1、BRITISH STANDARD BS 4401-10: 1997 ISO 13730: 1996 Methods of test for Meat and meat products Part 10: Determination of total phosphorus content: spectrometric method ICS 67.120.10BS4401-10:1997 This British Standard, having been prepared under the directionof the Consumer Products and Services Secto
2、r Board, was published under theauthority of the Standards Board and comes into effect on 15 April 1997 BSI 12-1999 ISBN 0 580 27241 9 National foreword This British Standard reproduces verbatim ISO13730:1996 and implements it as the UK national standard. It supersedes BS4401-10:1975 which is withdr
3、awn. The UK participation in its preparation was entrusted to Technical Committee AW/6, Chemical analysis of meat and meat products, which has the responsibility to: aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation,
4、 or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. A list of organizations represented on this committee can be obtained on request. Cross-references The British Standards which implement international
5、or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the
6、necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, t
7、heISO title page, pages ii to iv, pages 1 to 4 and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Amendments issued since publication Amd. No. Date CommentsBS4401-10:
8、1997 BSI 12-1999 i Contents Page National foreword Inside front cover Foreword iii Text of ISO 13730 1ii blankISO 13730:1996 ii BSI 12-1999 Contents Page Foreword iii 1 Scope 1 2 Normative reference 1 3 Definition 1 4 Principle 1 5 Reagents 1 6 Apparatus 2 7 Sampling 2 8 Preparation of test sample 2
9、 9 Procedure 2 10 Calculation 3 11 Precision 3 12 Test report 3 Annex A (informative) Bibliography 4 Descriptors: Agricultural products, animal products, food products, meat, poultry meat, meat products, chemical analysis, determination of content, phosphorus, spectrophotometric analysis, spectromet
10、ric method.ISO 13730:1996 BSI 12-1999 iii Foreword 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
11、body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electr
12、otechnical Commission (IEC) on all matters of electrotechnical standardization. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least75% of the member bodies casting a v
13、ote. International Standard ISO13730 was prepared by Technical Committee ISO/TC34, Agricultural food products, Subcommittee SC6, Meat and meat products. Annex A of this International Standard is for information only.iv blankISO 13730:1996 BSI 12-1999 1 1 Scope This International Standard specifies a
14、 method for the determination of the total phosphorus content of all kinds of meat and meat products, including poultry. The precision results quoted in this method relate only to processed sausages. 2 Normative reference The following standard contains provisions which, through reference in this te
15、xt, constitute provisions of this International Standard. At the time of publication, the edition indicated was valid. All standards are subject to revision, and parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editi
16、on of the standard indicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 936:, Meat and meat products Determination of ash 1) . 3 Definition For the purposes of this International Standard, the following definition applies. 3.1 total phosphorus co
17、ntent of meat and meat products mass of phosphorus pentoxide determined by the procedure specified in this International Standard, expressed as a percentage of the mass of the test portion 4 Principle Drying of the test portion and incineration of the residue. After cooling, hydrolysis of the ash wi
18、th nitric acid. Filtration and dilution followed by the formation of a yellow compound with a mixture of ammonium monovanadate and ammonium heptamolybdate. Photometric measurement at a wavelength of430nm. 5 Reagents Use only reagents of recognized analytical grade and distilled or demineralized wate
19、r or water of at least equivalent purity. 5.1 Nitric acid, 1 + 2 (V/V) dilution. Mix 1 volume of nitric acid 65% (m/m); 20= 1,40g/ml with two volumes of water. 5.2 Ammonium monovanadate solution (NH 4 VCO 3 ),2,5g/l. Dissolve 2,5g of ammonium monovanadate in500ml of boiling water. Cool and transfer
20、quantitatively to a1000ml volumetric flask (6.7). Add20ml of the nitric acid (5.1), dilute to the mark with water and mix. 5.3 Ammonium heptamolybdate solution, (NH 4 ) 6 Mo 7 O 24 4H 2 O, 50g/l. Dissolve 50g of ammonium heptamolybdate tetrahydrate in about800ml of warm water (at approx.50 C). Cool
21、and transfer quantitatively to a1000ml volumetric flask. Dilute to the mark with water and mix. 5.4 Colour reagent Mix one volume of the nitric acid (5.1) with one volume of the ammonium monovanadate solution(5.2). Subsequently add one volume of the ammonium heptamolybdate solution (5.3) and mix. Th
22、e colour reagent should turn from pale yellow to completely clear. 5.5 Phosphate stock solution, c(P) = 218mg/l; c(P 2 O 5 )= 500mg/l. Dissolve in water958,8mg of potassium dihydrogen phosphate (KH 2 PO 4 ), previously dried for3h at103 C 2 C and allowed to cool in a desiccator. Transfer quantitativ
23、ely to a1000ml volumetric flask (6.7). Dilute to the mark with water and mix. 5.6 Phosphate standard solutions, containing between0,05mg and0,30mg of P 2 O 5per millilitre. Transfer by pipette or burette to100ml volumetric flasks (6.7)10ml, 20ml, 30ml, 40ml, 50ml and60ml of the phosphate stock solut
24、ion (5.5). Add10ml of the nitric acid (5.1). Dilute to the mark with water and mix. 5.7 Blank solution Pipette 2ml of the nitric acid (5.1) and30ml of the colour reagent (5.4) into a100ml volumetric flask(6.7). Dilute to the mark with water and mix. 1) To be published. (Revision of ISO 936:1978)ISO
25、13730:1996 2 BSI 12-1999 6 Apparatus IMPORTANT: All glassware shall be thoroughly cleaned using a phosphate-free detergent and then rinsed with water. Usual laboratory equipment and, in particular, the following. 6.1 Mechanical or electrical equipment capable of homogenizing the laboratory sample. T
26、his includes a high speed rotational cutter, or a mincer fitted with a plate with holes not exceeding4,5mm in diameter (see also clause8). 6.2 Water bath, capable of being maintained at100 C. 6.3 Fluted filter paper, of diameter15cm, phosphate-free. 6.4 Spectrometer, capable of being used at a wavel
27、ength of430nm2nm, or a photo-electric colorimeter with an interference filter with absorption maximum at430nm 2nm. 6.5 Glass cells, of10mm optical path length. 6.6 Analytical balance, capable of weighing to an accuracy of 0,001g. 6.7 One-mark volumetric flasks, of capacities100ml and1000ml. 6.8 Muff
28、le furnace For details of this and other apparatus needed for the incineration procedure, see ISO936. 7 Sampling It is important that the laboratory receive a sample which is truly representative and has not been damaged or changed during transport or storage. Sampling is not part of the method spec
29、ified in this International Standard. A recommended sampling method is given in ISO3100-1. Proceed from a representative sample of at least200g. Store the sample in such a way that deterioration and change in composition are prevented. 8 Preparation of test sample Homogenize the laboratory sample wi
30、th the appropriate equipment (6.1). Take care that the temperature of the sample material does not rise above25 C. If a mincer is used, pass the sample at least twice through the equipment. Fill a suitable airtight container with the prepared test sample, close the container and store in such a way
31、that deterioration and change in composition are prevented. Analyse the test sample as soon as practicable, but always within24h after homogenization. 9 Procedure NOTEIf it is required to check whether the repeatability requirement (11.1) is met, carry out two single determinations in accordance wit
32、h9.1 to 9.3. 9.1 Test portion Weigh, to the nearest0,001g, about5g of the prepared test sample. 9.2 Determination 9.2.1 Carry out the mineralization of the test portion (9.1) by using an incinerator (6.8) and the method described in ISO936. 9.2.2 Take up the resulting ash in10ml of the nitric acid (
33、5.1) using a stirring rod to aid dissolution. 9.2.3 Cover the dish with a watch glass and heat for30min on a boiling water bath (6.2). Allow to cool and transfer the liquid quantitatively to a100ml volumetric flask (6.7). Dilute to the mark with water, mix and filter through the filter paper(6.3), r
34、ejecting the first5ml to10ml of filtrate. 9.2.4 Pipette20ml of the clear and colourless filtrate into a100ml volumetric flask (6.7) and add30ml of the colour reagent (5.4) by pipette or burette. Dilute to the mark with water and mix. Allow to stand for at least15min. 9.2.5 Measure the absorbance at
35、a wavelength of430nm 2nm in a glass cell (6.5) against the blank solution (5.7), using the spectrometer or the photo-electric colorimeter equipped with an interference filter (6.4). 9.2.6 Read the phosphorus concentration of the sample solution from the calibration graph obtained as described in9.3.
36、 9.3 Calibration graph 9.3.1 Pipette20ml of each phosphate standard solution (5.6) into100ml volumetric flasks (6.7). Add to these solutions30ml of the colour reagent(5.4). Dilute to the mark withwaterto obtain concentrations of104g, 204g, 304g, 404g, 504g and 604g of P 2 O 5per millilitre, respecti
37、vely. Mix and allow to stand for at least15min. 9.3.2 Carry out the procedure described in9.2.5. 9.3.3 Plot the measured absorbance values, corrected for the blank value, against the concentrations of the diluted phosphate standard solutions (9.3.1). Construct the best-fitting straight line through
38、the plotted points and the origin. It is necessary to prepare a new calibration graph for each series of analyses.ISO 13730:1996 BSI 12-1999 3 10 Calculation Calculate the total phosphorus content, expressed as phosphorus pentoxide as a percentage by mass of the test portion, by the formula: where R
39、eport the result rounded to three decimal places. 11 Precision The precision of the method has been established by an interlaboratory test (see refs. 3,4), only with processed sausages, carried out in accordance with ISO5725 (ref. 2). 11.1 Repeatability The absolute difference between two independen
40、t single test results, obtained using the same method on identical test material in the same laboratory by the same operator using the same equipment within a short interval of time, should not be greater than0,0070% (m/m). 11.2 Reproducibility The absolute difference between two single test results
41、, obtained using the same method on identical test material in different laboratories with different operators using different equipment, should not be greater than0,0117% (m/m). 12 Test report The test report shall specify: the method in accordance with which sampling was carried out, if known; the
42、 method used; the test result obtained; and if the repeatability has been checked, the final quoted result obtained. It shall also mention all operating details not specified in this International Standard, or regarded as optional, together with details of any incidents which may have influenced the
43、 test result. The test report shall include all information necessary for the complete identification of the sample. c is the phosphorus pentoxide concentration, in micrograms per millilitre, of the sample solution (9.2.4) as read from the calibration graph; m is the mass, in grams, of the test port
44、ion (9.1). c 20m -ISO 13730:1996 4 BSI 12-1999 Annex A (informative) Bibliography 1 ISO 3100-1:1991, Meat and meat products Sampling and preparation of test samples Part 1: Sampling. 2 ISO 5725:1986, Precision of test methods Determination of repeatability and reproducibility for a standard test met
45、hod by inter-laboratory tests. 3 Bundesverband der Deutschen Feinkostindustrie eV. Untersuchungsmethoden fr die Feinkostindustrie. Bonn, Germany, 1978. 4 Bestimmung des Gesamtphosphorgehaltes in Fleisch und Fleischerzeugnissen. Amtliche Sammlung von Untersuchungsverfahren nach 35LMGB, Method 06.00 9
46、, Beuth Verlag, Berlin, December 1992.blankBS 4401-10: 1997 ISO 13730: 1996 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution BSI is the independent national body responsible for preparing BritishStandards. It presents the UK view on standards in Europe and at the international
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