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GB 31604.38-2016National food safety standard - Food contact materials and articles - Determination of arsenic and migration (English PDF)

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Issued by

National Health and Family Planning Commission of the PRC

Level / Type

National · Mandatory

Issue date

October 19, 2016

Implementation date

April 19, 2017

Scope

GB 31604.38-2016 (National food safety standard - Food contact materials and articles - Determination of arsenic and migration) is available as an English-translated PDF.

GB 31604.38-2016 — This standard specifies the hydride atomic fluorescence spectrometry, inductively coupled plasma mass spectrometry, and inductively coupled plasma emission spectroscopy for the determination of arsenic migration of the food contact materials and articles after soaked in the food simulants as well as the determination of arsenic in the paper articles and cork stoppers.

This standard applies to determination of the arsenic migration in the food contact materials and articles as well as the determination of arsenic in the paper articles and cork stoppers.

Part 1.Determination of arsenic Method 1.Hydride atomic fluorescence spectrometry

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Document preview — GB 31604.38-2016

National Standard of the People's Republic of China

Issued by: National Health and Family Planning Commission of the PRC

Contents

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

Foreword

This standard replaces the determination of arsenic and in the GB/T

5009.68-2003 "Method for analysis of hygienic standard of

perchlorovinyl-coating for inner wall of food container", GB/T 5009.72-2003

"Method for analysis of hygienic standard of aluminum-wares for food use",

GB/T 5009.78- 2003 "Method for analysis of hygienic standard of papers for

food packaging", GB/T 5009.81-2003 "Method for analysis of hygienic

standard of stainless steel food containers and table wares", SN/T 2900-2011

"Food contact materials for export - Paper, recycled fiber materials –

Determination of arsenic – Atomic fluorescence spectrometry", SN/T

2594-2010 "Food contact materials – Determination of lead, cadmium,

chromium, and arsenic in cork stoppers by inductively coupled plasma mass

spectrometry", SN/T 2597-2010 "Determination of lead, cadmium, chromium,

arsenic, antimony, germanium migration quantity in polymer for food contact

materials – Inductively coupled plasma atomic emission spectrometry method",

SN/T 2829-2011 "Food contact materials for export - Metallic materials -

Determination of migrant heavy metals in food simulant - Inductively coupled

plasma atomic emission spectrometric method".

As compared with GB/T 5009.68-2003, the main changes of this standard are

as follows.

- CHANGE the standard name into "National food safety standard - Food

contact materials and articles – Determination of arsenic and migration";

- ADD the arsenic determination;

- ADD the inductively coupled plasma mass spectrometry;

- ADD the inductively coupled plasma emission spectroscopy;

- DELETE the silver salt method and the arsenic spot method.

National food safety standard

Food contact materials and articles –

Determination of arsenic and migration

1 Scope

This standard specifies the hydride atomic fluorescence spectrometry,

inductively coupled plasma mass spectrometry, and inductively coupled

plasma emission spectroscopy for the determination of arsenic migration of the

food contact materials and articles after soaked in the food simulants as well

as the determination of arsenic in the paper articles and cork stoppers.

This standard applies to determination of the arsenic migration in the food

contact materials and articles as well as the determination of arsenic in the

paper articles and cork stoppers.

Part 1.Determination of arsenic

Method 1.Hydride atomic fluorescence spectrometry

2 Principles

Paper products and cork stoppers are crushed AND then subjected to dry ash

digestion, thiourea is added to the digestion solution to pre-reduce the

pentavalent arsenic to trivalent arsenic, which reacts with the reduction

hydrogen to produce the arsenic hydride; the arsenic hydride is carried by the

argon into the quartz atomizer AND decomposed into atomic arsenic, which

generates the atomic fluorescence under the excitation light of the arsenic

hollow cathode lamp. The fluorescence intensity is proportional to the arsenic

concentration in the measured solution, AND it is quantified through

comparison with the standard series.

3 Reagents and materials

Unless otherwise specified, the reagents used in this method are of analytical

pure AND the water is the level II water as specified in GB/T 6682.

3.1 Reagents

3.1.1 Potassium hydroxide (KOH).
3.1.2 Potassium borohydride (KBH4).
3.1.8 Magnesium oxide (MgO).

3.2 Reagent preparation

3.2.1 Potassium hydroxide solution (5 g/L). WEIGH 5 g of potassium hydroxide;

USE water to dilute it to 1000 mL; MIX it uniformly.

3.2.2 Potassium borohydride alkaline solution (10 g/L). WEIGH 10 g of

potassium borohydride; USE potassium hydroxide solution (5 g/L) to dissolve it;

3.2.3 Pre-reducing agent solution. WEIGH 5.0 g of thiourea; ADD about 80 mL

of water to dissolve it; ADD 5.0 g of ascorbic acid; after it is completely

dissolved, USE water to dilute it to 100 mL; MIX it uniformly; AND this solution

shall be prepared before use.

3.4 Standard solution preparation

3.4.1 Arsenic standard stock solution (1000 mg/L). USE the standard solution

certified by the state AND awarded with the standard substance certificate, or

PREPARE it in accordance with the requirements of GB/T 602.

3.4.2 Arsenic standard intermediate (1.00 mg/L). accurately PIPETTE 10.0 mL

of arsenic standard stock solution into a 100 mL volumetric flask; ADD the

hydrochloric acid solution (5 + 95) to the mark;

4 Instrument and equipment

4.1 Atomic fluorescence photometer. with arsenic hollow cathode lamp.

4.2 Muffle furnace.

4.3 Analytical balance. sensitivity of 1 mg.

5 Analytical procedures

5.1 Pretreatment of sample

TAKE appropriate amount of sample; CRUSH it and MIX it uniformly. WEIGH 1

g ~ 3 g of sample (accurate to 0.001 g); PLACE it in a crucible with cover; ADD

10 mL of magnesium nitrate solution (150 g/L);

5.2 Determination

5.2.1 Instrument test conditions

ADJUST the performance of the instrument to the best condition, AND the

instrument reference conditions are as follows. photomultiplier tube voltage.

400 V; arsenic hollow cathode lamp current. 35 mA; atomizer. temperature

820 °C ~ 850 °C; height. 8 mm; argon flow rate. carrier gas 400m L/min.

5.2.3 Sample determination

TAKE 20 mL of the sample digestion solution into a 25 mL colorimetric tube;

ADD 5 mL of pre-reducing agent solution; MIX it uniformly; PLACE it for 30 min;

MAKE determination on the instrument; QUANTIFY it by comparison with the

standard series; and meanwhile MAKE the blank test.

6 Expression of analysis results

The arsenic content in the sample is calculated in accordance with the formula

7 Precision

The absolute difference between the two independent determinations obtained

under repeatability shall not exceed 20% of the arithmetic mean.

8 Others

When calculated using the sample amount of 0.5 g and the constant volume of

25 mL, the method detection limit is 0.05 mg/kg AND the limit of quantification

is 0.15 mg/kg.

9 Principles

The food simulant is used to soak the portion of the food contact materials and

products which are expected to contact with the food part, thiourea is added to

the soaking solution to pre-reduce the pentavalent arsenic to trivalent arsenic,

which reacts with the reduction hydrogen to produce the arsenic hydride;

10 Reagents and materials

Unless otherwise specified, the reagents used in this method are of analytical

pure AND the water is the level II water as specified in GB/T 6682.

10.1 Reagents

10.2 Reagent preparation

10.2.1 Potassium hydroxide solution (5 g/L). WEIGH 5 g of potassium

hydroxide; USE water to dilute it to 1000 mL; MIX it uniformly.

10.2.2 Potassium borohydride alkaline solution (10 g/L). WEIGH 10 g of

potassium borohydride; USE potassium hydroxide solution (5 g/L) to dissolve it;

MAKE its volume reach to 1000 mL; AND this solution shall be prepared before

use.

10.4 Standard solution preparation

10.4.1 Arsenic standard stock solution (1000 mg/L). USE the standard solution

certified by the state AND awarded with the standard substance certificate, or

PREPARE it in accordance with the requirements of GB/T 602.

10.4.2 Arsenic standard intermediate (1.00 mg/L). accurately PIPETTE 10.0

mL of arsenic standard stock solution into a 100 mL volumetric flask; ADD the

hydrochloric acid solution (5 + 95) to the mark; MIX it uniformly. And then

accurately PIPETTE 1.00 mL of this arsenic standard solution into a 100 mL

volumetric flask; ADD hydrochloric acid solution (5 + 95) to the mark; MIX it

uniformly.

......

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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 11 pages — is available in the English PDF.

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