GB 5009.182-2017 PDF in English
GB 5009.182-2017 (GB5009.182-2017) PDF English
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Food safety national standard -- Determination of aluminum in food
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| GB/T 5009.182-2003 | English | 199 |
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Determination of aluminium in flour products
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Standards related to (historical): GB 5009.182-2017
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GB 5009.182-2017: PDF in English GB 5009.182-2017
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National food safety standard -
Determination of aluminum in foods
ISSUED ON. APRIL 6, 2017
IMPLEMENTED ON. OCTOBER 6, 2017
Issued by. National Health and Family Planning Commission of the PRC;
China Food and Drug Administration.
3. No action is required - Full-copy of this standard will be automatically &
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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 ... 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. The absorbance value is measured at a wavelength of 620
nm and compared with the standard series for quantitation.
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.
3.1.4 Ammonium hydroxide (NH3 • H2O). guaranteed reagent.
3.1.5 Anhydrous ethanol (C2H6O). guaranteed reagent.
3.1.6 P-nitrophenol (C6H5NO3).
3.1.7 Chrome azurol S (C23H13O9SCl2Na3).
3.1.8 Ethylenediamine (C2H8N2).
3.1.9 Polyethylene glycol octyl phenyl ether (Triton X-100).
3.1.10 Cetylpyridinium bromide (CPB, C21H38BrN).
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.
3.2.3 P-nitrophenol ethanol solution (1 g/L). WEIGH 0.1 g of p-nitrophenol;
DISSOLVE it in 100 mL of anhydrous ethanol; MIX it uniformly.
3.2.4 Nitric acid solution (5%). MEASURE 5 mL of nitric acid; ADD water to
dilute it to 100 mL; MIX it uniformly.
3.2.5 Nitric acid solution (2.5%). MEASURE 2.5 mL of nitric acid; ADD water to
dilute it to 100 mL; MIX it uniformly.
3.2.6 Ammonium hydroxide solution (1+1). MEASURE 10 mL of ammonium
hydroxide; POUR into 10 mL of water; MIX it uniformly.
3.2.7 Nitric acid solution (2+98). MEASURE 2 mL of nitric acid; MIX it uniformly
with 98 mL of water.
3.2.8 Ethanol solution (1+1). MEASURE 50 mL of anhydrous ethanol;
DISSOLVE it in 50 mL of water; MIX it uniformly.
3.2.9 Chrome azurol S solution (1 g/L). WEIGH 0.1 g of chrome azurol S;
DISSOLVE it in 100 mL of ethanol solution (1+1); MIX it uniformly.
3.2.10 TritonX-100 solution (3%). PIPETTE 3 mL of TritonX-100; PLACE it into
100 mL volumetric flask; ADD water to dilute it to the mark; MIX it uniformly.
3.2.11 CPB solution (3 g/L). WEIGH 0.3 g of CPB; DISSOLVE it in 15 mL of
anhydrous ethanol; ADD water to dilute it to 100 mL; MIX it uniformly.
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.
After crushing the samples of flour products, bean products, shrimp flavorings
and bakery products uniformly, TAKE out 30 g of sample; PLACE it into
constant-temperature oven at 85°C for 4h.
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. heat it at
100°C for 1h; rise to 150°C and heat it for 1h; rise to 180°C and heat it for 2h;
then rise to 200°C. If it becomes brownish black, ADD nitric acid again to digest;
until the tube mouth emits white smoke, digestive juice is colorless and
transparent or slightly yellow. TAKE it out; after cooling, USE water to transfer
and dilute it to 50 mL (V1) volumetric flask; MIX it uniformly for spare-use.
Meanwhile, DO a reagent blank test.
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.
ADD dropwise 1 drop of p-nitrophenol ethanol solution (1 g/L) into standard
tube, sample tube and reagent blank tube; MIX it uniformly; ADD dropwise
ammonium hydroxide solution (1+1) until the solution is light yellow; ADD
dropwise nitric acid solution (2.5%) until the yellow just disappears; ADD again
1 mL of nitric acid solution; ADD 1 mL of ascorbic acid solution (10 g/L); after
mixing it uniformly, ADD 3 mL of chrome azurol S solution (1 g/L); after mixing
it uniformly, ADD 1 mL of TritonX-100 solution (3%), 3 mL of CPB solution (3
g/L), 3 mL of ethylenediamine - hydrochloric acid buffer solution; ADD water to
dilute it to 25.0 mL; MIX it uniformly; PLACE it for 40min.
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.
10.4.2 Aluminum standard working solution (1.00 mg/L). Accurately PIPETTE
1.00 mL of aluminum standard intermediate solution (100 mg/L) into 100 mL
volumetric flask; USE nitric acid solution (5 + 95) to dilute it to the mark; after
mixing it uniformly, PIPETTE accurately 1.00 mL from the solution; PLACE it
into 100 mL volumetric flask; USE water to dilute it to the mark; MIX it uniformly.
10.4.3 Aluminum standard series solution. PIPETTE respectively aluminum
standard solution (1.00 mg / L) 0 mL, 2.50 mL, 5.00 mL, 10.0 mL, 15.0 mL and
20.0 mL into 100 mL volumetric flask; ADD nitric acid solution (1+99) to the
mark; MIX it uniformly. The mass concentration of the aluminum standard
solution is 0 μg/L, 25.0 μg/L, 50.0 μg/L, 100 μg/L, 150 μg/L and 200 μg/L
respectively.
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
hollow cathode lamp.
11.2 Balance. sensitivity is 1 mg.
11.3 Adjustable temperature-control electric furnace.
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
12 Analytical procedures
12.1 Sample preparation
temperature, OPEN the digestion tank; CATCH-acid to dry on electric hot plate;
when it is reduced to room temperature, USE a small amount of water to wash
the digestion tank for 3~4 times; COMBINE washing liquid in 25 mL volumetric
flask; Use water to dilute it to the mark; MIX it uniformly for spare-use.
Meanwhile, DO a sample blank test.
12.2.3 Pressure-tank digestion
WEIGH 0.2 g ~ 1 g of solid sample (accurate to 0.001 g) or accurately MOVE
0.500 mL ~ 5.00 mL of liquid sample into pressure digestion inner-tank; ADD 5
mL~ 8mL of nitric acid; COVER inner-cap; TIGHTEN outer-sheath; PLACE it
into constant-temperature oven; after digestion tank is cooled to room
temperature, OPEN the pressure digestion tank; TAKE out inner-tank; CATCH-
acid to dry on electric hot plate; when it is reduced to room temperature, USE
a small amount of water to wash the digestion tank for 3~4 times; COMBINE
washing liquid in 25 mL volumetric flask; Use water to dilute it to the mark; MIX
it uniformly for spare-use. Meanwhile, DO a sample blank test. (specific
digestion conditions refer to Appendix B).
12.3 Determination
12.3.1 Instrument’s test conditions
Adjust to optimum state according to performance of each instrument. The
reference conditions are a wavelength of 257.4 nm, a slit of 0.5 nm, a lamp
current of 10 mA ~ 15 mA, a drying temperature of 85° C. ~ 120° C. for 30 s; an
ashing temperature of 1000° C. ~ 1200° C. for 15 s to 20 s; an atomization
temperature of 2750° C. for 4s ~ 5s; internal gas flow 0.3 L/min, the injection
volume 10 μL, stop gasification during atomization.
12.3.2 Drawing of standard curve
LEAD 10 μL of standard series solution (select the best injection volume
according to instrumentation) into graphite tube from low to high according to
mass concentration; MEASURE absorbance value after atomization. With the
mass concentration as abscissa AND absorbance value as vertical axis, DRAW
a standard curve.
12.3.3 Determination of sample solution
According to the best injection volume of instrument, ...
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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