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GB 29210-2012: Food additive copper sulphate
Status: Valid
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Food additive copper sulphate
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Basic data
Standard ID: GB 29210-2012 (GB29210-2012)
Description (Translated English): Food additive copper sulphate
Sector / Industry: National Standard
Classification of Chinese Standard: X40
Classification of International Standard: 67.220.20
Word Count Estimation: 10,182
Regulation (derived from): Ministry of Health Bulletin 2012 No. 23
Issuing agency(ies): Ministry of Health of the People's Republic of China
Summary: This Chinese standard applies to copper oxide and sulfuric acid reaction of the food additive copper sulphate.
GB 29210-2012: Food additive copper sulphate
---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Food additive copper sulphate
National Standards of People's Republic of China
National standards for food safety
Food Additives Copper Sulfate
2012-12-25 release
2013-01-25 Implementation
Issued by the Ministry of Health of the People's Republic of China
National standards for food safety
Food Additives Copper Sulfate
1 Scope
This standard applies to copper oxide and sulfuric acid reaction prepared by the food additive copper sulfate.
2 Chemical name, molecular formula and relative molecular mass
2.1 Chemical name
Copper sulfate pentahydrate
2.2 Molecular formula
CuSO4 · 5H2O
2.3 Relative molecular mass
249.7 (according to the.2007 International Relative Atomic Quality)
3 technical requirements
3.1 sensory requirements
Shall comply with the provisions of Table 1.
Table 1 sensory requirements
The project requires a test method
Color blue
State granular crystals or powder
Take appropriate sample in a 50 mL beaker and observe the color and state under natural light
3.2 Physical and chemical indicators
Shall comply with the provisions of Table 2.
Table 2 Physical and chemical indicators
Item Index Test Method
Copper sulfate (CuSO4 · 5H2O) content, w /% 98.0 ~ 102.0 Appendix A A.4
Hydrogen sulfide does not precipitate, w /% ≤ 0.3 Appendix A A.5
Iron (Fe), w /% ≤ 0.01 Appendix A A.6
Lead (Pb)/(mg/kg) ≤ 4 Appendix A A.7
Arsenic (As)/(mg/kg) ≤ 3 Appendix A A.8
Appendix A
Testing method
A.1 Warning
Some of the reagents used in the test methods of this standard are toxic or corrosive and should be operated with appropriate safety and protective measures.
A.2 General provisions
The reagents and water used in this standard, when not specified in other requirements, refer to the analysis of pure reagents and GB/T 6682-2008 in the provisions of the three
Water level. Standard titration solution used in the test, the standard solution for the determination of impurities, preparations and products, without any other requirements,
GB/T 601, GB/T 602, GB/T 603. The solution used refers to an aqueous solution when it is not specified with any solvent formulation.
A.3 Identification test
A.3.1 Reagents and materials
A.3.1.1 Hydrochloric acid.
A.3.1.2 Hydrochloric acid solution. 1 4.
A.3.1.3 Hydrochloric acid solution. 1 1.
A.3.1.4 Ammonia solution. 2 3.
A.3.1.5 barium chloride solution. 100 g/L.
A.3.1.6 Lead acetate solution. 80 g/L.
A.3.1.7 Ammonium acetate solution. 100 g/L.
A.3.1.8 potassium ferrocyanide solution. Weigh 1 g of potassium ferrocyanide [K4Fe (CN) 6 · 3H2O] and dissolve in 10 mL of water. The solution
Liquid is now available.
A.3.2 Identification method
A.3.2.1 Identification of copper ions
A.3.2.1.1 Take about 1g sample, dissolve in 20mL water, add a small amount of hydrochloric acid acidification sample solution. Will be a bright rusty metal
Iron tablets into the acidification of the sample solution, the iron surface will form a red metal copper film.
A.3.2.1.2 Take about 1g sample, dissolve in 20mL water, add excess ammonia solution, first blue precipitate, and then into dark blue
Color solution.
A.3.2.1.3 Take about 1g sample, dissolve in 20mL water, add potassium ferrocyanide solution, generate reddish brown precipitate, precipitate insoluble in hydrochloric acid
Liquid (A.3.1.2).
A.3.2.2 Identification of sulfate ions
A.3.2.2.1 Take about 1g sample, dissolve in 20mL water, add barium chloride solution, which produces a white precipitate, this white precipitate is insoluble in hydrochloric acid
Solution (A.3.1.3).
A.3.2.2.2 Take about 1g sample, dissolve in 20mL water, add lead acetate solution, which produces white precipitate, this white precipitate dissolved in ammonium acetate
Solution.
A.3.2.2.3 Take about 1g sample, dissolve in 20mL water, add hydrochloric acid does not produce precipitation.
A.4 Determination of copper sulfate (CuSO4 · 5H2O) content
A.4.1 Methodological Summary
In the slightly acidic conditions, the sample by adding excess potassium iodide and divalent copper quantitative reaction, with sodium thiosulfate standard titration solution titration precipitation
Of iodine, with starch as an indicator, by the color change to determine the end point.
A.4.2 Reagents and materials
A.4.2.1 Potassium iodide.
A.4.2.2 Glacial acetic acid.
A.4.2.3 Ammonium thiocyanate solution. 100 g/L.
A.4.2.4 sodium thiosulfate standard titration solution. c (Na2S2O3) = 0.1mol/L.
A.4.2.5 Starch indicator. 10 g/L (for a period of 2 weeks).
A.4.3 Analysis steps
Weigh 0.8g ~ 1.0g sample, accurate to 0.0002g, placed in 250mL iodine bottle, add 50mL water dissolved, add 4mL ice
Acetic acid and 3g potassium iodide, shake, placed in the dark place 10min. Titration with sodium thiosulfate standard titration solution to the solution was pale yellow, plus
Into the 3mL starch indicator solution, continue to titration to the solution was light blue, add 20mL ammonium thiocyanate solution, shake. Continue titration to solution blue
Color disappears, that is the end.
While the blank test. Blank test in addition to no sample, the other operations and the type and amount of reagents added (standard titration solution
And the same).
A.4.4 Calculation of results
The mass fraction w1 of copper sulfate (CuSO4 · 5H2O) is calculated according to formula (A.1)
w1 =
[(V1-V0)/1000] cM
m x 100%
(A.1)
Where.
V1 --- titration sample solution consumed sodium thiosulfate standard titration solution volume value in milliliters (mL);
V0 --- titration blank sample solution consumed by sodium thiosulfate standard titration solution volume in milliliters (mL);
c - the exact value of the concentration of sodium thiosulfate standard titration solution in moles per liter (mol/L);
m - the mass of the sample, in grams (g);
M - copper (CuSO4 · 5H2O) molar mass in grams per mole (g/mol) (M = 249.7);
1000 --- conversion factor.
The experimental results are based on the arithmetic mean of the parallel measurement results. The absolute difference between the two independent determinations obtained under repeatability conditions
The value is not greater than 0.3%.
Determination of hydrogen sulfide non - precipitate
A.5.1 Methodological Summary
Hydrogen sulfide precipitated in the sample of copper plasma, non-precipitated ions remain in the solution, filtered filtrate by evaporation, after burning determination of sulfur
Hydrogen does not precipitate the content.
A.5.2 Reagents and materials
A.5.2.1 Hydrogen Sulfide.
WARNING. Hydrogen sulfide is a toxic gas and the operation should be carried out in a fume hood.
A.5.2.2 Sulfuric acid solution. 1 100.
A.5.3 Instruments and equipment
A.5.3.1 porcelain evaporative dish (or porcelain crucible). capacity of 100mL.
A.5.3.2 High temperature furnace. can control the temperature of 800 ℃ ± 25 ℃.
A.5.3.3 Hydrogen Sulfide Absorber.
The hydrogen sulphide absorption device is shown in Figure A.1. A saturated copper sulfate solution is used in the tail gas absorption bottle.
Figure A.1 Hydrogen Sulfide Absorption Device
A.5.4 Analysis steps
Weigh the sample of 5.00 g ± 0.01 g, placed in a sample solution absorption flask (250 mL Erlenmeyer flask), add.200 mL of sulfuric acid solution,
To 70 ℃, according to the hydrogen sulphide absorption device diagram to connect the sample solution absorption bottle and tail gas absorption bottle, the first leak test,
Liquid hydrogen sulfide gas into the liquid until the copper ion precipitation completely. The precipitated sample solution was transferred to a 250 mL volumetric flask and diluted with water
Release to the scale, shake. Placed to precipitate sinking, with a slow qualitative filter paper dry filter, discard the initial filtrate 10mL. Remove.200 mL with pipette
The filtrate is transferred to a 250 mL beaker, covered with a surface dish, placed in a pad of asbestos net on a small furnace to heat the solution (the heating process should be adjusted at any time
The whole furnace temperature, to prevent the solution splash). Evaporated to about 20 mL of solution, and the solution was transferred to a temperature of 800 ° C ± 25 ° C until the mass was constant
(Or porcelain crucible), placed in a water bath heated to dry, and then in the electric furnace with a fire heated to sulfuric acid smoke exhausted, transferred to high temperature
Furnace, at 800 ℃ ± 25 ℃ under the conditions of burning to a constant quality. After cooling, weigh. Retention residue A was used for the determination of iron (A.6.2).
A.5.5 Calculation of results
Hydrogen sulfide does not precipitate the mass fraction w2, calculated according to formula (A.2).
w2 =
m1-m0
m × (200/250) × 100%
(A.2)
Where.
m1 --- the value of the residue and porcelain evaporative dish, in grams (g);
m0 --- porcelain evaporative dish quality value, the unit is grams (g);
m - the mass of the sample, in grams (g);
200 --- the value of the volume of the sample solution, in milliliters (mL);
250 --- Volume of the volume of the bottle, in milliliters (mL).
The experimental results are based on the arithmetic mean of the parallel measurement results. The absolute difference between the two independent determinations obtained under repeatability conditions
The value is not more than 0.02%.
A.6 Determination of iron (Fe)
A.6.1 Inductively Coupled Plasma Atomic Emission Spectrometry (Arbitration)
A.6.1.1 Method Summary
The content of iron in the sample was determined by inductively coupled plasma emission spectrometry, and the interference of copper matrix was corrected with yttrium as internal standard.
A.6.1.2 Reagents and materials
A.6.1.2.1 Nitric acid solution. 1 1.
A.6.1.2.2 Yttrium (Y) internal standard liquid. 0.2 mg/mL.
Accurately weighed 0.127g of yttrium oxide (Y2O3), dissolved in a small amount of hydrochloric acid, diluted with hydrochloric acid solution (99) to 100mL. The
Solution for the yttrium internal standard stock solution, 1mL solution containing yttrium (Y) 1mg.
20 mL of the above solution was removed from the pipette, placed in a 100 mL volumetric flask, diluted with hydrochloric acid solution (99) to a graduated volume and shaken. The
Solution for the yttrium internal standard use of liquid, 1mL solution containing yttrium (Y) 0.2mg.
A.6.1.2.3 Iron (Fe) standard solution. 0.1 mg/mL.
A.6.1.2.4 Water. in line with GB/T 6682-2008 in the provisions of secondary water.
A.6.1.3 Instruments and equipment
Full - spectrum Direct - reading Inductively Coupled Plasma Atomic Emission Spectrometer (ICP - OES).
A.6.1.4 Analysis steps
A.6.1.4.1 Preparation of sample solution
Weigh about 2g sample, accurate to 0.0002g, add water dissolved into the 100mL volumetric flask, add 2.00mL yttrium internal standard use
Liquid, 2mL nitric acid solution, diluted with water to the mark, shake.
A.6.1.4.2 Preparation of working curve solutions
Transfer the 0 mL, 1.00 mL, 2.00 mL, 4.00 mL iron standard solutions separately in four 100 mL volumetric flasks
2.00mL yttrium internal standard use of liquid, 2mL nitric acid solution, diluted with water to the mark, shake.
A.6.1.4.3 Determination
Select the best instrument operating conditions, at the wavelength of 238.204nm, the sample solution and the working curve of the solution, with the internal standard
The calibration wavelength of the internal standard yttrium was 242.219 nm.
A.6.1.5 Calculation of results
The mass fraction w3 of iron (Fe) is calculated according to formula (A.3)
w3 = ρ
× 0.1
m x 1000 x 100%
(A.3)
Where.
ρ --- the value of the iron concentration detected by the working curve in milligrams per liter (mg/L);
m - the mass of the sample, in grams (g);
0.1 --- volume of the volume of the bottle, in liters (L);
1000 --- conversion factor.
The experimental results are based on the arithmetic mean of the parallel measurement results. The absolute difference between the two independent determinations obtained under repeatability conditions
The value is not more than 0.001%.
A.6.2 Thiocyanate colorimetric method
A.6.2.1 Methodological summary
The iron contained in the sample was oxidized to ferric iron by ammonium persulfate, reacted with ammonium thiocyanate to form a blood red complex, and reacted with a standard colorimetric solution
Comparison.
A.6.2.2 Reagents and materials
A.6.2.2.1 Hydrochloric acid.
A.6.2.2.2 Nitric acid.
A.6.2.2.3 ammonium persulfate.
A.6.2.2.4 Ammonium thiocyanate solution. 80 g/L.
A.6.2.2.5 iron standard solution. 1mL solution containing iron (Fe) 0.010mg. Transfer 10 mL of iron prepared according to GB/T 602 with pipettes
Standard solution, placed in 100mL volumetric flask, diluted with water to the mark, shake.
A.6.2.3 Analysis steps
A.6.2.3.1 Determination of hydrogen sulfide non-precipitate residue A (A.5.4) by adding 2mL hydrochloric acid and 0.1mL nitric acid, capped surface dish, set
Digestion on a steam bath for 20 min. Remove the surface pan and continue to evaporate to dryness. Add 1 mL of hydrochloric acid to dissolve the residue and transfer to a capacity of 50 mL
Bottle, diluted with water to the mark, shake. Five mL of the above solution was removed from the pipette, placed in a 50 mL colorimetric tube, and diluted with water to about
30mL, add 2mL hydrochloric acid, shake. Add 0.04g ammonium persulfate, shake to dissolve, add 10mL ammonium thiocyanate solution, diluted with water to
Scale, shake. The color of the sample solution should not be deeper than the color produced by the standard colorimetric solution.
A.6.2.3.2 Standard colorimetric solution is to remove 5mL iron standard solution with pipette, placed in 50mL colorimetric tube, the following according to A.6.2.3.1
From "diluted with water to about 30mL" to start with the same sample solution operation.
A.7 Determination of lead (Pb)
A.7.1 Methodological Summary
The iron salts were added to the samples, and the iron ions and lead ions in the samples were co-precipitated with aqueous ammonia to separate them from the main copper salt. The precipitate was filtered, washed,
Dissolved by atomic absorption spectrophotometry for determination.
A.7.2 Reagents and materials
A.7.2.1 Ammonium carbonate.
A.7.2.2 nitric acid.
A.7.2.3 Ammonia.
A.7.2.4 Hydrochloric acid solution. 1 1.
A.7.2.5 Hydrochloric acid solution. 1 100.
A.7.2.6 Nitric acid solution. 1 5.
A.7.2.7 Iron solution. 8g/L. Weigh 57.8 g of ferric nitrate [Fe (NO3) 3 · 9H2O] in 1000 mL of nitric acid (1 100)
Mix well.
A.7.2.8 Washing solution. Weigh 10 g of ammonium carbonate in 500 mL of water, add 20 mL of ammonia and mix well.
A.7.2.9 Lead (Pb) standard solution. 0.10 mg/mL.
A.7.2.10 Water. in line with GB/T 6682-2008 in the provisions of secondary water.
A.7.3 Instruments and equipment
Atomic Absorption Spectrophotometer. With lead hollow cathode lamp.
A.7.4 Analysis steps
A.7.4.1 Cleaning of the instrument
The glass instruments used were soaked in nitric acid solution (A.7.2.6) overnight, rinsed with tap water, and finally rinsed with water.
A.7.4.2 Drawing of working curves
Remove the 0 mL, 1.00 mL, 2.00 mL, 3.00 mL lead standard solution with a pipette and place in a 50 mL volumetric flask
Into 2mL hydrochloric acid solution (A.7.2.4), 10.0mL iron solution, diluted with water to the mark, shake. Use air - acetylene flame at wavelength
283.3nm, water zero, the use of atomic absorption spectrophotometer to determine the absorbance of the working curve. The absorbance from each standard solution
Minus the absorbance of the blank solution, the concentration of lead for the abscissa, the corresponding absorbance for the vertical axis, drawing the work curve.
A.7.4.3 Preparation of sample solution
Weigh about 20g sample, accurate to 0.01g, placed in 250mL beaker, add appropriate amount of water and 3 drops of nitric acid, heated to boiling, slightly cold, adding
10.0mL iron solution, diluted with water to about.200mL, slowly stirring with ammonia water to the solution showed dark blue and excessive 20mL, by adding
10g ammonium carbonate, cover the surface of the solution will be heated to micro-boiling 5min, 70 ℃ ~ 80 ℃ water bath for 1h, precipitation with medium-speed qualitative filter
Paper filter, wash the beaker with a hot wash solution and filter paper to the filter paper without blue, and then warm water (40 ℃ ~ 50 ℃) washing once, discard the filtrate. Water will be
The precipitate was washed into the original beaker and the remaining precipitate on the filter paper was dissolved in 10 mL of hot hydrochloric acid solution (A.7.2.4) and washed with hot hydrochloric acid solution (A.7.2.5)
Polyester to filter paper colorless, and then wash 3 times, lotion into the original beaker, the water bath evaporation to the solution left 2mL ~ 3mL, into the 50mL volumetric flask
, Cooled to room temperature, diluted with water to the mark, shake.
A.7.4.4 Determination
The air-acetylene flame was used at zero wavelength of 283.3 nm, and the sample was measured by atomic absorption spectrophotometer.
Luminosity. Check the concentration of lead in the sample solution from the working curve (mg/L).
A.7.5 Calculation of results
Lead (Pb) mass fraction w4, expressed in milligrams per kilogram (mg/kg), calculated according to formula (A.4).
w4 = ρ
× 0.05 × 1000
(A.4)
Where.
ρ --- the concentration of lead detected by the working curve in milligrams per liter (mg/L);
m - the mass of the sample, in grams (g);
0.05 --- volume of the volume of the bottle, the unit is liters (L);
1000 --- conversion factor.
The experimental results are based on the arithmetic mean of the parallel measurement results. The absolute difference between the two independent determinations obtained under repeatability conditions
The value is not greater than 1mg/kg.
A.8 Determination of arsenic (As)
A.8.1 Methodological Summary
Thiourea - ascorbic acid as matrix modifier to eliminate the interference of copper in the sample, the use of hydride generation atomic fluorescence spectrometry determination of arsenic content.
A.8.2 Reagents and materials
A.8.2.1 Hydrochloric acid solution. 5 95.
A.8.2.2 Sodium hydroxide solution. 5 g/L.
A.8.2.3 Potassium borohydride solution. 20 g/L. About 20 g of potassium borohydride was weighed and dissolved in 1000 mL of 5 g/L sodium hydroxide solution.
A.8.2.4 thiourea - ascorbic acid mixture. Weigh 10g thiourea, add about 80mL water to stir, add 10g ascorbic acid, dissolved
Diluted with water to 100 mL.
A.8.2.5 arsenic standard solution Ⅰ. 1mL solution containing arsenic (As) 0.010mg. Transfer with 10 mL of pipettes according to GB/T 602
Arsenic standard solution, placed in 100mL volumetric flask, diluted with water to the mark, shake. The solution is now used.
A.8.2.6 arsenic standard solution II. 1mL solution containing arsenic (As) 0.5μg. Remove 5 mL of arsenic standard solution I with a pipette and place in 100 mL capacity
Bottle, diluted with water to the mark, shake. The solution is now used.
A.8.3 Instruments and equipment
Dual-channel atomic fluorescence photometer. with arsenic hollow cathode lamp.
A.8.4 Analysis steps
A.8.4.1 Drawing of working curves
Remove 0 mL, 0.50 mL, 1.00 mL, 1.50 mL, 2.00 mL, 2.50 mL of arsenic standard solution II with a pipette, placed in 100 mL
Volume bottle, add 5mL hydrochloric acid solution, 20mL thiourea - ascorbic acid mixture, diluted with water to the mark, shake. Place it for 15min
The absorbance of the solution was measured with a two-channel atomic fluorescence spectrometer. The absorbance of the blank solution is subtracted from the absorbance of each standard solution,
The qu......
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