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Food additive -- Brilliant blue
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GB 1886.217-2016
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Basic data | Standard ID | GB 1886.217-2016 (GB1886.217-2016) | | Description (Translated English) | Food additive -- Brilliant blue | | Sector / Industry | National Standard | | Classification of Chinese Standard | X42 | | Word Count Estimation | 15,180 | | Date of Issue | 2016-08-31 | | Date of Implementation | 2017-01-01 | | Older Standard (superseded by this standard) | GB 7655.1-2005 | | Regulation (derived from) | Announcement of the State Administration of Public Health and Family Planning 2016 No.11 | | Issuing agency(ies) | National Health and Family Planning Commission of the People's Republic of China, State Food and Drug Administration |
GB 1886.217-2016: Food additive -- Brilliant blue---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 safety national standard - Food additive - Bright blue)
National Standards of People's Republic of China
National Food Safety Standard
Food Additives bright blue
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 7655.1-2005 "Food Additives bright blue."
This standard compared with GB 7655.1-2005, the main changes are as follows.
--- Standard name was changed to "national food safety standards for food additives bright blue";
--- Increasing the chemical name;
--- Index name Appearance modify sensory requirements, modify the index requirements;
--- Loss on drying and chloride (based on NaCl) and sulfate (Na2SO4 to count) aggregates merger;
--- Heavy Metals (as Pb) Index name changed to lead, to modify the test method;
--- Revised test methods for arsenic;
--- Modify the dissolution test test.
National Food Safety Standard
Food Additives bright blue
1 Scope
This standard applies to benzaldehyde and N- ethyl-o-sulfonic acid -N- (3- sulfo benzyl) - aniline by condensation, oxidation obtained food additives
PPD bright blue.
2 chemical name, molecular formula, molecular mass and structural formula
2.1 Chemical Name
3- [N- Ethyl -N- [4 - [[4- [N- Ethyl -N- (3- sulfo-benzyl) - amino] phenyl] (2-sulfophenyl) methylene ] -2,5-cyclohexadiene
Yl-1-ylidene] aminomethyl] - benzenesulfonic acid disodium salt
Formula 2.2
C37H34N2Na2O9S3
2.3 formula
2.4 relative molecular mass
792.85 (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
Color purple to blue-violet
The state of a powder or granules
Take the right amount of sample is placed in a clean, dry white porcelain dish, self
Under natural light, 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
Item Index Test Method
Bright blue content, w /% ≥ 85.0 Appendix A A.4
Loss on drying, chloride (based on NaCl) and sulfate (Na2SO4 to count)
Total, w /% ≤
14.0 Appendix A A.5
Water-insoluble, w /% ≤ 0.20 A.6 in Appendix A
Deputy dye, w /% ≤ 6.0 Appendix A A.7
Arsenic (As)/(mg/kg) ≤ 1.0 GB 5009.11 or GB 5009.76
Lead (Pb)/(mg/kg) ≤ 10.0 GB 5009.12 or GB 5009.75
Manganese a (Mn)/(mg/kg) ≤ 50.0 GB/T 5009.90
Chromium b (Cr)/(mg/kg) ≤ 50.0 GB 5009.123
a manganese method process control projects.
b chromium law process control projects.
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
This standard reagents and water in the absence of other specified requirements, refer to the three water analytical reagent and GB/T 6682 regulations. Test
The standard solution, standard solution for measuring impurities, formulations and products, did not indicate when the other requirements according to GB/T 601, GB/T 602,
GB/T 603 provisions of the preparation. 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
Ammonium acetate solution. 1.5g/L.
A.3.2 Instruments and Equipment
A.3.2.1 Spectrophotometer.
A.3.2.2 cuvette. 10mm.
A.3.3 Identification method
A.3.3.1 dissolution test
Weigh about 0.1g sample (accurate to 0.01g), was dissolved in 100mL of water, a clear solution was blue.
A.3.3.2 Test absorbance
Weigh about 0.1g sample (accurate to 0.01g), was dissolved in 100mL ammonium acetate solution of this solution 1mL, plus ammonium acetate solution equipped to
200mL, the maximum absorption wavelength of this solution is 628nm ~ 632nm.
Note. The measured absorbance value should be 0.3 to 0.7, otherwise adjust the concentration of the sample.
A.4 Determination of bright blue Content
A.4.1 Titanium trichloride titration (Arbitration Act)
A.4.1.1 Method summary
In acidic medium, light blue is titanium trichloride reductive decomposition, according to the consumption of titanium trichloride standard titration solution, calculate its content.
A.4.1.2 Reagents and materials
A.4.1.2.1 sodium bitartrate.
A.4.1.2.2 titanium trichloride standard titration solution. c (TiCl3) = 0.1mol/L (now with the existing, method of preparation see Appendix B).
A.4.1.2.3 Carbon dioxide. content ≥99%.
A.4.1.3 instruments and equipment
Titanium trichloride titration apparatus shown in Figure A.1.
Explanation.
A --- conical flask (a 500 mL);
B --- brown burette (50mL);
C --- package under glass bottle of black paper (2000mL);
D --- containing ferrous sulfate and ammonium carbonate equivalent mixture container (5000mL);
E --- piston;
F --- bottles;
G --- washing bottle filled with water.
Figure A.1 apparatus of FIG titanium trichloride titration
A.4.1.4 analysis step
Weigh about 1g sample (accurate to 0.0001g), placed in 500mL conical flask, dissolved in 50mL freshly boiled and cooled to room temperature, water
, And after adding 15g of sodium hydrogen tartrate and 150mL of freshly boiled water, dissolved by shaking, according to Figure A.1 instrument installed at the surface through dioxide
While carbon, heated to boiling, and treated with titanium trichloride standard titration solution to titrate the sample solution inherent color disappears as the end point.
A.4.1.5 Calculation Results
Bright blue content of the mass fraction w1, according to equation (A.1) Calculated.
w1 =
V × c × M
m × 1000 × 2 ×
100% (A.1)
Where.
Volume V --- titrate the sample consumed titanium trichloride standard titration solution, in milliliters (mL);
C --- concentration of titanium trichloride standard titration solution, expressed in moles per liter (mol/L);
--- The M molar mass of brilliant blue, in units of grams per mole (g/mol) [M (C37H34N2Na2O9S3) = 792.85];
M --- the quality of the sample, in grams (g);
1000 --- volume conversion factor;
2 --- molar conversion coefficient.
The results parallel arithmetic mean of the measurement results shall prevail (reserved a decimal). In two independent test repeated conditions
Given absolute difference is not more than the arithmetic mean of 1.0%.
A.4.2 Colorimetric method
A.4.2.1 Method summary
After dissolving each sample with a known water content in bright blue reference, at the maximum absorption wavelength, were measured absorbance, then calculate
Its content.
A.4.2.2 Reagents and materials
A.4.2.2.1 ammonium acetate solution. 1.5g/L.
A.4.2.2.2 bright blue Reference Sample. Content ≥85.0% (measured according to A.4.1).
A.4.2.3 instruments and equipment
A.4.2.3.1 spectrophotometer.
A.4.2.3.2 cuvette. 10mm.
Preparation A.4.2.4 brilliant blue of the reference solution
Weigh about 0.25g bright blue standard (accurate to 0.0001g), was dissolved in an appropriate amount of water, transferred to 1000mL volumetric flask, diluted with water
To the mark. Imbibe 5mL, transferred to 500mL volumetric flask, add ammonium acetate solution was diluted to the mark, shake, spare (maximum
Absorbance at a wavelength of absorption should be 0.3 to 0.7).
Preparation A.4.2.5 brilliant blue of the sample solution
Weighing and preparation methods of operation with the bright blue of the reference solution.
A.4.2.6 analysis step
The reference solution and the brilliant blue light blue sample solution were placed in 10mm cuvettes, with the maximum absorption wavelength using a spectrophotometer
Determination of the respective absorbance ammonium acetate solution as reference solution.
A.4.2.7 Calculation Results
Bright blue content of the mass fraction w1, according to equation (A.2) Calculated.
w1 =
A1 × m0
A0 × m1 ×
w0 × 100% (A.2)
Where.
A1 --- absorbance of the sample solution;
m0 --- bright blue reference mass, expressed in grams (g);
A0 --- blue light absorbance of the reference solution;
M1 --- the quality of the sample, in grams (g);
w0 --- bright blue reference mass fraction of (measured according to A.4.1),%.
The results parallel arithmetic mean of the measurement results shall prevail (reserved a decimal). In two independent test repeated conditions
Given absolute difference is not more than the arithmetic mean of 1.0%.
A.5 Determination of loss on drying, chloride (based on NaCl) and sulfate (Na2SO4 in dollars) of the total
A.5.1 Determination of loss on drying
A.5.1.1 Method summary
Sample is placed in a weighing bottle and dried in the electric oven to constant mass after weighing the material after drying.
A.5.1.2 instruments and equipment
Ovens.
A.5.1.3 analysis step
Weigh about 2g sample (accurate to 0.0001g), has placed constant at 135 ℃ ± 2 ℃ constant temperature oven φ (30 ~ 40) mm, said
Flask, at 135 ℃ ± 2 ℃ constant temperature oven drying to constant weight.
A.5.1.4 Calculation Results
Loss on drying mass fraction w2, according to equation (A.3) Calculated.
w2 =
m2-m3
m4 ×
100% (A.3)
Where.
M2 --- sample mass before drying and weighing bottles in grams (g);
m3 --- After drying to constant mass and weighing the sample bottles in grams (g);
m4 --- sample mass, in grams (g).
The results parallel arithmetic mean of the measurement results shall prevail (reserved a decimal). In two independent test repeated conditions
Given absolute difference is not more than 0.2% of the arithmetic mean.
A.5.2 chloride (as NaCl) Determination
A.5.2.1 Method summary
An acidic medium a known amount of silver nitrate solution, the chlorine ion as silver chloride precipitate, ferric ammonium sulfate solution was then added as a
Indicator, the use of ammonium thiocyanate standard titration solution titrate the excess silver nitrate.
A.5.2.2 Reagents and materials
A.5.2.2.1 nitrobenzene.
A.5.2.2.2 nitric acid solution. 11.
A.5.2.2.3 silver nitrate solution. c (AgNO3) = 0.1mol/L.
A.5.2.2.4 ammonium ferric sulfate solution. Weigh 14g of ammonium ferric sulfate, dissolved in 100mL of water, filter, add 10mL of nitric acid, stored in brown
Bottle.
A.5.2.2.5 ammonium thiocyanate standard titration solution. c (NH4SCN) = 0.1mol/L.
A.5.2.2.6 carbon. 767 needle.
A.5.2.3 preparation of the sample solution
Weigh about 2g sample (accurate to 0.0001g), was dissolved in 150mL of water, add about 15g of activated carbon, a moderate boil 2min ~ 3min.
Cooled to room temperature, a solution of nitric acid was added 1mL, continue to shake evenly placed 30min (from time to time during the swing). Filtered through a dry filter paper. Such as
The filtrate was colored, then coupled with activated carbon 5g, placed 60min (during shaking from time to time), and then dried filter paper (such as color still replace the activated carbon
Repeat until the filtrate was colorless). 10mL each wash with water three times activated carbon, and the filtrate combined move 200mL volumetric flask, add water to the mark,
Shake well. For the determination of chloride and sulfate content.
A.5.2.4 analysis step
Pipette 50mL sample solution, placed in 500mL conical flask, add 10mL 2mL nitric acid solution and silver nitrate solution (chloride more
May be appropriate to pay more) and 5mL nitrobenzene, shake vigorously to unite silver chloride, ferric ammonium sulfate is added 1mL solution, with drops of ammonium thiocyanate standard
Given titrate the excess silver nitrate to the end and keep 1min, at the same time in the same way blank test.
A.5.2.5 Calculation Results
Chloride (as NaCl) mass fraction w3, according to equation (A.4) Calculated.
w3 =
V1 (-V0) × c1 × M1
m5 × 1000 ×
× 100% (A.4)
Where.
V1 --- blank titration solution consumed volume of ammonium thiocyanate standard titration solution, in milliliters (mL);
V0 --- titration sample consumption volume of ammonium thiocyanate standard titration solution, in milliliters (mL);
c1 --- ammonium thiocyanate standard titration solution concentration, in units of moles per liter (mol/L);
--- Ml molar mass of sodium chloride, in units of grams per mole (g/mol) [M (NaCl) = 58.4];
M5 --- the quality of the sample, in grams (g);
1000 --- volume conversion factor;
Volume 50 --- Pipette sample solution, in milliliters (mL);
200 --- dose volume of sample solution, in milliliters (mL).
The results parallel arithmetic mean of the measurement results shall prevail (reserved a decimal). In two independent test repeated conditions
Given the absolute difference between the results of not more than 0.3% of the arithmetic mean.
A.5.3 Sulfate (Na2SO4 meter) measurement
A.5.3.1 Method summary
The sample solution of barium chloride standard titration solution, barium sulfate ion to form sulfate precipitation, with rose red indicator solution of sodium as an external means
It shows agents used to determine the titration end point.
A.5.3.2 Reagents and materials
A.5.3.2.1 sodium hydroxide solution. 0.2g/L.
A.5.3.2.2 hydrochloric acid solution. 11999.
A.5.3.2.3 barium chloride standard titration solution. c (
2BaCl2
) = 0.1mol/L. (Preparation see Appendix C).
A.5.3.2.4 phenolphthalein indicator solution. 10g/L.
A.5.3.2.5 Rose sodium indicator solution. Weigh 0.1g of sodium red roses, was dissolved in 10mL of water (using now).
A.5.3.3 analysis step
Draw 25mL sample solution (A.5.2.3), placed in 250mL conical flask, add 1 drop of phenolphthalein indicator solution, sodium hydroxide solution was added dropwise
Pink, then a solution of hydrochloric acid solution to the pink color disappeared, shake, titrated with barium chloride standard titration solution is constantly shaking dissolved, with rose
Rose red indicator solution of sodium for outward indicator solution, and the reaction liquid indicator solution on filter paper presents the intersection of rose red spots and kept 2min does not fade
As the end point.
At the same time in the same manner as a blank test.
A.5.3.4 Calculation Results
Sulfate (Na2SO4 meter) mass fraction w4, according to equation (A.5) Calculated.
w4 =
V3-V2 () × c2 × M2
m6 × 1000 × 2 ×
× 100% (A.5)
Where.
Volume V3 --- titration solution consumed barium chloride standard titration solution, in milliliters (mL);
V2 --- blank titration solution consumed volume of barium chloride standard titration solution, in milliliters (mL);
c2 --- barium chloride standard titration solution concentration, in units of moles per liter (mol/L);
Molar mass of the M2 --- sodium sulfate, units of grams per mole (g/mol) [M (Na2SO4) = 142];
M6 --- the quality of the sample, in grams (g);
1000 --- conversion factor;
2 --- molar conversion factor;
Volume 25 --- pipetting the sample solution, in milliliters (mL);
200 --- dose volume of sample solution, in milliliters (mL).
The results parallel arithmetic mean of the measurement results shall prevail (reserved a decimal). In two independent test repeated conditions
Given absolute difference is not more than 0.2% of the arithmetic mean.
Results A.5.4 Loss on drying, chloride (based on NaCl) and sulfate (Na2SO4 in dollars) the total amount of calculation
Loss on drying, chloride (based on NaCl) and sulfate (Na2SO4 in dollars) of the total mass fraction w5, according to equation (A.6) Calculated.
w5 = w2 w3 w4 (A.6)
Where.
w2 --- Loss on drying mass fraction,%;
w3 --- chloride (as NaCl) mass fraction,%;
w4 --- Sulfate (Na2SO4 meter) mass fraction,%.
Reserved a decimal calculations.
A.6 Determination of insoluble matter
A.6.1 Method summary
After the sample was dissolved filtration, placed in a thermostatic oven dried to constant mass after weighing the insoluble material.
A.6.2 Instruments and Equipment
A.6.2.1 crucible glass frit (G4). a pore size of 5μm ~ 15μm.
A.6.2.2 oven thermostat.
A.6.3 Analysis step
Weigh about 3g sample (accurate to 0.001g), placed in 500mL beaker, add 50 ℃ ~ 60 ℃ water 250mL, dissolved,
(G4) filter has been used in 135 ℃ ± 2 ℃ drying to constant sand core glass crucible and washed thoroughly with hot water to the washing liquid colorless, ± at 135 ℃
2 ℃ constant temperature oven drying to constant weight.
A.6.4 Calculation Results
The mass fraction of water-insoluble w6, according to equation (A.7) calculated as follows.
w6 =
m7-m8
m9 ×
100% (A.7)
Where.
m7 --- After drying quality water insoluble and glass sand core crucible in grams (g);
M8 --- quality glass sand core crucible in grams (g);
m9 --- sample mass, in grams (g).
The results parallel arithmetic mean of the measurement results shall prevail (2 decimal places). In two independent test repeated conditions
Given absolute difference is not more than 0.2% of the arithmetic mean.
Determination A.7 deputy dye
A.7.1 Method summary
The components are separated by paper chromatography, eluted and quantified by spectrophotometry.
A.7.2 Reagents and materials
A.7.2.1 ethanol.
A.7.2.2 n-butanol.
Acetone solution A.7.2.3. 1 1.
A.7.2.4 ammonia solution. 496.
A.7.2.5 sodium bicarbonate solution. 4g/L.
A.7.3 Instruments and Equipment
A.7.3.1 Spectrophotometer.
A.7.3.2 chromatography filter paper. No. 1 in speed, 150mm × 250mm.
A.7.3.3 chromatography tank. φ240mm × 300mm.
A.7.3.4 micro injector. 100μL.
A.7.3.5 Nessler colorimetric tube. 50mL glass grinding mouth stopper.
A.7.3.6 glass frit funnel (G3). a pore diameter of 15μm ~ 40μm.
A.7.3.7 50mm cuvette.
A.7.3.8 10mm cuvette.
A.7.4 Analysis step
A.7.4.1 paper chromatographic conditions
A.7.4.1.1 developing solvent. n-butanol ethanol solution of aqueous ammonia = 623.
A.7.4.1.2 Temperature. 20 ℃ ~ 25 ℃.
A.7.4.2 preparation of the sample solution
Weigh about 1g sample (accurate to 0.001g), placed in a beaker, adding the right amount of water dissolved and transferred to 100mL volumetric flask, dilute to
Scale, shake up the concentration of the sample solution is 1%.
A.7.4.3 wash out the sample preparation liquid
With micro-injector draw 100μL sample solution evenly note on the bottom edge of the filter paper from a baseline of 25mm, a straight line, so that
On filter paper width is not more than 5mm, length 130mm, with a hair dryer. The filter paper containing preformulated good developer
Expand the chromatography tank, filter paper dipped under the bottom edge of the agent level 10mm, to be solvent front line rose to 150mm or until the dye deputy
Separation satisfied. Remove the filter paper chromatography, with cold dry.
Blank filter paper under the same conditions to expand the blank paper and the above steps should be expanded with the adjacent portion of the filter paper on the same piece of filter paper
Clipping.
Deputy dye paper chromatography is shown in Figure A.2.
Figure A.2 deputy dye paper chromatography schematic
After each sub-dye made and will start on a blank paper to each subsidiary colors corresponding parts of the paper in the same size cut, and
Cut into thin strips about 5mm × 15mm, and were placed in 50mL of Nessler colorimetric tube, accurately added to the acetone solution 5mL, shake 3min ~
5min, then the exact solution of sodium bicarbonate was added 20mL, shake well, and then were in the glass frit funnel (G3) in natural filtration, filtration
Liquid should be clarified without suspension. Respectively each subsidiary colors and blank eluate. Deputy dye in their maximum absorption wavelength, with
50mm cuvette, wash the dye out of each sub-liquid measuring their absorbance on a spectrophotometer.
When the absorbance was measured on a spectrophotometer, with a mixture of 5mL and 20mL acetone solution of sodium bicarbonate solution as a reference solution.
A.7.4.4 preparation of standard solution
2mL1% of the sample solution is transferred to absorb 100mL volumetric flask, dilute to the mark, shake, and the solution as the standard solution.
A.7.4.5 Preparation of standard eluate
With micro-injector draw 100μL standard solution, uniform injection site on the bottom edge of the filter paper from a baseline of 25mm with a hair dryer blowing
dry. The filter paper containing previously prepared well eluent chromatography tank to expand, to be solvent front line up 40mm, remove with cold wind
Dry, cut out all the dye partially deployed, according to A.7.4.3 operating procedure, the standard eluate. 10mm cuvette with maximum suction
Absorbance was measured at a wavelength of income.
Meanwhile blank filter paper under the same conditions to start operating in the same manner after the measured absorbance white wash liquid.
A.7.4.6 Calculation Results
Mass fraction deputy dye w7, according to equation (A.8) Calculated.
w7 =
Σ An-bn ()
As-bs () ×
× w1 × 100% (A.8)
Where.
An --- each sub-dye eluate 50mm optical path length measured absorbance;
bn --- dye control each sub-blank eluate 50mm optical path length measured absorbance;
As --- Standard eluate 10mm path length measured absorbance;
bs --- standard control blank eluate 10mm path length measured absorbance;
5 --- converted into multiples of 10mm optical path length;
--- Standard eluate converted into multiples of one percent of the sample solution;
Mass fraction w1 --- sample,%.
The results parallel arithmetic mean of the measurement results shall prevail (reserved a decimal). In two independent test repeated conditions
Given absolute difference is not more than 0.2% of the arithmetic mean.
Appendix B
The method of preparation of titanium trichloride standard titration solution
B.1 Reagents and materials
B.1.1 hydrochloric acid.
B.1.2 ferrous ammonium sulfate.
B.1.3 ammonium thiocyanate solution.200g/L.
B.1.4 sulfuric acid solution. 11.
B.1.5 titanium trichloride solution.
B.1.6 potassium dichromate standard titration solution. c (
6K2Cr2O7
) = 0.1mol/L.
B.2 instruments and equipment
Titration apparatus is shown in Figur...
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