इंटरनेट मानक 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. “जान1 का अ+धकार, जी1 का अ+धकार” “प0रा1 को छोड न’ 5 तरफ” Mazdoor Kisan Shakti Sangathan Jawaharlal Nehru “The Right to Information, The Right to Live” “Step Out From the Old to the New” IS 5960-16 (2004): Meat and Meat Products - Methods of Test, Part 16: Determination of Total Phosphorus Content - Spectrometric Method [FAD 18: Slaughter House and Meat Industry] “!ा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 5960 (Part 16): 2004 ISO 13730:1996 Vlm%7Wm +wih+i%mTiv—— WMJl W-fa WPT16 qyFWWiktiW5W5?=t T— #@idt&5~ Indian Standard I’vIEATAND MEAT PRODUCTS — METHODS OF TEST PART 16 DETERMINATION OF TOTAL PHOSPHORUS CONTENT — SPECTROMETRIC METHOD Ics 07,100.30 0 BIS 2004 BUREAU OF INDIAN STANDARDS MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG NEW DELHI 110002 JL{}7e 2004 Price Group 3 Slaughter House and Meat Industry Sectional Committee, FAD 56 NATIONAL FOREWORD This Indian Standard (Part 16) which is identical with 1S0 13730 : 1996 ‘Meqt and meat products — Determination oftotal phosphorus content — Spectrometric method’ issued by the International Organization for Standardization (1S0) was adopted by the Bureau of Indian Standards on the recommendations of Slaughter House and Meat Industry Sectional Committee and approval of the Food and Agriculture Division Council. In the adopted standard, certain terminology and conventions are, however, not identical to those used in Indian Standards. Attention isdrawn especially 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 apoint (.) asthe decimal marker. ,-+-+ ,! CROSS REFERENCES In the adopted standard, normative reference appears to the following International Standard, for which Indian Standard also exists. The corresponding Indian Standard which isto be substituted in its place is given below along with its degree of equivalence for the edition indicated: International Standard Corresponding Indian Standard Degree of Equivalence 1S0 936: 1998Meat and meat products — IS 5960 (Part 2) : 2000 Meat and meat Identical Determination of total ash products — Methods of test: Part 2 Determination oftotal ash In reporting the results of atest or analysis made in accordance with this standard, ifthe final value, observed or calculated, is to be rounded off, it shall be done in accordance with IS 2: 1960 ‘Rules for rounding off numerical values (revised)’. IS 5960 (Part 16) :2004 ISO 13730:1996 Indian Standard MEAT AND MEAT PRODUCTS — METHODS OF TEST PART 16 DETERMINATION OF TOTAL PHOSPHORUS CONTENT — SPECTROMETRIC METHOD 1 Scope This International Standard specifies a 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 text, 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 edition of the standard indicated below. Members of IEC and 1S0 maintain registers of currently valid Internatio nal Standards. 1S0 936:—1),Meat and meat products — Determination of ash. 3 Definition Forthe purposes ofthis International Standard, the following definition applies. 3.1 total phosphorus content of meat and meat products: Mass of phosphorus pentoxide determined bythe procedure specified inthis international Standard, expressed asapercentage of the mass of the test portion. 4 Principle Drying of the test portion and incineration of the residue. Afler cooling, hydrolysis of the ash with nitric acid. Filtration and dilution followed by the formation of a yellow compound with a mixture of ammonium monovanadate and ammonium heptamolybdate. Photometric measurement atawavelength of 430 nm. I) To be published. (Revision of ISO 936: 1978) 1 IS 5960 (Part 16) :2004 ISO 13730:1996 5 Reagents Use only reagents of recognized analytical grade and distilled or demineralized water or water of at least equivalent purity. 5.1 Nitric acid, 1+2 (HP’) dilution. Mix 1volume of nitric acid [65‘X. (rdrn); p20 = 1,40 g/ml] with two volumes ofwater. 5.2 Ammonium monovanadate solution (NH~VCOJ, 2,5 g/1. Dissolve 2,5 g of ammonium monovanadate in 500 ml of boiling water. Cool and transfer quantitatively to a 1000mlvolumetric flask (6.7). Add 20ml ofthe nitric acid (5.1), dilute tothe mark with water and mix. 5.3 Ammonium heptamolybdate soiution, [(NH&h’fo@NoAH@], 50 g/1. Dissolve 50 gof ammonium heptamolybdate tetrahydrate in about 800ml of warm water (at approx. 50 ‘C). Cool and transfer quantitatively to a 1000ml volumetric flask. Dilute tothe mark with water and mix. 5.4 Colour reagent. Mix one volume of the nitric acid (5.1)with one volume ofthe ammonium monovanadate solution (5.2). Subsequently add one volume ofthe ammonium heptamolybdate solution (5.3) and mix. The colour reagent should turn from pale yellow to completely clear. 5.5 Phosphate stock solution, c(P) =218 mg/l; c(P*OJ = 500 mg/1. Dissolve in water 958,8 mg of potassium dihydrogen phosphate (KH2POJ, previously dried for 3h at 103‘C * 2“Cand allowed to cool inadesiccator. Transfer quantitatively to a 1000mlvolumetric flask (6.7). Dilute to the mark with water and mix. 5.6 Phosphate standard solutions, containing between 0,05 mg and 0,30 mgof P205per millilitre. Transfer by pipette or burette to 100ml volumetric flasks (6.7) 10ml, 20 ml, 30 ml, 40 ml, 50ml and 60 ml of the phosphate stock solution (5.5). Add 10mlofthe nitric acid (5.1). Dilute to the mark with water and mix. 5.7 BIank solution. Pipette 2ml of the nitric acid (5.1) and 30ml of the colour reagent (5.4) into a 100ml volumetric flask (6.7). Dilute to the mark with water and mix. 6 Apparatus IMPORTANT: All glassware shall be thoroughly cleaned using a phosphate-free detergent and then rinsed with water. Usual laboratory equipment and, inparticular, the following. 6.1 Mechanical or electrical equipment capable of homogenizing the laboratory sample. This includes a high speed rotational cutter, or a mincer fitted with a plate with holes not exceeding 4,5 mm in diameter (see also clause 8). 6.2 Water bath, capable of being maintained at 100‘C. 6.3 Fluted filter paper, of diameter 15cm, phosphate-free. 2 IS 5960 (Part 16) :2004 ISO 13730:1996 6.4 Spectrometer, capable of being used at a wavelength of 430 nm* 2nm, or a photo-electric calorimeter with an interference filter with absorption maximum at 430 nm+ 2nm. 6.5 Glass cells, of 10mmoptical path length. 6.6 Analytical balance, capable of weighing to an accuracy of * 0,001 g. 6.7 One-mark volumetric flasks, of capacities 100ml and 1000ml. 6.8 Muffle furnace Fordetails of this and other apparatus needed for the incineration procedure, see ISO 936. 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 specified in this International Standard. A recommended sampling method is given inISO3100-1. Proceed from arepresentative sample of at least 200 g. Storethe sample insuch away that deterioration and change incomposition are prevented. 8 Preparation of test sample Homogenize the laboratory sample with the appropriate equipment (6.1). Take care that the temperature of the sample material does not rise above 25 ‘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 that deterioration and change incomposit i on are prevented. Analyse the test sample as soon as practicable, but always within24 hafter homogenization. 9 Procedure NOTE —If it is required to check whether the repeatability requirement (11.1) is met, carry out two single determinations inaccordance with 9.1 to 9.3. 9.1 Test portion Weigh,tothe nearest 0,001 g,about 5gofthe 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 in1S0 936. 9.2.2 Take upthe resulting ash in 10ml ofthe nitric acid (5.1)using astirring rod to aid dissolution. 9.2.3 Cover the dish with awatch glass and heat for 30min on aboiling water bath (6.2). Allow to cool and transfer the liquid quantitatively to a 100ml volumetric flask (6.7). Dilute to the mark with water, mix and filter through the filter paper (6.3), rejecting the first 5mlto 10mlof filtrate. 3 IS 5960 (Part 16) :2004 ISO 13730:1996 9.2.4 Pipette 20 ml of the clear and colorless filtrate into a 100ml volumetric flask (6.7) and add 30 ml of the colour reagent (5.4) by pipette or burette. Dilute to the mark with water and mix. Allow to stand for at least 15min. 9.2.5 Measure the absorbance at a wavelength of 430 nm * 2 nm in a glass cell (6.5) against the blank ‘ solution (5.7), using the spectrometer or the photo-electric calorimeter 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. 9.3 Calibration graph 9.3.1 Pipette 20 ml of each phosphate standard solution (5.6) into 100mlvolumetric flasks (6.7). Add to these solutions 30 ml of the colour reagent (5.4). Dilute to the mark with water to obtain concentrations of 10pg, 20 ~g, 30 ~g, 40 pg, 50Ugand 60 ~g of Pz05per millilitre, respectively. Mix and allow to stand for at least 15min. 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 the plotted points and the origin. It isnecessary to prepare anew calibration graph for each series of analyses. 10 Calculation Calculate the total phosphorus content, expressed as phosphorus pentoxide as a percentage by mass of the test portion, bythe formula: c 20m where c isthe phosphorus pentoxide concentration, inmicrograms per millilitre, of the sample solution (9.2.4) asread from the calibration graph; m isthe mass, ingrams, ofthe test portion (9.1). Report 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 inaccordance with 1S0 5725 (ref. [2]). 11.1 Repeatability The absolute difference between two independent single test results, obtained using the same method on identical test material inthe same laboratory by the same operator using the same equipment within a short interval of time, should not be greater than 0,0070 ‘A(m/m). 4 IS 5960 (Part 16) :2004 ISO 13730:1996 11.2 Reproducibility The absolute difference between two single test results, obtained using the same method on identical test material in different laboratories with different operators using different equipment should not be greater than 0,0117% (mlm). 12 Test report Thetest report shall specifju themethod inaccordance with which sampling was carried out, ifknown; themethod used; thetest result obtained; and ifthe 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 test result. .- The test report shall include all information necessa~ forthe complete identification of the sample. 5