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GB 5009.182-2017National food safety standard - Determination of aluminum in foods (English PDF)

食品安全国家标准 食品中铝的测定

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Issued by

National Health and Family Planning Commission of the PRC

Level / Type

National · Mandatory

Issue date

April 6, 2017

Implementation date

October 6, 2017

Scope

GB 5009.182-2017 is the English-translated version of 食品安全国家标准 食品中铝的测定.

GB 5009.182-2017 — This standard specifies some methods for determination of aluminum content in foods, such as spectrophotometry, inductively coupled plasma mass spectrometry, inductively coupled plasma emission spectrometry and graphite furnace atomic absorption spectrometry.

Method I in this standard applies to the detection of aluminum in foods containing aluminum-based food additives. Method II, method III and method IV are applicable to the detection of aluminum in foods. Method I. Spectrophotometry

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Document preview — GB 5009.182-2017

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...7
  • 6 Analysis results expression...8
  • 7 Precision...8
  • 8 Others...8
  • 9 Principles...9
  • 10 Reagents and materials...9
  • 11 Instrument and equipment...10
  • 12 Analytical procedures...10
  • 13 Analysis results expression...13
  • 14 Precision...13
  • 15 Others...13
  • Appendix A Microwave digestion temperature-rise program...14
  • Appendix B Pressure-tank digestion reference heating conditions...15

Foreword

For the determination method of aluminum, this standard replaces GB/T

5009.182-2003 "Determination of aluminum in flour products", GB/T 23374-

2009 "Determination of aluminium in foods - Inductively coupled plasma mass

spectrometry", 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

spectrometric method (ICP-AES)", SN/T 2208-2008 "Determination of sodium,

magnesium, aluminium, calcium, chromium, iron, nickel, copper, zinc, arsenic,

strontium, molybdenum, cadmium, lead, mercury, selenium, in aquatic products

- Microwave digestion - ICP/MS method ".

As compared with GB/T 5009.182-2003, the main changes of this standard are

as follows.

---The standard name is changed to "National food safety standard -

Determination of aluminium in foods";

---Improve method I spectrophotometry;

---Add inductively coupled plasma mass spectrometry as method II;

---Add inductively coupled plasma emission spectrometry as method III;

---Add graphite furnace atomic absorption spectrometry as method IV.

National food safety standard -

Determination of aluminum in foods

1 Scope

This standard specifies some methods for determination of aluminum content

in foods, such as spectrophotometry, inductively coupled plasma mass

spectrometry, inductively coupled plasma emission spectrometry and graphite

furnace atomic absorption spectrometry.

Method I in this standard applies to the detection of aluminum in foods

containing aluminum-based food additives. Method II, method III and method

IV are applicable to the detection of aluminum in foods.

Method I. Spectrophotometry

2 Principles

After the sample is treated, it is in ethylenediamine-HCl buffer solution (pH 6.7-

7.0), with the existence of Triton X-100 and cetylpyridinium bromide (CPB),

trivalence aluminum ion reacts with chrome azurol S to generate blue-green

quaternary micelle.

3 Reagents and materials

Unless otherwise indicated, the reagents used in this method are analytical

pure, the experimental water is the grade-3 water specified in GB/T 6682.

3.1 Reagents

3.1.1 Nitric acid (HNO3). guaranteed reagent.
3.1.2 Sulfuric acid (H2SO4). guaranteed reagent.
3.1.3 Hydrochloric acid (HCl). guaranteed reagent.
3.1.11 Ascorbic acid (C6H8O6).

3.2 Reagent preparation

3.2.1 Hydrochloric acid solution (1+1). MEASURE 50 mL of hydrochloric acid;

MIX it uniformly with 50 mL of water.

3.2.2 Sulfuric acid solution (1%). PIPETTE 1 mL of sulfuric acid; POUR slowly

into 80 mL of water; USE water to dilute it to 100 ml after cooling; MIX it

uniformly.

3.2.12 Ethylenediamine solution (1+2). MEASURE 10 mL of ethylenediamine;

slowly POUR into 20 mL of water; MIX it uniformly.

3.2.13 Ethylenediamine-hydrochloric acid buffer solution (pH6.7~7.0).

MEASURE 100 mL of ethylenediamine; slowly POUR into 200 mL of water

along glass rod; after cooling, ADD slowly 190 mL of hydrochloric acid along

glass rod; MIX it uniformly; if pH > 7.0 or pH < 6.7, USE hydrochloric acid

solution (1+1) or ethylenediamine solution (1+ 2) to adjust pH respectively.

3.2.14 Ascorbic acid solution (10 g/L). WEIGH 1 g of ascorbic acid; USE water

to dilute it to 100 mL; MIX uniformly. Prepare it before use.

3.3 Standards

Aluminum standard solution. 1000 mg/L. Or aluminum standard solution with a

certain concentration which is identified by national authentication and awarded

a reference material certificate.

3.4 Standard solution preparation

3.4.1 Aluminum standard intermediate solution (100 mg/L). Accurately

PIPETTE 1.00 mL of aluminum standard solution (1000 mg/L) into 10 mL

volumetric flask; ADD nitric acid solution (5%) to dilute it to the mark; MIX it

uniformly.

4 Instrument and equipment

Note. All glassware must be soaked in nitric acid solution (1+5) for more than 24h, washed

repeatedly with tap water, finally rinsed with water. Dry it by airing before use.

4.1 Spectrophotometer.

4.2 Balance. sensitivity is 1 mg.

4.5 Constant-temperature oven.

5 Analytical procedures

5.1 Sample Preparation

In the process of sampling and sample preparation, pay attention not to

contaminate the sample; avoid using aluminum-containing appliances.

5.2 Sample digestion

WEIGH 0.2 g ~ 3 g of sample (accurate to 0.001g) or accurately MOVE 0.500

mL ~ 5.00 mL of liquid sample into hard glass digestion tube or conical flask;

ADD 10 mL of nitric acid and 0.5 mL of sulfuric acid; HEAT it on adjustable

temperature-control electric furnace or hot plate, reference conditions.

5.3 Color reaction and colorimetric determination

Respectively PIPETTE 1.00 mL (V2) of sample digestive juice and blank

solution; PLACE them into 25 mL plugged colorimetric tube; ADD water to 10

mL. In addition, TAKE seven 25 mL plugged colorimetric tubes; ADD

respectively aluminum standard working solution 0 mL, 0.500 mL, 1.00 mL,

2.00 mL, 3.00 mL, 4.00 mL and 5.00 mL (in the series standard solution, the

mass of aluminum is 0 µg, 0.500 µg, 1.00 µg, 2.00 µg, 3.00 µg, 4.00 µg, 5.00

µg respectively); ADD 1 mL of sulfuric acid solution (1%) in each tube

successively; ADD water to 10 mL.

6 Analysis results expression

The aluminum content in the sample is calculated according to equation (1).

7 Precision

The absolute difference between two independent determinations obtained

under repeatability conditions shall not exceed 10% of the arithmetic mean.

8 Others

When the sampling weight is 1 g(or 1 mL) and constant volume is 50 mL, the

method detection limit is 8 mg/kg (or 8 mg/L) and the quantitative limit is 25

mg/kg (or 25 mg/L).

9 Principles

After sample digestion, it is atomized through graphite furnace to measure

absorbance value at 257.4 nm.

10 Reagents and materials

Unless otherwise indicated, the reagents used in this method are guaranteed

reagent, the experimental water is the grade-2 water specified in GB/T 6682.

10.1 Reagents

mL of water; MIX it uniformly.

10.2.2 Nitric acid solution (5+95). MEASURE 5 mL of nitric acid; POUR into 95

mL of water; MIX it uniformly.

10.3 Standards

Aluminum standard solution. 1000 mg/L. Or aluminum standard solution with a

certain concentration which is identified by national authentication and awarded

a reference material certificate.

10.4 Standard solution preparation

10.4.1 Aluminum standard intermediate solution (100 mg/L). Accurately

PIPETTE 1.00 mL of aluminum standard solution (1000 mg/L) into 10 mL

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

uniformly.

11 Instrument and equipment

Note. All glassware and digestion pots must be soaked in nitric acid solution

(1+5) for more than 24h, washed repeatedly with tap water, finally rinsed with

water. Dry it by airing before use.

11.1 Graphite Furnace Atomic Absorption Spectrometer. Attached aluminum

11.4 Adjustable hot plate.

11.5 Microwave digestion instrument. equipped with Teflon digestion inner-tank.

11.6 Pressure digestion pot. equipped with Teflon digestion inner-tank.

11.7 Constant-temperature oven

......

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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 15 pages — is available in the English PDF.

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