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National Food Safety Standard -- Food Additives -- Dimethyl carbonate (also known as Viggo Ling)
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GB 1886.68-2015
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Basic data | Standard ID | GB 1886.68-2015 (GB1886.68-2015) | | Description (Translated English) | National Food Safety Standard -- Food Additives -- Dimethyl carbonate (also known as Viggo Ling) | | Sector / Industry | National Standard | | Classification of Chinese Standard | X40 | | Word Count Estimation | 9,950 | | Date of Issue | 2015-09-22 | | Date of Implementation | 2016-03-22 | | Regulation (derived from) | PRC National Health and Family Planning Commission 2015 No.8 | | Issuing agency(ies) | National Health and Family Planning Commission of the People's Republic of China |
GB 1886.68-2015: National Food Safety Standard -- Food Additives -- Dimethyl carbonate (also known as Viggo Ling) ---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.
(National food safety standards for food additives, dimethyl carbonate (aka Viggo Ling))
National Standards of People's Republic of China
National Food Safety Standard
Food Additives dimethyl carbonate
(Aka Viggo Ling)
Issued on. 2015-09-22
2016-03-22 implementation
People's Republic of China
National Health and Family Planning Commission released
National Food Safety Standard
Food Additives dimethyl carbonate
(Aka Viggo Ling)
1 Scope
This standard applies to methyl chlorine and alkali solution as raw materials in the catalyst, the condensation reaction, separation and purification of the resulting food
Dimethyl carbonate additive.
2 chemical name, molecular formula, relative molecular mass and structural formula
2.1 Chemical Name
Dimethyl carbonate
Formula 2.2
C4H6O5
2.3 formula
2.4 relative molecular mass
134.0874 (according to 2007 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
Under color is colorless transparent liquid
Take appropriate samples were placed in sealed colorless glass container, under natural light, observed
Color
NOTE. The product has a pungent odor, not directly sniffing, fume hood operation need to be.
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
Dimethyl carbonate, w /% ≥ 99.8 Appendix A A.4
Dimethyl carbonate, w /% ≤ 0.2 A.5 Appendix A
Lead (Pb)/(mg/kg) ≤ 2.0 GB 5009.12
Appendix A
Testing method
A.1 Warning
Dimethyl carbonate to the eyes, skin and respiratory system, corrosive, inhalation or ingestion can cause poisoning. Operation should be in a well-ventilated
Under good state, the operator should be good personal protection (such as wearing protective chemical safety glasses, rubber gloves, wear a filter type, if necessary
Poison mask).
A.2 General Provisions
Unless otherwise indicated, used in the analysis only identified as AR and above reagents, laboratory water should be consistent with GB/T 6682 Three
Grade water requirements. Test methods used in the standard titration solution, impurities measured by standard solution, preparations and products, in the absence of other requirements specified
When, according to GB/T 601, the provisions of the preparation of GB/T 602 and GB/T 603's. Solution was used in the tests did not indicate what is formulated with solvent
When, it refers to an aqueous solution.
A.3 Identification Test
A.3.1 solubility
Soluble in toluene, methylene chloride and other organic solvents. Decompose rapidly after dilution in water to produce carbon dioxide and trace amounts of methanol.
A.3.2 IR spectrum
At 1130nm and 1800nm accessory area maximum absorption peak in the infrared spectrum in Appendix B of Figure B.1.
A.4 Determination of dimethyl carbonate
A.4.1 Reagents and materials
A.4.1.1 acetone.
A.4.1.2 dibutylamine dichlorobenzene solution. Weigh dibutylamine 120g, accurate to 0.01g, was dissolved in 1L chlorobenzene.
A.4.1.3 hydrochloric acid standard titration solution. c (HCl) = 1mol/L.
A.4.2 Instruments and Equipment
Potentiometric titrator, Resolution. 1mV or higher.
A.4.3 Analysis step
Weigh 1.0g ~ 1.3g sample, accurate to 0.0001g, has been placed in the addition of about 70mL acetone 150mL beaker, added accurate
20mL dibutylamine dichlorobenzene solution, with stirring, titration with hydrochloric acid standard solution titration, potentiometric titration indicate the end. Meanwhile blank
test.
A.4.4 Calculation Results
Dimethyl carbonate mass fraction w1, according to formula (A.1) Calculated.
w1 =
(V1-V2) × c × M
m × 1000 ×
100% (A.1)
Where.
V1 --- sample consumption hydrochloric acid standard titrant volume in milliliters (mL);
V2 --- blank test volume of consumption hydrochloric acid standard titration solution, in milliliters (mL);
c --- hydrochloric acid standard titration solution concentration, in units of moles per liter (mol/L);
The M --- dimethyl carbonate molar mass in grams per mole (g/mol), [M (C4H6O5) = 134.09];
M --- the quality of the sample, in grams (g);
1000 --- conversion factor.
A.5 Determination of dimethyl carbonate
A.5.1 Reagents and materials
Methyl isobutyl ketone.
A.5.2 Instruments and Equipment
A.5.2.1 gas chromatograph. equipped with a flame ionization detector.
A.5.2.2 injector. with cool on-column injector type, or quartz micro-syringe needle (for manual injection).
A.5.3 Chromatography conditions
Recommended columns and typical operating conditions are shown in Table A.1, approximate retention times of the components shown in Table A.2, dimethyl carbonate content determination
A typical chromatogram Appendix B in Figure B.2. Others can achieve the same degree of separation columns and chromatographic operating conditions can be used.
Table A.1 column chromatography and typical operating conditions
Condition of the item
Column length 50m, column diameter 0.3mm, coated with a capillary column SE30-D
Temperature program
The initial temperature 30 ℃, maintained 5min, to 40 ℃/min heating rate to 120 ℃, final
Temperature. 120 ℃, maintained 5min
The gasification chamber temperature/℃ room temperature (about 25 ℃)
Detector temperature/℃ 200
The carrier gas (helium) before the column pressure/kPa 300
Column flow rate/(mL/min) 2.0
Gas (hydrogen) flow rate/(mL/min) 35
Supporting gas (air) flow rate/(mL/min) 300
Make-up gas flow rate/(mL/min) 28
The injection volume/μL 2
Table A.2 approximate retention times of the components
Ingredient name Approximate retention times/min
Dimethyl carbonate 5.5
Methyl isobutyl ketone 7.2
Dimethyl carbonate 8.8
A.5.4 Analysis step
It weighs about 10g sample, accurate to 0.0001g, placed in a covered bottle. Adding a certain amount of methyl isobutyl ketone, and the expected carbonate
Dimethyl content consistency (about 20mg, accurate to 0.1mg). Seal, mix thoroughly backward like 2μL.
A.5.5 Calculation Results
Dimethyl carbonate mass fraction w2, according to equation (A.2) Calculated.
w2 =
A × m1 × f
A1 × m ×
100% (A.2)
Where.
A --- dimethyl carbonate peak area;
m1 --- methyl isobutyl ketone mass, in milligrams (mg);
f --- correction coefficient dimethyl carbonate, the same mass of methyl isobutyl ketone and dimethyl carbonate (eg. each 20mg, accurate to
0.1mg), was added to a certain amount of dimethyl carbonate (eg. 10.0g), mix well, injection 2μL, gas chromatography
Fixed, methyl isobutyl ketone and dimethyl carbonate ratio of peak area, dimethyl carbonate is a correction coefficient;
A1 --- methyl isobutyl ketone peak area;
M --- the quality of the sample, in milligrams (mg).
Appendix B
Dimethyl carbonate and dimethyl carbonate IR spectra measured chromatograms
B.1 dimethyl carbonate IR spectrum
Dimethyl carbonate in the infrared spectrum shown in Figure B.1. Sample purity of 99.9%, directly on the sample in the optical system of the sample window, select
Reflective mode test the resulting spectra.
Figure B.1 dimethyl carbonate in the infrared spectrum
B.2 dimethyl carbonate measured chromatogram
Dimethyl carbonate measured chromatogram shown in Figure B.2.
Figure B.2 dimethyl carbonate measured chromatogram
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