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GB 5009.14-2017National food safety standard - Determination of Zinc in Foods (English PDF)

食品安全国家标准 食品中锌的测定

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Issued by

National Health and Family Planning Commission of the People 's Republic of China

Level / Type

National · Mandatory

Issue date

April 6, 2017

Implementation date

October 6, 2017

Scope

GB 5009.14-2017 is the English-translated version of 食品安全国家标准 食品中锌的测定.

GB 5009.14-2017 — This Standard specifies the flame atomic absorption spectrometry method, the inductively coupled plasma emission spectroscopy method, the inductively coupled plasma mass spectrometry method and the dithizone colorimetric method in the determination of zinc in foods.

This Standard is applicable to the determination of zinc in foods, irrespective of materials. Method 1 -- Flame atomic absorption spectrometry

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Document preview — GB 5009.14-2017

National Standard of the People's Republic of China

Issued by: National Health and Family Planning Commission of the People 's Republic of China

Contents

  • Foreword...3
  • 1 Scope...4
  • 2 Principle...4
  • 3 Reagents and materials...4
  • 4 Apparatus...5
  • 5 Analysis steps...6
  • 6 Expression of analysis results...8
  • 7 Precision...8
  • 8 Other...8
  • 9 Principle...9
  • 10 Reagents...9
  • 11 Apparatus...12
  • 12 Analysis steps...12
  • 13 Expression of analysis results...13
  • 14 Precision...14
  • 15 Other...14
  • Annex A Microwave digestion temperature rising program...15

Foreword

This Standard replaces GB/T 2009.14-2003 Determination of Zinc in Foods,

GB 5413.21-2010 National food safety standard Determination of calcium,

iron, zinc, sodium, potassium, magnesium, copper and manganese in foods

for infants and young children, milk and milk products, GB/T 23375-2009

Determination of copper, iron, zinc, calcium, magnesium and phosphorus

content in vegetables and derived products, GB/T 9695.20-2008 Meat and

meat products - Method for determination of zinc, GB/T 14609-2008

Inspection of grain and oils - Determination of copper, iron, manganese, zinc,

calcium, magnesium in cereals and derived products by atomic absorption

and flame spectrophotometry, GB/T 18932.12-2002 Method for the

determination of potassium, sodium, calcium, magnesium, zine, iron, copper,

manganese, chromium, lead, cadmium contents in honey - Atomic absorption

spectrometry, NY/T 1201-2006 Determination of copper iron and zinc content

in vegetables and derived products.

Compared with GB/T 2009.14-2003, the main modifications in this Standard

are as follows.

- modified the name of the standard to "National Food Safety Standard -

Determination of Zinc in Foods";

- in the pretreatment method, maintained the dry ashing method, added

the wet digestion, pressure tank digestion and microwave digestion;

- preserved flame atomic absorption spectrometry as Method 1, dithizone

colorimetric method as Method 4;

- added inductively coupled plasma emission spectroscopy as Method 2;

- added inductively coupled plasma mass spectrometry as Method 3;

- added microwave digestion procedures and flame atomic absorption

spectrometer for instrument reference conditions as appendix.

National Food Safety Standard –

Determination of Zinc in Foods

1 Scope

This Standard specifies the flame atomic absorption spectrometry method,

the inductively coupled plasma emission spectroscopy method, the

inductively coupled plasma mass spectrometry method and the dithizone

colorimetric method in the determination of zinc in foods.

This Standard is applicable to the determination of zinc in foods, irrespective

of materials.

Method 1 -- Flame atomic absorption spectrometry

2 Principle

After digestion of the sample, the absorbance shall be measured at 213.9 nm

by flame atomization. The absorbance of zinc in a certain concentration range

shall be proportional to the zinc content, quantitatively compared with the

standard series.

3 Reagents and materials

Unless otherwise noted, the reagents used in this method shall be

guaranteed reagents, and water shall be Grade Two water specified in GB/T

6682.

3.1 Reagents

3.1.1 Nitric acid (HNO3)
3.1.2 Perchloric acid (HClO4)

3.2 Reagent preparation

3.3 Standard product

Zinc oxide (ZnO, CAS number. 1314-13-2). zinc standard solution with a

purity >99.99%, or certified by the state and given a certain concentration of

the standard substance certificate.

3.4 Standard solution preparation

4 Apparatus

NOTE All glassware and polytetrafluoroethylene digestion tanks shall be soaked by

nitric acid (1+5) overnight, repeatedly rinsed with tap water, and finally washed clean

with water.

4.1 Atomic absorption spectrometer. with flame atomizer, with zinc hollow

cathode lamp.

4.5 Microwave digestion system. with polytetrafluoroethylene digestion

tank.

4.6 Pressure digestion tank. with polytetrafluoroethylene digestion tank.

4.7 Constant temperature drying oven.

4.8 Muffle stove.

5 Analysis steps

5.1 Sample preparation

NOTE During the sampling and sample preparation, the sample contamination should

be prevented.

5.1.1 Grain, bean samples

Remove the debris from the sample. Crush and store in a plastic bottle.

5.2 Sample pretreatment

5.2.1 Wet digestion

Accurately weigh 0.2 g ~ 3 g (nearest to 0.001 g) of solid sample OR

accurately remove 0.500 mL ~ 5.00 mL of liquid sample in a digestion tube

with scale. Add 10 mL of nitric acid, 0.5 mL of perchloric acid.

5.2.2 Microwave digestion

Accurately weigh 0.2 g ~ 0.8 g (nearest to 0.001 g) of solid sample OR

accurately remove 0.500 mL ~ 3.00 mL of liquid sample in the microwave

digestion tank. Add 5 mL of nitric acid. Digest the sample according to the

procedures of microwave digestion.

5.2.3 Pressure tank digestion

Accurately weigh 0.2 g ~ 1 g (nearest to 0.001 g) of solid sample OR

accurately remove 0.500 mL ~ 5.00 mL of liquid sample in the digestion tank.

Add 5 mL of nitric acid. Cover the inner cover. Tighten the stainless steel

jacket.

5.2.4 Dry ashing

Accurately weigh 0.5 g ~ 5 g (nearest to 0.001 g) of solid sample OR

accurately remove 0.500 mL ~ 10.0 mL of liquid sample in the crucible. Heat it

with small fire. Carbonize to smokeless. Transfer to the muffle furnace for 3h

~ 4h ashing at 550°C. Cool and take it out.

5.3 Determination

5.3.1 Instrument reference conditions

Adjust to the best conditions according to the performance of each instrument.

Refer to Annex B for the conditions for reference.

5.3.2 Standard curve making

Introduce the zinc standard series of solutions into the flame atomizer

according to the mass concentration from low to high. After atomization,

measure the absorbance value. Take the mass concentration as abscissa,

absorbance value as vertical axis to make the standard curve.

6 Expression of analysis results

When the zinc content >=10.0 mg/kg (or mg/L), the results shall be retained to

three effective figures. When the zinc content < 10.0 mg/kg (or mg/L), the

calculation results shall be retained to two significant figures.

7 Precision

The absolute difference between the two independent determinations

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

8 Other

When the sampling volume is 0.5 g (or 0.5 mL), the set volume is 25 mL, the

detection limit of this method shall be 1 mg/kg (or 1 mg/L) and the limit of

quantification shall be 3 mg/kg (or 3 mg/L).

9 Principle

After digestion of the sample, when pH is at 4.0 ~ 5.5, zinc ions and dithizone

shall form a purple red complex.

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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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