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GB 5009.16-2023 PDF English

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GB 5009.16-2023: National food safety standard - Determination of tin in foods
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GB 5009.16: Evolution and historical versions

Standard IDContents [version]USDSTEP2[PDF] deliveryName of Chinese StandardStatus
GB 5009.16-2023English215 Add to Cart 0-9 seconds. Auto-delivery National food safety standard - Determination of tin in foods Valid
GB 5009.16-2014English145 Add to Cart 0-9 seconds. Auto-delivery National Food Safety Standard -- Determination of Tin in food Obsolete
GB/T 5009.16-2003English279 Add to Cart 3 days Determination of tin in foods Obsolete
GB/T 5009.16-1996English199 Add to Cart 2 days Method for determination of tin in foods Obsolete
GB 5009.16-1985English199 Add to Cart 2 days Method for determination of tin in foods Obsolete

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GB 5009.16-2023: National food safety standard - Determination of tin in foods

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GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA National food safety standard - Determination of tin in foods Issued on. SEPTEMBER 06, 2023 Implemented on. MARCH 06, 2024 Issued by. National Health Commission of the People’s Republic of China; State Administration for Market Regulation.

Table of Contents

Foreword... 3 1 Scope... 4 2 Principle... 4 3 Reagents and materials... 4 4 Instruments and apparatuses... 6 5 Analysis steps... 6 6 Expression of analysis results... 8 7 Precision... 8 8 Others... 9 9 Principle... 9 10 Reagents and materials... 9 11 Instruments and apparatuses... 10 12 Analysis steps... 11 13 Expression of analysis results... 12 14 Precision... 12 15 Others... 13 16 Principle... 13 17 Reagents and materials... 13 18 Instruments and apparatuses... 14 19 Analysis steps... 14 20 Expression of analysis results... 15 21 Precision... 16 22 Others... 16 Appendix A Microwave digestion heating program... 17

Foreword

This Standard replaces GB 5009.16-2014 National Food Safety Standard - Determination of Tin in food. Compared with GB 5009.16-2014, the major changes of this Standard are as follows. -- Add inductively coupled plasma mass spectrometry as method II; -- Add inductively coupled plasma-atomic emission spectrometry as method III; -- Remove phenofluorenone colorimetry; -- Modify the scope of application of method I – hydride atomic fluorescence spectrometry, by adding the method detection limit. National food safety standard - Determination of tin in foods

1 Scope

This Standard specifies the methods for the determination of tin in foods by hydride atomic fluorescence spectrometry, inductively coupled plasma mass spectrometry and inductively coupled plasma-atomic emission spectrometry. This Standard applies to the determination of tin in foods. Method I – Hydride atomic fluorescence spectrometry

2 Principle

After the sample is digested, tin hydride (SnH4) is generated under the action of sodium borohydride (or potassium borohydride), and is brought into the atomizer by the carrier gas for atomization. Under the irradiation of a tin hollow cathode lamp, the ground state tin atoms are excited to an upper state.

3 Reagents and materials

Unless otherwise specified, all the reagents used in this method are analytical reagents, and the water used is grade-II water as specified by GB/T 6682. 3.1 Reagents 3.2 Preparation of reagents 3.2.1 Nitric acid-perchloric acid mixed solution (4+1). Measure 400 mL of nitric acid and 100 mL of perchloric acid, and mix well. 3.2.2 Sulfuric acid solution (1+9). Measure 100 mL of sulfuric acid, slowly add 900 mL of water, and mix well. 3.3 Standard Metal tin (Sn) standard product. purity ≥99.99%. Or tin standard solution of a certain concentration that is certified by the state and awarded a reference material certificate. 3.4 Preparation of standard solution 3.4.1 Tin standard solution (1.00 mg/mL). Accurately weigh 0.100 0 g of metal tin standard; place it in a small beaker; add 10.0 mL of sulfuric acid; cover with a watch glass; heat until the tin is completely dissolved; remove the watch glass; 3.4.2 Tin standard intermediate solution (10.0 mg/L). Accurately draw 1.00 mL of tin standard solution (1.00 mg/mL) into a 100 mL volumetric flask; use sulfuric acid solution (1+9) to dilute to the mark; mix well. Store at 0 °C ~ 5 °C, valid for 4 weeks. 3.4.3 Tin standard working solution (1.00 mg/L). Accurately draw 10.0 mL of tin standard intermediate solution (10.0 mg/L) into a 100 mL volumetric flask; use sulfuric acid solution (1+9) to dilute to the mark; mix well. Store at 0 °C ~ 5 °C, valid for 4 weeks.

4 Instruments and apparatuses

4.1 Atomic fluorescence spectrometer. equipped with tin hollow cathode lamp. 4.2 Adjustable temperature control electric hot plate. temperature control range 90 °C ~ 250 °C. 4.4 Electronic balance. the sensitivity is 0.1 mg and 1 mg. 4.5 Sample crushing equipment. homogenizer, high-speed crusher.

5 Analysis steps

5.1 Sample preparation 5.1.1 Solid samples 5.1.2 Liquid samples For samples such as soft drinks and liquid condiments, shake well. 5.1.3 Semi-solid sample Mix well. 5.2 Sample digestion 5.2.1 Weigh 1 g ~ 5 g (accurate to 0.001 g) of the sample or accurately transfer 1.00 mL ~ 5.00 mL of the liquid sample into a glass digestion vessel. 5.2.2 Accurately pipette 10.0 mL of blank solution and sample solution respectively; place them in a 25 mL volumetric flask; add 3.0 mL of sulfuric acid solution (1+9); add 2.0 mL of thiourea + ascorbic acid solution; then, use water to adjust the volume to 25 mL; mix well to obtain blank determination solution and sample determination solution. 5.3 Apparatus reference conditions Negative high voltage 380 V; lamp current 70 mA; atomization temperature 850 °C; shielding gas flow 1 200 mL/min; 5.4 Preparation of the standard curve After the instrument is preheated and stabilized, inject the standard series solution into the atomic fluorescence spectrometer; measure the fluorescence intensity of tin; draw a standard curve with the mass concentration of tin in the standard series solution as the abscissa and the fluorescence intensity as the ordinate. 5.5 Determination of sample solution Respectively inject the blank determination solution and the sample determination solution into the atomic fluorescence spectrometer;

6 Expression of analysis results

The content of tin in the sample is calculated according to Formula (1).

7 Precision

The absolute difference of 2 independent test results obtained under repeatability cannot exceed 10% of the arithmetic mean value.

8 Others

When the sampling volume is 1 g (or 1 mL), the constant volume of the sample solution is 50 mL, the detection limit of the method is 0.8 mg/kg (or 0.8 mg/L), and the quantitation limit of the method is 2.5 mg/kg (or 2.5 mg /L).

9 Principle

The sample is digested by nitric acid + hydrochloric acid, and the tin in it is dissolved and maintained stable under the action of hydrochloric acid. It is measured by an inductively coupled plasma mass spectrometer and qualitatively determined by the specific mass number (mass-to-charge ratio, m/z) of the tin element.

10 Reagents and materials

Unless otherwise stated, the reagents used in this method are guaranteed reagents, and the water is Grade-I water as specified in GB/T 6682. 10.1 Reagents 10.2 Preparation of reagents 10.3 Standard 10.3.1 Tin standard solution (1 000 mg/L). Use the tin reference solution certified by the state and awarded a reference material certificate. 10.4 Preparation of standard solution 10.4.1 Tin standard intermediate solution (10.0 mg/L). Accurately draw 1.00 mL of tin standard solution (1 000 mg/L) into a 100 mL volumetric flask; use hydrochloric acid solution (5+95) to dilute to the mark; mix well. Store at 0 °C ~ 5 °C, valid for 4 weeks. 10.4.2 Tin standard working solution (1.00 mg/L). Accurately draw 10.0 mL of tin standard intermediate solution (10.0 mg/L) into a 100 mL volumetric flask; use hydrochloric acid solution (5+95) to dilute to the mark; mix well. Store at 0 °C ~ 5 °C, valid for 4 weeks. 10.4.4 Internal standard working solution. Take an appropriate amount of internal standard element stock solution; use nitric acid-hydrochloric acid mixed solution (5+1+94) to dilute it step by step to prepare an internal standard working solution of appropriate concentration.

11 Instruments and apparatuses

11.1 Inductively coupled plasma mass spectrometer. 11.2 Analytical balance. the sensitivity is 1mg. 11.4 Microwave digestion system. equipped with polytetrafluoroethylene digestion inner tank. 11.5 Sample crushing equipment. homogenizer, high-speed crusher.

12 Analysis steps

12.1 Sample preparation Same as 5.1. 12.2 Sample digestion Weigh 0.2 g ~ 0.5 g (accurate to 0.001 g; the sampling amount can be appropriately increased to 1 g for samples containing more moisture) of the sample, or accurately transfer 0.500 mL ~ 3.00 mL of the liquid sample into the microwave digestion inner tank. For samples containing ethanol or carbon dioxide, heat at 90 °C for 30 minutes to remove ethanol or carbon dioxide. 12.3 Apparatus reference conditions Tin isotope 118 Sn, internal standard element 103 Rh or 185 Re; radio frequency power 1 550 W; plasma gas flow 15.0 L/min; carrier gas flow 1.00 L/min; auxiliary gas flow 0.90 L/min; sampling depth 10 mm; analysis mode the normal mode or collision/reaction cell mode; repeated for 2 ~ 3 times; flushing time 60 seconds. 12.5 Test of sample solution Inject the blank solution and sample solution into the inductively coupled plasma mass spectrometer respectively; measure the signal response values of tin element and internal standard element; obtain the mass concentration of tin element in the solution according to the standard curve.

13 Expression of analysis results

The content of tin in the sample is calculated according to Formula (2).

14 Precision

When the tin content in the sample is greater than 1 mg/kg (or 1 mg/L), the absolute difference between the two independent measurement results obtained under repeatability conditions shall not exceed 10% of the arithmetic mean;

15 Others

When the sampling volume is 0.5 g (or 0.5 mL) and the fixed volume is 50 mL, the detection limit of the method is 0.08 mg/kg (or 0.08 mg/L), and the quantitation limit is 0.25 mg/kg (or 0.25 mg/L). ......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.


      

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