampleinaccordance withISO6498.
8 Procedure
8.1 Detectionofpresenceoforganicmatter
Heat aspatula withsometest samplein aflame.If thetest samplemelts without smoke, little organic matter is present.If thetest samplechanges incolour andmelting does not occur, thetest samplecontains organic matter.
8.2 Test portion
Depending on the expected content, weigh 1gto5g of the prepared test sample (clause7), to the nearest 1mg,
into an incinerationdish(5.2).
If thetest samplecontains organic matter (see8.1), proceedinaccordance with8.3.If thetest samplecontains littleor noorganic matter (see8.1), proceed in accordance with 8.4.
8.3 Dryashing
Heat the incineration dish on a hot plate or over a gas burner (5.4) until the test portion has been completely
carbonized. Avoid burningthetest portion.
Transfer the dish to the mufflefurnace (5.6) which has alreadybeen at a temperature of 550 °C for 15min. Ash the
samplefor 3hat this temperature.
Allow the sample to cool down then moisten the contents of the dish with 2ml of water. If many carbon particles
arepresent, drythedishover the water bath(5.5).
Ashfor another 2h inthemufflefurnaceset at 550 °C.
Allowtocooldown thenadd 2ml of water.
8.4 Decomposition
While swirling, add 10ml of hydrochloric acid (4.3), first dropwise until effervescence (possible development of
carbon dioxide) has ceased, then faster. Swirl and heat the contents of the dish until almost dry. While drying, takecaretoavoid loss bysplattering.ISO 6869:2000(E)
© ISO2000 –All rights reserved 5Dissolve the residue by heating with 5ml of hydrochloric acid (4.3) and transfer the solution quantitatively with
some5mlportions of water to a50mlvolumetric flask.
Allow to cool, then dilute to the mark with water and mix. Allow the particles to settle and filter (see 5.9) the solution
if it is not clear after 4 h.
8.5 Blank solution
Prepare for each measuring series a blank solution by carrying out the procedure according to 8.2, 8.3 and 8.4without thetest sample.
8.6 Determination of copper, iron, manganeseand zinc
8.6.1 Measuring conditions
Adjust the atomic absorption spectrometer (5.7) in accordance with the manufacturer's instructions. Optimize the
response of the instrument for measurement with the air-acetylene flame. For the determination of Cu, Fe, Mn andZnset thefollowing wavelengths:
Cu: 324,8nm;Fe: 248,3nm;Mn: 279,5nm;
Zn: 213,8nm.
8.6.2 Preparation of calibration curve
Prepare a series of appropriate calibration solutions by diluting the standard solution (4.8) with dilute hydrochloric
acid(4.4).
Measure the absorbance of the hydrochloric acid (4.4). Measure the absorbance of the calibration solutions and
subtract the absorbancemeasuredfor the hydrochloric acid(4.4).
Draw a calibration curve by plotting the corrected absorbances 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) andtheblank solution(8.5). Subtract thelatter absorbancefrom thefirst absorbance.
If necessary, dilute a quantity of the test solution and blank solution with dilute hydrochloric acid (4.4) to obtain an
absorbanceinthelinear part of thecalibrationcurve.
Proceed in accordance with clause9.ISO 6869:2000(E)
6 © ISO2000 –All rights reserved8.7 Determination of calcium, magnesium, potassiumand sodium
8.7.1 Measuring conditions
Adjust the atomic absorption spectrometer in accordance with the manufacturer's instructions. Optimize the
response of the instrument for measurement with the air-acetylene flame. For the determination of Ca, K, Mg andNasetthefollowing wavelengths:
Ca: 422,6nm;K: 766,5nm;
Mg: 285,2nm;
Na: 589,6nm.
8.7.2 Preparation of calibration curve
Dilute the standard solution (4.10) with water (4.1). Add per 100ml of diluted standard solution 5ml of lanthanum
nitrate solution (4.5), 5ml of caesium chloride solution (4.6) and 5ml of hydrochloric acid (4.3). Choose thedilutions sothat appropriatecalibrationsolutions areobtained.
Measure the absorbanceof thelanthanum/caesium blank solution(4.11).
Measure the absorbance of the calibration solutions and subtract the absorbance measured for the
lanthanum/caesium blank solution (4.11).
Draw a calibration curve by plotting the corrected absorbances against the respective contents of Ca, K, Mg and
Na.
8.7.3 Measurement of test solution
Dilute a quantity of the test solution (8.4) and blank solution (8.5) with water (4.1). Add per 100ml of diluted
solution 5ml of lanthanum nitrate solution (4.5), 5ml of caesium chloride solution (4.6) and 5ml of hydrochloricacid(4.3).
Measure parallel to the calibration solutions, under identical circumstances, the absorbance of the diluted test
solution and the diluted blank solution. Subtract thelatter absorbancefrom thefirst absorbance.
If necessary, dilute a quantity of the test solution and blank solution with lanthanum/caesium blank solution (4.11)
toobtainanabsorbance inthe linear part of thecalibrationcurve.
9 Expression of results
Calculate the content of each of the elements calcium, copper, iron, magnesium, manganese, potassium, sodium
and zinc starting from the calibration curve and taking into account the mass of the test portion and the dilutionsapplied.
Round the result in accordance with Table1 and express the result inmilligrams per kilogram or grams per
kilogram.ISO 6869:2000(E)
© ISO2000 –All rights reserved 7Table1—Roundingof thecalculated content
Content
from toRoundto
5mg/kg 10mg/kg 0,1mg/kg
10mg/kg 100mg/kg 1mg/kg
100mg/kg 1g/kg 10mg/kg
1g/kg 10g/kg 100mg/kg
10g/kg 100 g/kg 1g/kg
10 Precision
10.1 Interlaboratorytests
Details of interlaboratory tests on the precision of the method are given in annexA. The values derived from these
tests maynot be applicabletoconcentrationranges andmatrices other thanthosegiven.
10.2 Repeatability
The absolute difference between two independent single test results, obtained using the same method on identicaltest material in the same laboratory by the same operator using the same equipment within a short interval of time,
willinnot morethan 5% of cases exceedtherepeatabilitylimit ( r) mentioned in or derivedfrom Table2or Table3.
Table2—Repeatabilitylimit (r)and reproducibilitylimit (R)forpremixes
Values inmilligramsperkilogram
Element content
Element
from torR
Ca 3000 300 000 0,07/Gb4w 0,20/Gb4w
Cu 200 20000 0,07/Gb4w 0,13/Gb4w
Fe 500 30000 0,06/Gb4w 0,21/Gb4w
K 2500 30000 0,09/Gb4w 0,26/Gb4w
Mg 1000 100 000 0,06/Gb4w 0,14/Gb4w
Mn 150 15000 0,08/Gb4w 0,28/Gb4w
Na 2000 250 000 0,09/Gb4w 0,26/Gb4w
Zn 3500 15000 0,08/Gb4w 0,20/Gb4w
wis the meanof the two results, inmilligrams perkilogram.ISO 6869:2000(E)
8 © ISO2000 –All rights reservedTable3—Repeatabilitylimit (r)and reproducibilitylimit (R)foranimal feeds
Values inmilligramsperkilogram
Element content
Element
from torR
Ca 5000 50000 0,07/Gb4w 0,28/Gb4w
Cu 10 100 0,27/Gb4w 0,57/Gb4w
Cu 100 200 0,09/Gb4w 0,16/Gb4w
Fe 50 1500 0,08/Gb4w 0,32/Gb4w
K 5000 30000 0,09/Gb4w 0,28/Gb4w
Mg 1000 10000 0,06/Gb4w 0,16/Gb4w
Mn 15 500 0,06/Gb4w 0,40/Gb4w
Na 1000 6000 0,15/Gb4w 0,23/Gb4w
Zn 25 500 0,11/Gb4w 0,19/Gb4w
wis the meanof the two results, inmilligrams perkilogram.
NOTE In Table 2 and Table 3, the repeatability and reproducibility limits are given in the form of a formula for each element
and for the indicated range. The factor in this formula is an average over the investigated samples in the indicated range. In
exceptional cases higher values have been obtained for the determination of a specific element in specific samples. These
samples have not been taken into account. Most likely cause of these deviations is lack of homogeneity of the samples
concerned (see annexA).
10.3 Reproducibility
The absolute difference between two single test results, obtained using the same method on identical test material
in different laboratories by different operators using different equipment, will in not more than 5% of cases exceed
the reproducibilitylimit ( R) mentioned in or derivedfrom Table2 or Table3.
11 Testreport
Thetest report shallspecify:
/Gbeall information necessaryfor the complete identification of the sample;
/Gbethesamplingmethodused, if known;
/Gbethetest methodused, withreferencetothis International Standard;
/Gbeall operating details not specified in this International Standard, or regarded as optional, together with details of
anyincidents whichmayhave influenced the test result(s);
/Gbethetest result obtained, or thetwo test results obtained if therepeatabilityhas beenchecked.ISO 6869:2000(E)
© ISO2000 –All rights reserved 9Annex A
(informative)
Results ofinterlaboratorytests
Starting in 1983, the precision of the method has been tested by several interlaboratory tests carried out on mixed
feeds and premixes in accordance with ISO5725:1986[2]. The statistical results of a first series of tests were
published in reference[7]. As a consequence of the results of these tests, the method was modified. The precisionof themodifiedmethod was establishedbytwo interlaboratorytests.
In the first test (in the period 1986-1987) 26laboratories from 7countries participated. Samples were investigated
of a premix, two mixed feeds, barley, wilted silage, milk powder and pigs ’faeces. In view of the unsatisfactory
results for premixes, it was decided to amend the method for premixes. The precision of the amended method for
premixes was established by an additional interlaboratorytest.
In this second test (in the period 1987-1988), 13laboratories participated. Samples were investigated of eight
premixes (five of which contained organic matter).
Thestatistical results of thetwointerlaboratorytests aresummarized inTablesA.1toA.8.ISO 6869:2000(E)
10 © ISO2000 –All rights reservedTableA.1 —Statistical resultsfor calcium
Parameterb
w srCVr r sRCVR R Samplean1 n2 n3
mg/kg mg/kg % mg/kg mg/kg % mg/kg
P1 12 0 24 51 000 1 413 2,9 4 000 5 654 10,9 16 000
P2 12 2 22 292 000 6 007 2,1 17 000 16 254 5,7 46 000
P3 12 2 22 136 000 2 120 1,6 6 000 12 367 9,0 35 000
PO1 12 0 24 156 000 2 120 1,3 6 000 10 247 6,5 29 000
PO2 12 2 22 11 900 389 3,2 1 100 636 5,5 1 800
PO3 12 2 22 3 000 106 3,8 300 247 8,6 700
PO4 12 0 24 7 900 177 2,1 500 530 6,9 1 500
PO5 12 0 24 5 700 141 2,4 400 318 5,9 900
B 21 8 34 592 62 10,4 175 179 30,3 507
WS 21 8 34 4 860 130 2,7 369 604 12,4 1 710
MFH 21 10 32 7 650 195 2,6 552 753 9,8 2 130
MP 21 6 36 13 300 417 3,1 1 180 1 484 11,1 4 200
PF 21 2 40 33 200 565 1,7 1 600 6 855 20,6 19 400
MFL 21 9 33 47 400 1 106 2,3 3 130 3 424 7,2 9 690
aP1 is premix;
P2 is premix;
P3 is premix;PO1 is premixcontaining organic matter;PO2 is premixcontaining organic matter;PO3 is premixcontaining organic matter;PO4 is premixcontaining organic matter;
PO5 is premixcontaining organic matter;
B is barley;WS is wiltedsilage;MFH is mixed feed H;MP is milkpowder;PF is pigs ’faeces;
MFL is mixed feed L;
bn1is the numberof laboratories with results;
n2is the numberof outliers;
n3is the numberof accepted results;
wis themean calciumcontent of thesample;
sris the repeatabilitystandard deviation;
CVr is the repeatabilitycoefficient of variation;
ris the repeatability limit [ r=2 ,8 /Gb4sr];
sRis the reproducibilitystandard deviation;
CVR is the reproducibilitycoefficient of variation;
Ris the reproducibility limit [ R=2 ,8 /Gb4sR].ISO 6869:2000(E)
© ISO2000 –All rights reserved 11TableA.2 —Statisticalresultsfor copper
Parameterb
w srCVr r sRCVR R Samplean1 n2 n3
mg/kg mg/kg % mg/kg mg/kg % mg/kg
P1 13 0 26 900 25 2,7 70 64 7,0 180
P2 13 0 26 1 000 28 2,8 80 67 6,8 190
P3 13 0 26 17 400 212 1,2 600 495 2,9 1 400
PO1 13 0 26 4 540 78 1,7 220 152 3,3 430
PO2 13 0 26 217 6,4 2,9 18 10 4,7 29
PO3 13 2 24 1 050 57 5,4 160 141 13,5 400
PO4 13 0 26 6 660 251 3,8 710 293 4,4 830
PO5 13 0 26 39 100 495 1,2 1 400 1 555 3,1 4 400
B 22 6 38 6 0,4 8,4 1 1,4 21,3 4
WS 22 4 40 14 1,1 7,0 3 2,1 15,9 6
MFH 22 4 40 15 2,1 14,5 6 3,5 23,8 10
MP 22 4 40 2 0,4 19,4 1 1,4 61,7 4
PF 22 10 34 224 4,9 2,2 14 11 5,0 32
MFL 22 4 40 118 5,3 4,6 15 7,4 6,3 21
a, bSee Table A.1, except that wisthemean coppercontent.
TableA.3 —Statistical resultsfor iron
Parameterb
w srCVr r sRCVR R Samplean1 n2 n3
mg/kg mg/kg % mg/kg mg/kg % mg/kg
P1 12 2 22 7 500 141 1,9 400 565 7,3 1 600
P2 12 2 22 22 600 565 2,5 1 600 1 555 6,9 4 400
P3 12 0 24 31 000 707 2,4 2 000 2 473 8,5 7 000
PO1 12 0 24 4 000 106 3,0 300 318 8,3 900
PO2 12 0 24 500 18 3,7 50 28 6,0 80
PO3 12 0 24 9 600 212 2,2 600 636 6,7 1 800
PO4 12 4 20 18 600 177 0,9 500 1 166 6,2 3 300
PO5 12 0 24 19 000 353 2,6 1 000 2 120 11,1 6 000
B 21 4 38 79 2,8 3,7 8 11 13,9 31
WS 21 8 34 599 10 1,7 29 70 11,6 197
MFH 21 2 40 362 59 16,2 166 85 23,5 241
MP 21 4 38 8 2,5 30,5 7 5,7 68,5 16
PF 21 4 38 3 430 86 2,5 244 491 14,4 1 390
MFL 21 6 36 1 290 40 3,1 113 111 8,6 315
a, bSee Table A.1, except that wisthemean iron content.ISO 6869:2000(E)
12 © ISO2000 –All rights reservedTableA.4 —Statisticalresultsfor magnesium
Parameterb
w srCVr r sRCVR R Samplean1 n2 n3
mg/kg mg/kg % mg/kg mg/kg % mg/kg
P1 12 0 24 111 000 2 120 1,9 6 000 5 654 5,2 16 000
P2 12 2 22 18 000 106 0,5 300 742 4,2 2 100
P3 12 0 24 2 050 53 2,5 150 152 7,4 430
PO1 12 2 22 5 770 113 2,0 320 145 2,5 410
PO2 12 2 22 1 640 28 1,7 80 49 3,2 140
PO3 12 0 24 1 000 32 3,2 90 67 6,6 190
PO4 12 0 24 1 670 42 2,5 120 110 6,6 310
PO5 12 2 22 1 650 28 1,6 80 71 4,2 200
B 22 10 34 1 200 34 2,8 95 58 4,8 163
WS 22 8 36 2 260 80 3,5 226 128 5,7 363
MFH 22 8 36 1 640 45 2,7 126 120 7,3 340
MP 22 4 40 1 250 94 7,5 265 147 11,8 417
PF 22 8 36 9 980 128 1,3 362 576 5,8 1 630
MFL 22 10 34 3 040 27 0,9 76 143 4,7 405
a, bSee Table A.1, except that wisthemean magnesiumcontent.
TableA.5 —Statisticalresultsfor manganese
Parameterb
w srCVr r sRCVR R Samplean1 n2 n3
mg/kg mg/kg % mg/kg mg/kg % mg/kg
P1 13 0 26 2 600 71 3,3 200 318 12,0 900
P2 13 0 26 4 800 106 2,6 300 742 15,6 2 100
P3 13 0 26 10 100 247 2,4 700 883 8,8 2 500
PO1 13 0 26 1 700 71 4,2 200 212 12,6 600
PO2 12 0 24 159 5 3,1 14 18 11,2 50
PO3 13 2 24 13 200 353 2,8 1 000 989 7,5 2 800
PO4 13 4 22 4 870 78 1,6 220 166 3,4 470
PO5 13 0 26 5 600 141 2,3 400 530 9,5 1 500
B 22 6 38 16 0,4 2,4 1 3,2 19,8 9
WS 22 4 40 174 2,5 1,4 7 14 8,2 41
MFH 22 4 40 65 2,1 3,1 6 11 17,1 32
MP 22 8 36 1 0,4 26,6 1 0,7 52,0 2
PF 22 2 42 417 8,1 2,0 23 66 15,8 187
MFL 22 4 40 361 3,5 1,0 10 35 9,8 100
a, bSee Table A.1, except that wisthemean manganese content.ISO 6869:2000(E)
© ISO2000 –All rights reserved 13TableA.6 —Statistical resultsforpotassium
Parameterb
w srCVr r sRCVR R Samplean1 n2 n3
mg/kg mg/kg % m/kg mg/kg % mg/kg
P1 11 0 22 700 71 8,3 200 212 33,9 600
P2 11 0 22 570 120 21,4 340 212 37,5 600
P3 11 0 22 1 000 71 7,7 200 247 25,0 700
PO1 11 2 20 3 700 141 3,7 400 459 12,8 1 300
PO2 11 0 22 10 000 247 2,4 700 989 9,9 2 800
PO3 11 0 22 2 400 71 3,4 200 247 9,9 700
PO4 11 2 20 14 900 495 3,3 1 400 777 5,2 2 200
PO5 11 0 22 3 900 141 3,7 400 318 8,1 900
B 17 2 32 4 850 118 2,4 334 746 15,4 2 110
WS 17 4 30 30 100 551 1,8 1 560 2 237 7,4 6 330
MFH 17 2 32 6 330 160 2,5 454 898 14,2 2 540
MP 17 2 32 17 100 583 3,4 1 650 1 336 7,8 3 780
PF 17 2 32 11 200 505 4,5 1 430 936 8,3 2 650
MFL 17 6 28 17 800 746 4,2 2 110 1 155 6,5 3 270
a, bSee Table A.1, except that wisthemean potassiumcontent.
TableA.7 —Statisticalresultsfor sodium
Parameterb
w srCVr r sRCVR R Samplean1 n2 n3
mg/kg mg/kg % mg/kg mg/kg % mg/kg
P1 11 0 22 237 000 636 2,7 1 800 12 721 5,4 36 000
P2 11 2 20 5 900 212 3,3 600 777 13,5 2 200
P3 11 0 22 155 000 3 536 2,3 10 000 9 187 5,9 26 000
PO1 11 0 22 33 900 1 025 3,0 2 900 2 155 6,4 6 100
PO2 11 0 22 1 840 78 4,3 220 212 11,5 600
PO3 11 2 20 680 120 17,6 340 120 17,9 340
PO4 11 0 22 660 110 16,7 310 141 21,3 400
PO5 11 0 22 580 134 23,0 380 155 26,8 440
B 15 8 22 117 10 8,7 29 20 17,3 57
WS 16 6 26 3 830 187 4,9 529 258 6,7 729
MFH 15 4 26 1 240 84 6,9 238 170 13,7 480
MP 16 6 26 4 210 142 3,4 402 246 5,8 696
PF 16 2 30 1 890 119 6,3 336 309 16,4 875
MFL 16 2 30 5 650 375 6,6 1 060 406 7,2 1 150
a, bSee Table A.1, except that wisthemean sodiumcontent.ISO 6869:2000(E)
14 © ISO2000 –All rights reservedTableA.8 —Statistical resultsforzinc
Parameterb
w srCVr r sRCVR R Samplean1 n2 n3
mg/kg mg/kg % mg/kg mg/kg % mg/kg
P1 13 2 24 5 200 177 3,1 500 353 7,1 1 000
P2 13 2 24 8 700 141 1,7 400 671 7,8 1 900
P3 13 4 22 14 600 318 2,3 900 459 3,2 1 300
PO1 13 0 26 3 500 141 4,0 400 353 10,4 1 000
PO2 13 0 26 260 21 7,6 60 39 15,0 110
PO3 13 0 26 10 900 318 2,9 900 1 237 11,4 3 500
PO4 13 2 24 10 000 247 2,4 700 671 6,6 1 900
PO5 13 2 24 11 900 283 2,3 800 565 4,9 1 600
B 22 8 36 29 1,1 3,4 3 2,8 9,4 8
WS 22 12 32 44 1,1 2,1 3 1,8 4,3 5
MFH 22 6 38 47 3,2 6,5 9 3,9 8,3 11
MP 22 8 36 46 2,1 4,5 6 3,2 7,0 9
PF 22 8 36 569 11 2,0 32 33 5,8 94
MFL 22 6 38 106 3,5 3,4 10 7,1 6,7 20
a, bSee Table A.1, except that wisthemean zinccontent.ISO 6869:2000(E)
© ISO2000 –All rights reserved 15Bibliography
[1] ISO 78-4:1983, Layouts for standards —Part 4: Standard for atomic absorptionspectrometric analysis.
[2] ISO 5725:1986, Precision of test methods —Determination of repeatability and reproducibility for a
standard testmethodby inter-laboratory tests1).
[3] ISO 5725-1:1994, Accuracy (trueness and precision) of measurement methods and results —Part1:
General principles and definitions.
[4] ISO 5725-2:1994, Accuracy (trueness and precision) of measurement methods and results —Part2: Basic
methodfor the determination of repeatability andreproducibility of a standardmeasurement method .
[5] ISO 6497, Animalfeedingstuffs —Sampling .
[6] ISO 6956, Atomic absorptionspectrometry —Introduction for use .
[7] Ruig,W.G. de, J.Assoc.Off. Anal. Chem .,69,1986, pp. 1009-1013.
1)Nowwithdrawn.ISO 6869:2000(E)
ICS 65.120
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© ISO2000 –All rights reserved