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National Food Safety Standard -- Food Additives -- Petroleum ether
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GB 1886.59-2015
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Basic data | Standard ID | GB 1886.59-2015 (GB1886.59-2015) | | Description (Translated English) | National Food Safety Standard -- Food Additives -- Petroleum ether | | Sector / Industry | National Standard | | Classification of Chinese Standard | X40 | | Word Count Estimation | 9,940 | | 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 1886.59-2015: National Food Safety Standard -- Food Additives -- Petroleum ether---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 petroleum ether)
National Standards of People's Republic of China
National Food Safety Standard
Food additives petroleum ether
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 petroleum ether
1 Scope
This standard applies to natural petroleum fractions prepared food additive petroleum ether. The product is at a boiling point between 25 ℃ ~ 105 ℃ of
Light petroleum products, mainly for mixed alkanes (n homogeneous and heterogeneous) and naphthenes.
2 Technical Requirements
2.1 Sensory requirements
Sensory requirements shall comply with the requirements of Table 1.
Table 1 Sensory requirements
Project requires test methods
Color colorless
Transparent liquid state
Odor similar to the smell of gasoline
Take appropriate sample in a clean, dry colorimetric tube, in natural light
By visually observe its color and status, olfactory odor
2.2 Physical indicators
Physical and chemical indicators should be consistent with the provisions of Table 2.
Table 2. Physical and chemical indicators
Item Index Test Method
Evaporation residue/(mg/100mL) ≤ 2 GB/T 6324.2
S/(mg/kg) ≤ 10 GB/T 6324.4
Benzene, φ /% ≤ 0.05 Appendix A A.4
Aromatic hydrocarbons (benzene), φ /% ≤ 0.3 Appendix A A.4
Bromine index/(mg/100g) ≤ 200 Appendix A A.5
Lead (Pb)/(mg/kg) ≤ 2.0 GB 5009.12
PAHs test by GB 7363
Appendix A
Testing method
A.1 Warning
Some test procedures prescribed test method can lead to dangerous situations. The operator shall take appropriate safety and health practices.
A.2 General Provisions
Unless otherwise indicated in the analysis using only recognized as analytical reagents and GB/T 6682 stipulated three water. Test Methods
The standard titration solution, impurity measurement standard solution, preparations and products, did not indicate when the other requirements, according to GB/T 601, GB/T 602
Preparation and provisions GB/T 603; and the solution, unless otherwise indicated, are the solution.
A.3 Identification Test
Insoluble in water, soluble in ethanol.
A.4 benzene and aromatics (benzene) Determination
A.4.1 Method summary
By gas chromatography under the selected chromatographic conditions, sample after vaporization separated by capillary column with flame ionization detector
Detection with internal standard.
A.4.2 Reagents and materials
A.4.2.1 Hydrogen. the volume fraction of not less than 99.99%, silica gel and molecular sieves, purified.
A.4.2.2 nitrogen. the volume fraction of not less than 99.99%, silica gel and molecular sieves, purified.
A.4.2.3 Air. silica gel and molecular sieves, purified.
A.4.2.4 isooctane. ≥99%, aromatic substance containing less than 0.05%.
A.4.2.5 internal standard. n- decane and n- undecane, chromatography; or n- decane and n- dodecane, chromatography.
A.4.2.6 standard solution A. 0.5% of the internal standard solution and 0.5% iso-octane benzene.
A.4.2.7 Standard solution B. 0.5% of n- decane, 0.5% of the internal standard solution and 0.5% iso-octane benzene.
A.4.3 Instruments and Equipment
A.4.3.1 Gas chromatograph. with a capillary column injector device and a flame ionization detector.
A.4.3.2 micro syringe. 10μL.
A.4.4 columns and operating conditions
The recommended standard chromatographic columns and the operating conditions are shown in Table A.1, n- decane can before the same degree of separation of the benzene peak column
And chromatographic operating conditions can also be used.
Table A.1 Recommended chromatographic columns and operating conditions
Project Parameters
Column pentaerythritol -β- cyanide ether capillary column
Column length 30m × 0.25mm × column diameter
Column temperature/℃ 95
Vaporization chamber temperature/℃ 275
Detector temperature/℃ 250
Carrier gas (nitrogen) flow rate/(mL/min) 3
Split ratio 100.1
Injection volume/μL 10
Determination of the internal standard response factor with respect to benzene A.4.5
Benzene with respect to the internal standard response factor to f expressed by the formula (A.1) Calculated.
f =
A1 × w
w1 × A
(A.1)
Where.
A1 --- internal standard peak area;
w --- A standard solution mass fraction of benzene;
W1 --- quality within the standard solution A standard material fraction;
A --- benzene peak area.
A.4.6 Analysis step
Approximately 0.1mL internal standard into a 25mL volumetric flask, using analytical balance. With the test sample was dissolved and diluted to the mark. press
Table A.1 given operating conditions inject 10μL sample containing internal standard. Before measuring the internal standard peak area and benzene, change the instrument failure
Save to ensure that the peak of the peak of at least 25% of full scale. Measurement and benzene internal standard peak area. Paul and typical chromatograms of the components
The residence time in Appendix B in Figure B.1 and Table B.1.
A.4.7 Quantitative Analysis
Using internal standard.
A.4.8 Calculation Results
The mass fraction of a measured component wi, according to equation (A.2) Calculated.
wi =
Ai × f × m1
A2 × m ×
100% (A.2)
Where.
Ai --- a peak area of component being tested;
f --- benzene with respect to the response factor of the internal standard;
m1 --- added mass of the internal standard in grams (g);
A2 --- internal standard peak area;
M --- the quality of the sample, in grams (g).
A.5 Determination of bromine index
A.5.1 Method summary
Aware of the large number of sample was dissolved by the standard bromide - bromate special solution titrate in. When there is the presence of free chlorine, causing the system
A sudden change in conductivity, potentiometric titrator indicate the end. Bromine index refers 100g sample occurred under the test conditions of the reaction mass of bromine
, And the unit of mg/100g.
A.5.2 Reagents and materials
A.5.2.1 mixed solvent. A 714mL glacial acetic acid, 134mL of carbon tetrachloride, 134mL of methanol and 18mL of sulfuric acid (15) were mixed.
A.5.2.2 sodium thiosulfate standard titration solution. c (Na2S2O3) = 0.05mol/L.
A.5.2.3 bromide - potassium bromate standard solution. c (
6KBr-KBrO3
) = 0.05mol/L. Weigh 5.1g 1.4g potassium bromide and potassium bromate,
Diluted with water to 1000mL. 1mL to 50mL glacial acetic acid and hydrochloric acid test solution was added to 500mL iodine bottle. Cooled in an ice-water bath
Possession of about 10min, and spinning iodine bottle, add 40mL ~ 50mL (accurate to 0.01mL) of bromide from 50mL burette -
Bromate solution, speed control between 90s ~ 120s. Quickly covered with caps, mix a solution, and this placed in an ice water bath. In the iodine bottle
The bottle plus 5.0mL15% potassium iodide solution. 5min after iodine bottle was removed from the ice water bath and remove the stopper, so that 15% of the iodide
Potassium iodine solution is slowly flowing into the bottle. Mix well with clean water 100mL cork, bottle and the bottle wall, and immediately with sulfur 0.05mol/L of
Sodium thiosulfate standard solution titration, near the end added starch test solution slowly titrated to a blue color disappears, is the end.
Potassium bromide - potassium bromate standard solution concentration c1, according to formula (A.3) Calculated.
c1 =
V2 × c2
V1
(A.3)
Where.
V2 --- consumption volume of sodium thiosulfate standard titration solution, in milliliters (mL);
Concentration c2 --- sodium thiosulfate standard titration solution, expressed in moles per liter (mol/L);
V1 --- added potassium bromide - potassium bromate standard solution volume, in milliliters (mL).
A.5.3 Instruments and Equipment
A.5.3.1 titrator.
A.5.3.2 titration vessel. capacity of about 150mL, and can be maintained with a glass casing 1 ℃ ~ 5 ℃ condensation plant. Two platinum electrodes
Place the distance is not greater than 5mm, and depth below the liquid level. Mechanical or magnetic stirrer, and stirred sufficiently not cause the bubbles.
A.5.3.3 dropper. capacity of 10mL and 50mL.
A.5.3.4 iodine bottle. with a glass stopper, capacity 500mL.
A.5.4 Analysis step
With a suitable cooling fluid through the casing titration vessel, circulating cooling titration vessel maintained at 1 ℃ ~ 5 ℃. The mixture was added 110mL
Co-solvent (A.5.2.1) and a sample of 8g ~ 10g. Open stirrer, stirring rate adjusted to the solution, but not from the whirlpool bubbles appropriate.
The vessel was cooled to 0 ℃ ~ 5 ℃, and the temperature was maintained during the titration. With 10mL burette slowly added in small amounts of potassium bromide - potassium bromate
Solution, until near the end of the detector display. 71/92 0.1mL potassium bromide - potassium bromate solution until a stable end point detector
(End holding 30s). Blank test, was added potassium bromide - potassium bromate solution should be less than 0.1mL.
A.5.5 Calculation Results
W bromine index bromine, the reaction mass under specified conditions with bromine 100g sample, the unit is milligram per hundred grams (mg/100g), press
Formula (A.4) Calculated.
w = bromine
(V3-V4) × c × M × 100
(A.4)
Where.
V3 --- sample consumption of potassium bromide - potassium bromate standard titration solution volume in milliliters (mL);
V4 --- blank test consumption of potassium bromide - potassium bromate standard titration solution volume in milliliters (mL);
c --- Potassium bromide - potassium bromate standard titration solution concentration, expressed in moles per liter (mol/L);
Molar mass M --- elemental bromine, in units of grams per mole (g/mol), [M (Br) = 79.9];
100 --- conversion factor;
M --- the quality of the sample, in grams (g).
Appendix B
Retention time typical chromatograms benzene and aromatics content and determination of the components
Typical chromatograms B.1 benzene and aromatics content determination
Typical chromatograms of benzene and aromatics content determination Figure B.1.
Explanation.
1 --- petroleum ether;
2 --- benzene;
3 --- n- decane;
4 --- toluene;
5 --- n- undecane;
6 --- ethylbenzene;
7 --- p-xylene;
8 --- xylene;
. 9 --- o-xylene.
A typical chromatogram Figure B.1 benzene and aromatics content determination
Typical chromatograms B.2 benzene and aromatics content determination of the retention time of each component
Typical chromatograms of benzene and aromatics content determination of the retention time of the components shown in Table B.1.
A typical chromatogram Table B.1 benzene and aromatics content determination of the retention time of each component
Ingredient name Retention time/min
Benzene 6.1
Toluene 7.0
Ethylbenzene 8.0
Table B.1 (continued)
Ingredient name Retention time/min
8.5 m-xylene and p-xylene
Ortho-xylene 10.0
n- dodecane 6.5
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