GB 31604.38-2016 English PDF

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GB 31604.38-2016: Food contact materials for export -- Paper, regenerated fibre materials -- Determination of arsenic -- Hydride generation-atomic fluorescence spectrometry
GB 31604.38-2016
GB
NATIONAL STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
National food safety standard
Food contact materials and articles –
Determination of arsenic and migration
食品接触材料及制品
ISSUED ON. OCTOBER 19, 2016
IMPLEMENTED ON. APRIL 19, 2017
Issued by. National Health and Family Planning Commission of the PRC
3. No action is required - Full-copy of this standard will be automatically and
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Table of 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).
3.1.3 Thiourea (CN2H4S).
volumetric flask; ADD hydrochloric acid solution (5 + 95) to the mark; MIX it
uniformly.
3.4.3 Arsenic standard series solution. respectively, PIPETTE 0 mL, 0.500 mL,
1.00 mL, 2.00 mL, 3.00 mL, and 4.00 mL of arsenic standard intermediate into
100 mL volumetric flasks; ADD hydrochloric acid solution (5 + 95) to the mark;
MIX it uniformly. The concentration of arsenic standard solution is 0 μg/L, 5.00
μg/L, 10.0 μg L, 20.0 μg/L, 30.0 μg/L and 40.0 μg/L, respectively.
Note. The specific concentration of arsenic in the standard solution series can
be determined in accordance with the sensitivity of the instrument, the linear
range, and the actual concentration of arsenic in the soaking solution.
4 Instrument and equipment
Note. All glassware need to be soaked in the nitric acid solution (1 + 5)
overnight, rinsed with tap water repeatedly, AND finally washed clean with
water.
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); MIX it uniformly; EVAPORATE
it dry at low heating; carefully COVER 1 g of magnesium oxide on the dry
residue; CARBONIZE it in the electrical furnace until there is no black smoke;
TRANSFER it into a 550 °C high temperature furnace for ashing for 4 h. TAKE
it out; LET it cool down; carefully ADD 10 mL of hydrochloric acid solution (1 +
1), to neutralize the magnesium oxide AND dissolve ash; TRANSFER it into a
25 mL volumetric flask; USE the hydrochloric acid solution (5 + 95) to wash the
crucible for several times; COMBINE the washing solution into the volumetric
flask; finally USE water to make its volume reach to the mark; MIX it uniformly
to prepare for use.
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.
100 mL volumetric flasks; ADD the corresponding food simulant to the mark;
MIX it uniformly. The concentration of arsenic standard solution is 0 μg/L, 5.00
μg/L, 10.0 μg L, 20.0 μg/L, 30.0 μg/L and 40.0 μg/L, respectively.
Note. The specific concentration of arsenic in the standard solution series can
be determined in accordance with the sensitivity of the instrument, the linear
range, and the actual concentration of arsenic in the soaking solution. If the
selected food simulant is neutral or alkaline, it is required to add appropriate
amount of nitric acid to make the nitric acid concentration in this solution at
about 5% (volume fraction).
11 Instruments and equipment
Note. All glassware need to be soaked in the nitric acid solution (1 + 5)
overnight, rinsed with tap water repeatedly, AND finally washed clean with
water.
11.1 Atomic fluorescence photometer. with arsenic hollow cathode lamp.
11.2 Analytical balance. sensitivity of 1 mg.
12 Analytical procedures
12.1 Pretreatment of sample
In accordance with the expected use and the conditions of use of the sample to
be measured, MAKE the migration test in accordance with the migration test
methods and test conditions as specified in GB 5009.156 and GB 31604.1.
After the soaking solution is fully mixed uniformly, TAKE portion of the soaking
solution for analysis. If the soaking test solution is neutral or alkaline, ADD
appropriate amount of nitric acid so that the concentration of nitric acid in the
test solution is about 5% (volume fraction). At the same time MAKE the sample
blank test.
12.2 Determination
12.2.1 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;...