Some standard content:
CS 67.040
National Standard of the People's Republic of China
GB/T 5009.13-2003
Agency GB/T ER9.13—1Uu6
Determination of copper in food
foods2003-08-11 Issued
Ministry of Health of the People's Republic of China
Standardization Administration of the People's Republic of China
2004-01-01 Implementation
GB/T5009.13--2003
This standard is marked with GB/T5009.13-19 Testing method for micro-copper in food 3. Compared with GB/000,13-16, this standard has the following modifications: 1. The Chinese name of the standard has been revised, and the main name of the standard is micro-copper in food. 2. The main name of the standard is micro-copper in food. 3. The main name of the standard is micro-copper in food. 4. The main name of the standard is micro-copper in food. 5. The main name of the standard is micro-copper in food. 6. The main name of the standard is micro-copper in food. 7. The main name of the standard is micro-copper in food. 8. The main name of the standard is micro-copper in food. 9. The main name of the standard is micro-copper in food. 10. The main name of the standard is micro-copper in food. 11. The main name of the standard is micro-copper in food. 12. The main name of the standard is micro-copper in food. 13. The main name of the standard is micro-copper in food. 14. The main name of the standard is micro-copper in food. 15. The main name of the standard is micro-copper in food. 16. The main name of the standard is micro-copper in food. 17. The main name of the standard is micro-copper in food. 18. The main name of the standard is micro-copper in food. 19. The main name of the standard is micro-copper in food. 20. The main name of the standard is micro-copper in food. The second method of this standard was developed by Tianwei Municipal Health and Epidemic Prevention Station, Chaoyang Provincial Health and Epidemic Prevention Station, and Xinjiang Health and Epidemic Prevention Station. This standard was first issued in 1985, revised for the second time in 1996, and this is the second revision: 1 Scope
Determination of copper in food
This standard specifies the determination method of copper in food: This standard is applicable to the determination of copper in food. GD/T 5009.13—2003
This detection limit: 2.0ng/kg for pyrolysis atomization method; 0.1mg/sg for atomization + 2.5mg/kg for colorimetric method: 2 Normative referenced documents
The following documents are incorporated into this standard through reference in this standard. For undated referenced documents, all subsequent revisions (excluding those due to interruption) or amendments will not apply to this standard. However, the parties selected based on this standard may use the latest version of this document. For undated referenced documents, the latest version shall apply to this standard. CB/T5CUU.11—2UUs The first method for determining total and inorganic carbon in food is based on absorption spectroscopy. 3 Principle: After the sample is treated, it is recorded in an atomic absorption spectrophotometer. After oxidation, it absorbs 324,800 nm of its vibration line. Its absorption value is proportional to the copper content and is adjusted by comparing with the standard series. 4 Reagents: 4.2 Petroleum ether: 4.3 Caustic soda 106 Take 10ml of caustic soda and add 199mL of fresh water. 4.4 Nitric acid 0.%: Take 0.5r:1. Nitric acid and put it in an appropriate amount of water. Then sieve it to 100rml. 4.5 Nitric acid 1+: 4.% nitric acid (nitric acid <4+6), measure 4Cr1. bacterial acid and put it in an appropriate amount of water, and then dilute it to 30m. 4.2 Copper standard solution: weigh the above-mentioned copper standard solution accurately, add 40% sodium hydroxide solution in several portions, the total amount should not exceed 3 μL. Transfer to a 1000mL volumetric bottle and dilute to the mark with water. This solution is equivalent to 1.0 mL of copper solution per liter. 4.9 Copper standard solution: use 1 μm volumetric bottle, dilute to the mark with 5% solution, and dilute several times to the mark with a ratio of 1.0 to 1.0. 4.9 Standard solution: dilute to the mark equivalent to 1.0 mL per liter according to the method in 4.8, and soak the container with 10% nitric acid for more than 24 hours, rinse with water repeatedly, and finally rinse with high-ion water before use. 5.1 Press the ball mill 5.2 Industrial furnace.
5.3 Absorption spectrophotometer is required.
6 Analysis steps
6.1 Sample treatment
6.1.1 Cereals (except 6 grams) tea, coffee, etc. are ground into silicon, passed through a 20 sieve, and the edible part is taken out by ladle, rice, water, etc., cut and slurry is made. Weigh 1.50 μl of nitric acid and place it in a pot or porcelain. Add 5 m nitric acid and place it for 3.5 hours. Steam it on a low heat for 10 minutes, continue to heat it, move it into a furnace, 50% nitric acid, take out the effect, and then 1? m acid and wet it, and steam it on a low heat for 10 minutes. Then heat at 500℃ for 5h. Cool and take out, add 1m. (1-4) solution/time, put into 15.0mL bottle, use wooden clock, and use new.
Take the same cracked whip as the digestion sample, and do the reagent test according to the time method. S.1.2 Aquatic products: Heat the part of the sample. Take 1, 5.3), and operate according to 6.1.1 "put in English or full". 1.3 Milk, condensed milk. Take 2.G3 mixed method, press t, 1.1 self\ need to fly or exhaust.\ knead according to 6.1.4 method lipids: weigh 2.00g mixed test, solid fats and oils are first heated to form a concentrated body, Place in a 100 ml separating funnel, add 10 ml of 10% acid (10%) twice, each time. Add 1 ml of nitric acid solution to a 50 ml volumetric flask. Dilute to the mark with water, filter and prepare the sample. 6.1.5 Prepare the sample, such as raw material, wine, code, etc., and measure it. If there are many samples or the sensitivity of the instrument is insufficient, perform the above test in 6.1.1.
6,2 determination
6. 2. 1 Pipette 2. 0, 1. 0, 2. 0, 4. 0, 6. 5, 8. 0. 10. 0 L of standard rapid-release liquid (T<1, 0 g/mL): 40 g/mL) and separate into 1 ml volume, add 0.5%> dilution to the mark, and adjust. Each liter in the volumetric flask is equivalent to 0, 0.19, 0.20. 4U, 1.60G, HD, 1. 00 AR.
The treated liquid, reagents and each empty inventory are introduced into the flame oxidizer for measurement. The working conditions are: lamp current 1mA~&mA, drum limit 324.8t, spectral band 0. nm, air thickness 3L/mi. Fast flow rate "./min, lamp head commercial mm, gas lamp back correction: use the corresponding light waste content of the standard non-free liquid, make a standard curve or calculate the white residual, test Compare the sample absorption position with the time line or substitute the pollution process to obtain the life 6.2.2 absorb 0, 3.2.0.4.0.f, 0,8.c, 5.5m1. Prepare standard Ⅱ (0.10/ml.) and divide it into 10mL volume bottles, add nitroglycerin (0.56) to release it to room temperature! , take a spoon, and measure each amount in the bottle: 0.0.22, 0.02.3.04, 0,36.0.08, and adjust.
Put the treated sample Liquid, reagent blank solution and each sample of copper standard solution) are measured under the conditions of .-20 others. Microfurnace atomizer is used for measurement. Reference conditions: lamp current 3A.~imA, wavelength 324.cm, light passband 3.L protective gas limit ionization step (take off the gas). Operand FS0T.23 ashing, 20:30020 original 232045. Inquire the standard case II containing the most and corresponding aurora, make standard line or calculate the straight line return square rate, The sample absorption is estimated by comparing with the curve or by using a substitute method.
6.2.3 When there is a disturbance of sodium or other substances: ammonium nitrate (1m/ml) or phosphorus-hydrogen-containing effector or sample tablets (convex value) can be added to the sample before the sample is passed. The above substances can be used as matrix modifiers. Calculation of results
7.1 Flame method
The content of sodium in the test is calculated by the formula (1). X-(AA)XVXi00bzxZ.net
n - 000
Wherein:
X—the content of copper in the test sample, in gram per gram or gram per liter mgg or g/4:—the content of copper in the test sample for determination, in microgram per liter (μg/mL):—the content of silver in the reagent solution, in microgram per liter (ug/mL):—the total volume of the sample after treatment, in milliliter (mL); 192
The mass of the test sample is converted into volume, in units Grams to milliliters (6 or mL): 7.2 Star furnace method
The copper content in the sample is calculated according to formula (2). X=A-A2xI(00
m×V/V>x.1300
——In the test, the unit is grams per kilogram to obtain the mass of the digestion solution adjusted with the test sample, the unit is grams (temperature); A: the appropriate amount of the blank solution prepared in the test.=Microgram (R): Pressure (volume) in grams or milliliters (or): V-test digestion quotient, unit is stoichiometric (mL); test sample digestion volume, unit is liter (ml)) Calculation results retain two significant figures, sample content exceeds 1 (m/k village retain three significant figures. 8 Auxiliary density
GB/T5539.1320C3
The absolute difference between the two clean test results obtained under the conditions of multiplexed density shall not exceed the arithmetic mean value of 10. Second method Diethyl diamino Sodium formate method 9 Principle
After the sample is digested, sodium monoethyl dithiocarbamate forms a yellow complex on copper ions in a reduced pressure wave, and the reaction rate is 10.10.10.2 ...
10.5 Phenol red index (1gI) weighed into 0.1 mmol/l H2O and dissolved to 1cc ml., 16 Copper reagent: -ethyl-hydroxymethylformamide (H2O)N(3H2O): dilute to 1cc ml. If necessary, add more than 30% nitric acid and store in a concentration box.
10.7 Nitric acid (3-9): take 60 mT of nitric acid and dilute to 16cc ml with water. 10.8 Standard saw dust: add water to 4.7.
10.9 Standard saw dust: add water to 4.8.
1 Receiver
Salt photometry
12 Analysis steps required
12.1 Sample digestion
GP/1 5393,11--200312.1.
GH/T 5009.13—2003
12.2 Add the final volume of 1.0 mL of the diluted solution and the same reagent white concentrate, and place them in 125 mL of separate liquid buckets. Add 25 mL of 9.9.50, 1.00, 1.00, 2.00, 2.50 mL of standard solution (equivalent to 5.0), 5.0 (, 15.0, 1.3.0, 20.0, 25.08), and place them in 125 mL of separate liquid buckets. Add 23 mL of each solution (117) to the sample digestion solution, reagent solution, and standard solution, and add 5.0% lemon to each. Mix the indicator liquid of diamine tetrachloride, diamine tetraaldehyde and enzyme red with 3% fluorine water (1:1) until red. Mix the reagents such as 1:1 carbon tetrachloride and 2% carbon tetrachloride, and adjust the concentration by 1% fluorine. After separation, filter the tetrachloride layer through absorbent cotton into a 2cm colorimetric cup and adjust the concentration by 1:10. After the absorbance value of each point is marked, draw a curve or a straight line equation, compare the absorbance of the sample with the curve, and the result is the precision of the measurement.
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