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GB 5009.87-2016 PDF English

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GB 5009.87-2016: National food safety standard - Determination of Phosphorus in Foods
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GB 5009.87: Evolution and historical versions

Standard IDContents [version]USDSTEP2[PDF] deliveryName of Chinese StandardStatus
GB 5009.87-2016English70 Add to Cart 0-9 seconds. Auto-delivery National food safety standard - Determination of Phosphorus in Foods Valid
GB/T 5009.87-2003English239 Add to Cart 3 days Determination of phosphorus in foods Obsolete

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GB 5009.87-2016: National food safety standard - Determination of Phosphorus in Foods

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GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA National Food Safety Standard - Determination of Phosphorus in Foods Issued on. DECEMBER 23, 2016 Implemented on. JUNE 23, 2017 Issued by. National Health and Family Planning Commission of the PRC; China Food and Drug Administration.

Table of Contents

Foreword... 3 1 Scope... 4 2 Principles... 4 3 Reagents and materials... 4 4 Instruments and equipment... 6 5 Analytical procedures... 6 6 Analysis results expression... 8 7 Precision... 9 8 Others... 9 9 Principles... 9 10 Reagents and materials... 10 11 Instruments and equipment... 11 12 Analytical procedures... 11 13 Analysis results expression... 12 14 Precision... 12 15 Others... 12

Foreword

This Standard replaces the method for determination of phosphorus in GB/T 5009.87-2003 “Determination of phosphorus in foods”, GB 5413.22-2010 “National food safety standard - Determination of phosphorus in foods for infants and young children, milk and milk products”, GB/T 22427.11-2008 “Starches and derived products - Determination of total phosphorus content”, GB/T 9695.4-2009 “Meat and meat products -Determination of total phosphorus”, GB/T 18932.11-2002 “Method for the determination of potassium, phosphorus, iron, calcium, zinc, aluminium, sodium, magnesium, boron, manganese, copper, barium, titanium, vanadium, nickel, cobalt, chromium contents in honey - Inductively coupled plasma atomic emission spectrum”, GB/T 23375-2009 “Determination of copper, iron, zinc, calcium, magnesium and phosphorus content in vegetables and derived products”, NY/T 1018-2006 “Determination of phosphorus content in vegetables and derived products”, NY/T 1738-2009 “Determination of phosphorus content in crops and derived products - Spectrophotometry”, SN/T 0446-1995 “Method for the determination of phosphorus in milk product for export”, and SN/T 0801.2-2011 “Animal and vegetable oil and fats for import and export - Part 2.Determination of phosphorous”. As compared with GB/T 5009.87-2003, the main changes of this Standard are as follows. - The standard’s name is changed to “National Food Safety Standard - Determination of Phosphorus in Foods”; - DELETE weight method. National Food Safety Standard - Determination of Phosphorus in Foods

1 Scope

This Standard specifies spectrophotometry and inductively coupled plasma emission spectrum for the determination of phosphorus in foods. Methods 1 and 3 of this Standard are applicable to the determination of phosphorus in various foods. Method 2 is applicable to the determination of phosphorus in foods for infants and young children, milk and milk products. Method 1 -- Molybdenum blue spectrophotometry

2 Principles

After the sample is digested, phosphorus, under acidic conditions, is combined with ammonium molybdate to form ammonium phosphomolybdate. This compound is reduced to blue compound molybdenum blue by hydroquinone, sodium sulfite, or stannous chloride, hydrazine sulfate. The absorbance value of key blue at 660 nm is directly proportional to the concentration of phosphorus. USE a spectrophotometer to determine the absorbance value of the sample solution; and COMPARE it with standard series to quantify.

3 Reagents and materials

Unless otherwise stated, the reagents used in this method are analytically pure. The water is the Grade III water specified in GB/T 6682. 3.1 Reagents 3.1.1 Sulfuric acid (H2SO4). guaranteed reagent. 3.1.2 Perchloric acid (HClO4). guaranteed reagent. 3.1.7 Ammonium molybdate [(NH4)6Mo7O24 · 4H2O]. 3.1.8 Stannous chloride (SnCl2 · 2H2O). 3.1.9 Hydrazine sulfate (NH2NH2 · H2SO4). 3.2 Preparation of reagents 3.2.1 Sulfuric acid solution (15%). MEASURE 15 mL of sulfuric acid; ADD slowly to 80 mL of water; after cooling, USE water to dilute to 100 mL; and MIX it well. 3.2.6 Hydroquinone solution (5 g/L). WEIGH 0.5 g of hydroquinone in 100 mL of water to dissolve it; ADD a drop of sulfuric acid; and MIX well. 3.3 Standard Potassium dihydrogen phosphate (KH2PO4, CAS No.7778-77-0). Purity >99.99%. Or a phosphorus standard solution of certain concentration which has been certified by the state and awarded a reference material certificate. 3.4 Preparation of standard solutions

4 Instruments and equipment

4.1 Spectrophotometer. 4.4 Analytical balance. The sensitivity is 0.1 mg and 1 mg.

5 Analytical procedures

5.1 Preparation of samples During sampling and sample preparation, contamination shall be avoided. 5.1.1 Grain, beans After removing the dopants, the samples are crushed and stored in plastic bottles. 5.2 Pretreatment for samples 5.2.1 Wet digestion WEIGH 0.2 g~3 g (accurate to 0.001 g) of the sample or accurately PIPETTE 0.500 mL~5.00 mL of the liquid sample in a graduated digestive tube; ADD 10 mL of nitric acid, 1 mL of perchloric acid, 2 mL of sulfuric acid; to DIGEST it on the adjustable electric heating furnace (reference conditions. 5.2.2 Dry ashing WEIGH 0.5 g~5 g (accurate to 0.001 g) of the sample or accurately PIPETTE 0.500 mL~10.0 mL of the liquid sample; BURN it on the fire to charcoal; and then at 550 °C, FORM ash, until the ash is white (If necessary, ashing may be performed after wetting with concentrated nitric acid and drying); ADD 10 mL of hydrochloric acid solution (1+1); and EVAPORATE on a water bath. 5.3 Determination Note. Optional hydroquinone, sodium sulfite reduction method or stannous chloride, hydrazine sulfate reduction method. 5.3.1 Hydroquinone, sodium sulfite reduction method 5.3.2 Stannous chloride, hydrazine sulfate reduction method 5.3.2.1 Making of standard curve Accurately PIPETTE 0 mL, 0.500 mL, 1.00 mL, 2.00 mL, 3.00 mL, 4.00 mL, and 5.00 mL of phosphorus standard use solution, equivalent to 0 μg, 5.00 μg, 10.0 μg, 20.0 μg, 30.0 μg, 40.0 μg, and 50.0 μg of phosphorus content; PLACE them in 25 mL test tubes with stoppers separately;

6 Analysis results expression

The phosphorus content in the sample shall be calculated according to the equation (1).

7 Precision

The absolute difference between the two independent determination results, obtained under repeated conditions, shall not exceed 5% of the arithmetic mean.

8 Others

When the sample volume is 0.5 g (or 0.5 mL) and is diluted to 100 mL, the limit of detection is 20 mg/100 g (or 20 mg/100 mL);

9 Principles

After the sample is digested, phosphorus, under acidic conditions, forms yellow complex vanadium molybdenum yellow with ammonium vanadium molybdate.

10 Reagents and materials

Unless otherwise stated, the reagents used in this method are analytically pure. The water is the Grade III water specified in GB/T 6682. 10.1 Reagents 10.1.6 Sodium hydroxide (NaOH). 10.1.7 2,6-dinitrophenol or 2,4-dinitrophenol [C6H3OH(NO2)2]. 10.2 Preparation of reagents 10.2.1 Ammonium vanadium molybdate reagent. Solution A. WEIGH 25 g of ammonium molybdate, and DISSOLVE it in 400 mL of water. 10.2.4 Nitric acid solution (0.2 mol/L). PIPETTE 12.5 mL of nitric acid; USE water to dilute to 1000 mL and MIX well. 10.2.5 Dinitrophenol indicator (2 g/L). WEIGH 0.2 g of 2,6-dinitrophenol or 2,4- dinitrophenol to dissolve in 100 mL of water and MIX well. 10.3 Standard Potassium dihydrogen phosphate (KH2PO4, CAS No.7778-77-0). Purity >99.99%. Or a phosphorus standard solution of certain concentration which has been certified by the state and awarded a reference material certificate. ......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.


      

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