GB 5009.15-2014 (GB 5009.15-2023 Newer Version) PDF English
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National food safety standard - Determination of cadmium in foods
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| GB 5009.15-2014 | English | 80 |
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National Food Safety Standard -- Determination of Cadmium in food
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| GB/T 5009.15-2003 | English | 399 |
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Determination of cadmium in foods
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| GB/T 5009.15-1996 | English | 279 |
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Method for determination of cadmium in foods
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| GB 5009.15-1985 | English | 199 |
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Method for determination of cadmium in foods
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GB 5009.15-2014: PDF in English GB 5009.15-2014
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard
Determination of Cadmium in Foods
ISSUED ON. JANUARY 28, 2015
IMPLEMENTED ON. JULY 28, 2015
Issued by. National Health and Family Planning Commission of the PRC
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Principle ... 4
3 Reagents and Materials ... 4
4 Apparatuses and Instruments ... 5
5 Analytical Procedure ... 6
6 Analytical Result Expression ... 9
7 Precision ... 9
8 Others ... 9
Foreword
This Standard replaces GB/T 5009.15-2003 Determination of Cadmium in Foods.
Compared with GB/T 5009.15-2003, this Standard mainly has the following changes.
--- Change the standard name into National Food Safety Standard. Determination
of Cadmium in Foods.
--- Delete the Method 2 Atomic Absorption Spectrometry, Method 3 Colorimetry,
and Method 4 Atomic Fluorescence Spectrometry.
National Food Safety Standard
Determination of Cadmium in Foods
1 Scope
This Standard specifies the method for the determination of cadmium in all kinds of
food by graphite furnace atomic absorption spectrometry.
This Standard is applicable to the determination of cadmium in all kinds of food.
2 Principle
After ashing or acid digestion of the specimen, inject certain amount of sample’s
digestive juice into graphite furnace of atomic absorption spectrophotometer; after the
electro-thermal atomic absorption, absorb 228.8nm resonance line; within certain
concentration range, the absorbance value is directly proportional to the content of
cadmium; quantify it by the standard curve method.
3 Reagents and Materials
NOTE 1. Unless otherwise specified, the reagents used in this method are analytical pure;
while the water used is Grade-2 water stated in GB/T 6682.
NOTE 2. The glassware used is required to soak in the nitric acid solution (1+4) for 24h above,
repeatedly resin with water; finally, rinse with deionized water.
3.1 Reagents
3.1.1 Nitric acid (HNO3). guaranteed reagent.
3.1.2 Hydrochloric acid (HCL). guaranteed reagent.
3.1.3 Perchloric acid (HCLO4). guaranteed reagent.
3.1.4 Hydrogen peroxide (H2O2, 30%),
3.1.5 Ammonium dihydrogen phosphate (NH4H2PO4).
3.2 Preparation of reagents
3.2.1 Nitric acid solution (1%). take 10.0mL of nitric acid, add it to 100mL of water,
dilute to 1000mL.
3.2.2 Hydrochloric acid solution (1+1). take 50mL of hydrochloric acid, slowly add it
to 50mL of water.
3.2.3 Nitric acid - perchloric acid mixed solution (9+1). take 9 portions of nitric acid,
and mix with 1 portion of perchloric acid.
3.2.4 Ammonium dihydrogen phosphate solution (10g/L). weigh 10.0g of ammonium
dihydrogen phosphate; after dissolving into 100mL of nitric acid solution (1%),
quantitatively move into 1000mL flask, then dilute with nitric acid solution (1%) to the
specified scale.
3.3 Reference standard material
As for the reference standard material of metal cadmium (Cd). its purity is 99.99% or
the standard substance authenticated nationally and awarded by the standard
substance certificate.
3.4 Preparation of standard solution
3.4.1 Cadmium standard stock solution (1000mg/L). accurately weigh 1g of metal
cadmium reference standard material (accurate to 0.0001g) into a small beaker; add,
for several times, 20mL of hydrochloric acid solution (1+1) to dissolve; add 2 drops of
nitric acid; move to the 1000mL flask; dilute with water to the scale, mix thoroughly; or
purchase the standard substance authenticated nationally and awarded by standard
substance certificate.
3.4.2 Cadmium standard solution (100ng/mL). absorb 10.0mL of cadmium standard
stock solution into a 100mL flask; dilute with nitric acid solution (1%) to the scale; after
diluting in such a way for several times, it becomes the standard solution containing
100.0ng of cadmium per liter.
3.4.3 Cadmium standard curve work solution. accurately absorb 0mL, 0.50mL,
1.0mL, 1.5mL, 2.0mL, 3.0mL of cadmium standard solution into the 100mL flasks
respectively; dilute with nitric acid solution (1%) to the scale; then obtain the standard
serial solutions with the cadmium content of 0ng/mL, 0.50ng/mL, 1.0ng/mL, 1.5ng/mL,
2.0ng/mL, 3.0ng/mL.
4 Apparatuses and Instruments
4.1 Atomic absorption spectrophotometer, attached with graphite furnace.
4.2 Cadmium hollow cathode lamp.
and dilute with nitric acid solution (1%) to the scale, mix thoroughly, and store for
later use; meanwhile, do the reagent blank test.
b) Microwave digestion. weigh dry specimen 0.3g~0.5g (accurate to 0.0001g),
fresh (wet) specimen 1g~2g (accurate to 0.001g), place them into the
microwave digestion tank; add 5mL of nitric acid and 2mL of hydrogen peroxide.
Microwave digestion procedure can, according to the apparatus model, adjust to
the optimal condition. After the completion of the digestion, open the digestion
tank after cool down; the digestive juice turns to be colorless or pale yellow;
conduct heating, acid-driven till it is nearly dry; use small amount of nitric acid
solution (1%) to wash the digestion tank for three times; move the solution to the
10mL or 25mL flask; dilutee with nitric acid solution (1%) to the scale; mix
thoroughly, store for later use; meanwhile do the reagent blank test.
c) Wet digestion method. weigh dry specimen 0.3g~0.5g (accurate to 0.0001g),
fresh (wet) specimen 1g~2g (accurate to 0.001g), place them into conical flask;
put a few glass beads; add 10mL of nitric acid-perchloric acid mixed solution
(9+1), cover the cap, and soak overnight; equip a small funnel, and digest on
the electric hot plate; if it turns to be black-brown, add nitric acid till there is white
smoke; when the digestive juice turns to colorless, transparent, and pale yellow;
after cool down, wash the digestive juice into 10mL or 25mL flask; use small
amount of nitric acid solution (1%) to wash the conical flask for three times;
combine the washings into the flask, and dilute with nitric acid solution (1%) to
the scale; mix thoroughly, store for later use; meanwhile do the reagent blank
test.
d) Dry ashing. weigh dry specimen 0.3g~0.5g (accurate to 0.0001g), fresh (wet)
specimen 1g~2g (accurate to 0.001g), liquid specimen 1g~2g (accurate to
0.001g), place them into the porcelain crucible; firstly use the gentle fire to
carbonize till there is no smoke on the adjustable electric furnace; move into
500°C muffle furnace to do ashing for 6h~8h; then cool down. If individual
specimen is not completely ashed, add 1mL of mixed acid, and heat with gentle
fire on the adjustable electric furnace; after the mixed acid is evaporated,
transfer to the 500°C muffle furnace to do ashing for 1h~2h again till specimen
is digested thoroughly and turns to gray or light gray. Cool down, use nitric acid
solution (1%) to dissolve the ash; move the specimen digestive juice into 10mL
or 25mL flask; use small amount of nitric acid solution (1%) to wash the
porcelain crucible for three times; combine the washings into the flask; dilute
with nitric acid solution (1%) to the scale, mix thoroughly, and store for later use;
meanwhile, do the reagent blank test.
NOTE. Carry out experiment in a well ventilated hood. For the grease-containing sample, try to
avoid using the wet digestion method to digest; preferably take the dry digestion method; if the
wet digestion method is required, then the amount of the sample taken shall not exceed a
maximum of 1g.
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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