GB 1886.235-2016 English PDF (GB1886.235-2016)

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GB 1886.235-2016: National food safety standard - Food additives - Citric acid
GB 1886.235-2016
(Food safety national standard - Food additive - Citric acid)
National Standards of People's Republic of China
National Food Safety Standard
Food additive citric acid
Issued on.2016-08-31
2017-01-01 implementation
People's Republic of China
National Health and Family Planning Commission released
Foreword
This standard replaces GB 1987-2007 "food additive citric acid."
This standard compared with GB 1987-2007, the main changes are as follows.
--- Standard name was changed to "national food safety standards of food additive citric acid";
--- Remove the water insoluble, light transmittance and rail projects;
--- Modify the total arsenic (arsenic meter) detection method;
--- Modify the detection method of lead.
National Food Safety Standard
Food additive citric acid
1 Scope
This standard applies to starch or sugar feedstock by fermentation of food additive citric acid.
2 molecular formula, relative molecular mass and structural formula
Formula 2.1
Anhydrous citric acid. C6H8O7
Citric acid monohydrate. C6H8O7 · H2O
2.2 formula
CHO COOH
CH2 COOH
CH2 COOH
CHO COOH · H2O
CH2 COOH
CH2 COOH
Anhydrous citric acid citric acid monohydrate
2.3 relative molecular mass
Anhydrous Citric Acid. 192.13 (according to 2013 international relative atomic mass)
Citric acid monohydrate. 210.14 (according to 2013 international relative atomic mass)
3 Technical requirements
3.1 Sensory requirements
Sensory requirements shall comply with the requirements of Table 1.
Table 1 Sensory requirements
Project requires test methods
Colorless or white color
status
Crystalline granules or powder, odorless, taste very acid monohydrate
Slightly citric acid weathering in dry air
Take the right amount of sample is placed in a clean, dry white porcelain dish, in natural light
The line, observe its color and status
3.2 Physical and Chemical Indicators
Physical and chemical indicators should be consistent with the provisions of Table 2.
Table 2. Physical and chemical indicators
project
index
Anhydrous citric acid citric acid monohydrate
Testing method
Citric acid content, w /% 99.5 ~ 100.5 99.5 ~ 100.5 Appendix A A.4
Water, w /% ≤0.5 7.5 ~ 9.0 A.5 Appendix A
Easy carbonized matter ≤ 1.0 1.0 A.6 in Appendix A
Sulfated ash, w /% ≤ 0.05 0.05 Appendix A A.7
Sulfate, w /% ≤ 0.010 0.015 Appendix A A.8
Chloride, w /% ≤ 0.005 0.005 Appendix A, A.9
Oxalate, w /% ≤ 0.01 0.01 Appendix A A.10
Calcium, w /% ≤ 0.02 0.02 Appendix A A.11
Lead (Pb)/(mg/kg) ≤ 0.5 0.5 GB 5009.12
Total arsenic (As)/(mg/kg) ≤ 1.0 1.0 GB 5009.11
Appendix A
Testing method
A.1 Safety Tips
Reagents The standard test methods used for toxic or corrosive, the operation should take appropriate safety and health practices.
A.2 General Provisions
Unless otherwise specified in this standard, the purity of the reagents used should be analytically pure, the standard titration solution, impurity measurement standard solution preparation
And products, should be GB/T 601, GB/T 602, the provisions of the preparation of GB/T 603, the test water should be consistent with GB/T 6682 in the three water regulation
set. Solution was used in the tests did not indicate what is formulated with solvent, it refers to an aqueous solution.
A.3 Identification Test
A.3.1 Reagents and materials
A.3.1.1 ethanol.
A.3.1.2 ether.
A.3.1.3 sulfuric acid solution. amount of sulfuric acid 29mL, slowly inject approximately 700mL of water, cooled and diluted to 1000mL.
A.3.1.4 mercury sulfate solution. Weigh mercuric oxide 5g, add water 40mL, slowly adding sulfuric acid 20mL, with stirring, add water 40mL
Stirring to dissolve.
A.3.1.5 potassium permanganate solution. c (
5 KMnO4
) = 0.1mol/L.
A.3.1.6 sodium hydroxide solution. 50g/L.
A.3.1.7 pyridine - acetic anhydride solution. pyridine and acetic anhydride were 3.1 volume ratio.
A.3.2 Analysis step
A.3.2.1 sample soluble in water, soluble in alcohol, ether-soluble.
A.3.2.2 take appropriate 25mL sample in the crucible, ignition, that decompose slowly, but may not occur caramel smell.
A.3.2.3 Weigh samples 50mg, dissolved in water and diluted to 10mL. 2mL draw in 25mL colorimetric tube with sodium hydroxide solution
Neutralized, add 1 drop of sulfuric acid solution, heated to boiling, plus potassium permanganate solution 1 drop, shake, purple will fade; adding mercury sulfate solution
1 drop, producing a white precipitate.
A.3.2.4 Weigh 5mg sample in 25mL colorimetric tube, add pyridine - acetic anhydride solution of about 5mL, shaking, that is generated to the red or yellow
Purple solution.
A.4 Determination of citric acid content
A.4.1 Method summary
In an aqueous medium, with phenolphthalein as the indicator solution, titration using sodium hydroxide standard titration solution of citric acid solution, sodium hydroxide according to consumption
The amount of the standard titration solution of citric acid content is calculated.
A.4.2 Reagents and materials
A.4.2.1 sodium hydroxide standard titration solution. c (NaOH) = 0.5mol/L.
A.4.2.2 phenolphthalein indicator solution. 10g/L.
A.4.2.3 carbon dioxide-free water.
A.4.3 Analysis step
Weigh the sample 1g, accurate to 0.0001g, placed in 150mL conical flask, adding carbon dioxide-free water 50mL dissolved, add phenolphthalein
3 drops of indicator solution, titration with sodium hydroxide standard titration solution to the pink end point. While doing the blank test.
A.4.4 Calculation Results
A water content of citric acid citric acid (anhydrous citric acid meter) mass fraction w1 according to formula (A.1) calculation of citric acid anhydrous citric acid
The content of the mass fraction w2 according to equation (A.2) calculations.
w1 =
(V1-V0) × c × 0.06404
m × (1-0.08570) ×
100% (A.1)
w2 =
(V1-V0) × c × 0.06404
m × 100%
(A.2)
Where.
Volume V1 --- sample titration by the consumption of sodium hydroxide standard titration solution, in milliliters (mL);
V0 --- blank titration by the consumption of sodium hydroxide standard titration solution volume in milliliters (mL);
C --- concentration of sodium hydroxide standard titration solution, expressed in moles per liter (mol/L);
0.06404 --- anhydrous citric acid and sodium hydroxide 1.00mL [c (NaOH) = 1.000mol/L] equivalent in grams of
In grams;
m --- sample mass, in grams (g);
0.08570 --- citric acid monohydrate in water content of the theory, namely 18.01/210.14 = 0.08570.
The test results of the arithmetic mean of the results of parallel determination prevail retain a decimal.
Two independent determination results under the absolute difference between the same condition is not more than 0.2% of the arithmetic mean.
A.5 Determination of Moisture
According to GB 5009.3 Karl Fischer method. Wherein the sample weight of citric acid monohydrate 0.1g, anhydrous citric acid take 1g; absolute methanol
20mL.
In two independent determination results obtained under repeatability conditions, anhydrous citric absolute difference is not more than 5% of the arithmetic mean; a water
Citric acid is the absolute difference is not more than 2% of the arithmetic mean.
Determination A.6 easily charcoals
A.6.1 Reagents and materials
A.6.1.1 hydrochloric acid solution. lessons hydrochloric acid 24mL, diluted to 1000mL.
A.6.1.2 sulfuric acid solution. c (
2H2SO4
) = 1mol/L.
A.6.1.3 sodium thiosulfate standard titration solution. c (Na2S2O3) = 0.1mol/L.
A.6.1.4 hydrogen peroxide solution. lessons of 30% hydrogen peroxide 10mL, diluted with water to 100mL.
A.6.1.5 sodium hydroxide solution. 300g/L.
A.6.1.6 starch indicator solution. 10g/L.
A.6.1.7 yellow liquid. c (FeCl3 · 6H2O) = 46mg/mL.
Weigh ferric chloride (FeCl3 · 6H2O) 46g, was dissolved in approximately 900mL of hydrochloric acid solution, and then the hydrochloric acid solution was diluted to 1000mL.
When calibration, adjust this yellow liquid with hydrochloric acid solution to 46mg per ml ferric chloride (FeCl3 · 6H2O). Solution should be protected from light protection
Deposit, now with the current calibration.
Calibration. lessons 10mL freshly prepared ferric chloride solution, water was added 15mL, hydrochloric acid and potassium iodide 4g 5mL, immediately stuffed
Dark cap standing 15min, water was added 100mL, iodine with sodium thiosulfate standard titration solution precipitation titration to pale yellow, add starch means
Shown liquid 0.5mL, continue titration to the end.
NOTE. 0.1mol/L sodium thiosulfate standard titration solution equivalent to 27.03mg per ml ferric chloride (FeCl3 · 6H2O).
A.6.1.8 red stock solution. c (CoCl2 · 6H2O) = 59.5mg/mL.
Weigh cobalt chloride (CoCl2 · 6H2O) 60g, was dissolved in approximately 900mL of hydrochloric acid solution, and then the hydrochloric acid solution was diluted to 1000mL.
Adjust this red liquid when calibrated with hydrochloric acid solution to 59.5mg per ml of cobalt chloride (CoCl2 · 6H2O). Solution should be protected from light,
Now with the current calibration.
Calibration. lessons cobalt chloride solution 5.0mL freshly prepared by adding a solution of hydrogen peroxide and sodium hydroxide solution 5mL 10mL, slowly cook
Boiling 10min, cooled. Plus potassium iodide 2g, sulfuric acid solution 60mL, immediately stuffed caps and gently shake to dissolve the precipitate. With thiosulfate
Sodium standard solution titration titration to pale yellow, add starch indicator solution 0.5mL, continue titration to the end point of the solution was pink.
NOTE. 0.1mol/L sodium thiosulfate standard titration solution equivalent to 23.79mg per ml of cobalt chloride (CoCl2 · 6H2O).
A.6.1.9 limit color standard solution. yellow and red liquid stock solution by 9.1 (volume ratio).
A.6.2 Analysis step
Weigh 0.75g sample in 25mL tube with a stopper colorimetric, adding sulfuric acid 10mL, heated at 90 ℃ ± 1 ℃ water bath after 1min fast
Speed shaking uniform heating was continued for 1h at 90 ℃ ± 1 ℃ water bath, remove and quickly cooled with ice water. Slowly into 1cm cuvette for
Water is blank, the absorbance was measured at a wavelength of 500nm at the A; the limit color standard solution slowly into 1cm cuvette, the measured absorbance
Luminosity A1.
A.6.3 Calculation Results
Easy carbide absorbance ratio K said, according to the formula (A.3) Calculated.
K =
A1
(A.3)
Where.
A --- absorbance value of the sample solution;
A1 --- absorbance values of standard solutions.
The test results of the arithmetic mean of the results of parallel determination prevail retain a decimal.
Two independent determination results under the absolute difference between the same condition is not more than 5% of the arithmetic mean.
A.7 Determination of sulfated ash
A.7.1 Method summary
After burning the sample, adding sulfuric acid to convert the residue into sulfates, burning at a high temperature to a constant quality, it can calculate the sample ash sulfuric acid
Value points.
A.7.2 Instruments and Equipment
A.7.2.1 dryer (discoloration silica gel desiccant).
A.7.2.2 high-temperature furnace.
A.7.3 Reagents and materials
sulfuric acid.
A.7.4 Analysis step
Weigh the sample 2g, accurate to 0.0001g, has been placed in a constant mass of quartz or platinum crucible, slowly burn to completely carbonized. Let cool,
Sulfuric acid 0.5mL ~ 1.0mL wetted on the electric heated slowly to sulfuric acid mist after divisible, at 700 ℃ ~ 800 ℃ high temperature furnace
Ignition to completely gray. Removed, placed in a desiccator to cool, weighed, and then at 700 ℃ ~ 800 ℃ ignition until constant mass.
A.7.5 Calculation
Sulfated ash mass fraction w3, according to equation (A.4) Calculated.
w3 =
m1-m0
m × 100%
(A.4)
Where.
After the mass m1 --- burning crucible and ash in grams (g);
m0 --- constant quality crucible after mass, in grams (g);
M --- the quality of the sample, in grams (g).
The test results of the arithmetic mean of the results of parallel determination prevail, 2 decimal places.
Two independent determination results under the absolute difference between the same condition is not more than 0.005%.
Determination of sulfate A.8
A.8.1 Method summary
Under acidic conditions, the citric acid solution sulfate ions and barium chloride solution was precipitated barium sulfate, standard solution with the same treatment of
Comparison, do a limited test.
A.8.2 Reagents and materials
A.8.2.1 hydrochloric acid solution. 6mol/L. Draw hydrochloric acid 54mL, diluted to 100mL.
A.8.2.2 barium chloride solution. 250g/L.
A.8.2.3 acetic acid solution. amount of acetic acid 298mL, diluted to 1000mL.
A.8.2.4 ethanol. the amount of anhydrous ethanol 300mL, diluted with water to 1000mL.
A.8.2.5 sulfate standard stock solution. c (SO4) = 0.1g/L.
A.8.2.6 sulfate standard solution Ⅰ. c (SO4) = 0.01g/L. Draw sulfate standard stock solution 10mL, diluted with ethanol solution to
100mL.
A.8.2.7 sulfate standard solution Ⅱ. c (SO4) = 0.015g/L. Draw sulfate standard stock solution 15mL, diluted with ethanol solution to
100mL.
A.8.3 Analysis step
Weigh the sample 1g, accurate to 0.01g, set 50mL stoppered colorimetric tube, add water 15mL dissolved by adding barium chloride solution 1mL,
Sulfate standard solution 1mL, shaking, standing 1min, adding hydrochloric acid and acetic acid solution 1mL solution 0.5mL, shake, standing 5min.
Draw sulfate standard solution 10mL in 50mL colorimetric tube with stopper, water was added 5mL, from "barium chloride solution is added 1mL" began with
Treated in the same sample. Sample tube turbidity No deeper than the standard pipe.
NOTE. anhydrous citric acid sulfate standard solution Ⅰ; a water citric acid sulfate standard solution Ⅱ.
Determination A.9 chloride
A.9.1 Method summary
Under acidic conditions, the citric acid solution of chloride and silver nitrate solution to form a white precipitate of silver chloride standard solution with the same treatment of
Comparison, do a limited test.
A.9.2 Reagents and materials
A.9.2.1 nitric acid solution. Measure 150mL nitric acid, diluted to 1000mL.
A.9.2.2 silver nitrate solution. c (AgNO3) = 0.1mol/...