Some standard content:
Chemical Industry Standard of the People's Republic of China
HG/T2662—95
Industrial 1,2-dichloroethane
Published on March 6, 1995
Ministry of Chemical Industry of the People's Republic of China
Implementation on June 1, 1996
W2
Chemical Industry Standard of the People's Republic of China
Industrial 1,2-dichloroethane
Subject content and scope of application
HG/T2662—-95
Replaces HG/T2—1438—81
This standard specifies the technical requirements, test methods, inspection rules, marking, packaging, transportation and storage of industrial 1,2-dichloroethane. Molecular formula: C, H, Cl2
Relative molecular mass: 98.96 (according to the international relative atomic mass in 1991) Reference standards
Dangerous goods packaging mark
GB/T601
GB/T603
GB/T1250
GB/T2366
GB/T3143
GB/T3723
GB/T4472||t t||GB/T6678
GB/T6680
3 Technical requirements
Preparation of standard solutions for titration analysis (volumetric analysis) of chemical reagents Preparation of preparations and products used in test methods for chemical reagents Methods of expressing and judging limit values Determination of water content in chemical products Gas chromatography Color determination of liquid chemical products (Hazen-General safety rules for sampling of industrial chemical products General rules for determination of density and relative density of chemical products General rules for sampling of chemical products
General rules for sampling of liquid chemical products
3.1 Appearance: transparent liquid, free of suspended matter. 3.2 The quality of industrial 1,2-dichloroethane shall meet the requirements of the following table: Item
Content, %
Density (pao), 8/cm
Water, %
Colour, Hazen unit (platinum-cobalt colour number) Acidity (in HCI), %
Ministry of Chemical Industry of the People's Republic of China 1995 -03-06 approved platinum-cobalt color number)
1.253~1.256
Qualified products
1.2501.257
1996-06-01 implementation
W.bzsoso:com4 test method
HG/T2662-95
The reagents and water used in this standard, unless otherwise specified, are analytical reagents and distilled water, or water of equal purity. The standard solutions and products used in this standard are prepared in accordance with the provisions of GB/T601 and GB/T603 unless otherwise specified. The instruments are general laboratory instruments.
4.1 Determination of content
4.1.1 Summary of method
Use gas chromatography and internal standard method to determine the impurity content in 1,2-dichloroethane, and then subtract the total amount of all impurities and water from 100 to obtain the content of 1,2-dichloroethane, expressed as mass percentage. 4.1.2 Reagents and materials
Internal standard: benzene, dodecane, purity should be greater than 99.0%; impurity standard sample: purity greater than 99.0%;
Nitrogen: purity greater than 99.99%
Hydrogen: purity greater than 99.99%;
Air: fully dried and purified by silica gel and molecular sieve; dichloroethane.
4.1.3 Instruments and Equipment
4.1.3.1 The gas chromatograph shall be equipped with a hydrogen flame ionization detector. Under the condition that the injection volume does not exceed the permissible load of the chromatographic column, the peak height of the impurity tested with a final outflow content of 10 mg/kg shall be at least 5 times greater than the instrument noise. 4.1.3.2 Recording system: a recorder with a full scale equal to or less than 2 mV or a suitable chromatographic data processor of various types. 4.1.3.3 Micro syringe: 10μL, 50μL; 4.1.3.4 Chromatographic column
Column 1: stainless steel tube with inner diameter of 3mm and length of 3m; Column 2: stainless steel tube with inner diameter of 3mm and length of 1m; a.
Fixed liquid: polyethylene glycol 1500;
Carrier: acid-washed silanized chromium MSA 0.18~0.25mm (60~80 mesh); c.
Filling material ratio:
Column 1 carrier: fixed liquid = 100:12;
Column 2 carrier fixed liquid = 100:3.
4.1.3.5 Preparation of stationary phase and aging of columns a Preparation of stationary phase
According to the ratio of the filling materials of columns 1 and 2, accurately weigh the required stationary liquid into a 400mL beaker, add chloroform equivalent to 1.2 times the volume of the carrier and stir continuously to dissolve it, then slowly pour the carrier in, gently stir it to make it evenly soaked, stir it intermittently in a 40℃ infrared oven, transfer it into an evaporating dish, let the solvent evaporate slowly to dryness, and finally dry it at 60-70℃, cool it, sieve it and fill it into the column. The filling amount is about 2g for a 1-meter column and about 6g for a 3-meter column. b. Aging of the column
Install the filled chromatographic column on the chromatograph, temporarily disconnect one end of the detector, and age it at 140-150℃ for 6-8h with nitrogen.
c. Column performance
(1) For the peak sequence and typical chromatogram of impurities in dichloroethane, see Appendix A (reference). (2) Separation: The separation of difficult-to-separate pairs of substances is R>1. 4.1.4 Determination of correction factor
Use known pure substances to prepare a mixture with a composition similar to that of the sample impurities for testing, and then calculate the relative mass correction factor under the conditions specified in the 2
W.bzsosO.coI HG/T2662-95
standard according to the components in the prepared sample, see Appendix B (reference). 4.1.5 Analysis steps
a. Adjust the instrument and adjust the instrument according to the following reference conditions. Vaporization chamber temperature: 150℃;
Detection chamber temperature: 140℃;
Column box temperature: 80℃;
Nitrogen flow rate: 20mL/min;
Hydrogen flow rate: 45mL/min;
Air flow rate: 350mL/min;
Injection volume: 0.4μL.
b. Quantitative method: internal standard method.
c. Quantitative determination: Weigh 5-6g of sample, according to the mass percentage of impurities in the product, use a microsyringe to absorb 2μL of benzene (low-boiling internal standard) and 10L of dry trioxane (high-boiling internal standard), mix and shake the obtained mixture, analyze according to the specified conditions, and determine the peak area of the internal standard and each impurity component for calculation. 4.1.6 Calculation and result expression
The mass percentage content (X) of each impurity is calculated according to formula (1): Xx-m..ft:Ax100 ....
Where: ms——mass of internal standard, g;
——peak area of the component to be measured, mm2;
A.——peak area of internal standard, mm\;
f——mass correction factor of impurity component relative to internal standard; m——sample mass, g.
The mass percentage of dichloroethane X is calculated according to formula (2): X1-1002X,-water
Wherein: 2X-
-the sum of chromatographic impurity contents.
Take the arithmetic mean of the results of two parallel determinations as the determination result, and the difference between the two parallel determination results shall not exceed 0.06%. 4.2 Determination of density
It shall be carried out in accordance with the provisions of 2.3.3 densimeter method in GB/T4472. The difference between the two parallel determination results shall not exceed 0.0005g/cm2. 4.3 Determination of chromaticity
It shall be carried out in accordance with the provisions of GB/T3143.
4.4 Determination of water
It shall be carried out in accordance with the provisions of GB/T2366, and the test conditions are shown in Appendix C (reference). 4.5 Determination of acidity
4.5.1 Reagents and solutions
4.5.1.1 Standard sodium hydroxide titration solution: c (NaOH) = 0.01 mol/L; 4.5.1.2 Phenolic indicator solution: 10 g/L.
4.5.2 Analysis steps
Use a pipette to draw 100 mL of the sample and inject it into a separating funnel. Add 25 mL of distilled water and shake for 1 min. After standing and stratifying, separate the dichloroethane from the water phase. Wash the separated dichloroethane with water twice in the same steps. Collect the three water washings in the same conical flask, add 12 drops of phenolic indicator solution, and titrate with a standard sodium hydroxide titration solution until a slightly reddish color is the end point. 4.5.3 Calculation and result expression
The acidity percentage (X) is calculated according to formula (3): X2--Vx0.036 5x100.
100p2o
Where: V—volume of sodium hydroxide standard titration solution consumed in titration, mL; c——actual concentration of sodium hydroxide standard titration solution, 0.01mol/L; p20——density of the sample, g/cm2;
(3)
0.0365——mass of hydrochloric acid equivalent to 1.00mL sodium hydroxide standard titration solution [c(Na0H)=1.000mol/L], g.
The arithmetic mean of the results of two parallel determinations is taken as the determination result, and the difference between the results of two parallel determinations shall not exceed 0.0001%. 5 Inspection rules
5.11, 2-Dichloroethane shall be inspected by the quality inspection department of the manufacturer. The manufacturer shall ensure that the technical indicators of the products shipped meet the requirements of this product standard and attach a quality certificate in a certain format. The certificate content includes the manufacturer name, product name, batch number, production date, product grade and standard number. 5.2 When leaving the factory, any number of the same grade is considered as a batch, and the sampling method is carried out in accordance with the corresponding content of the liquid in the flowing state at room temperature in GB/T6680. The number and amount of samples shall be carried out in accordance with Article 6.6 of GB/T6678. The sampler shall also be familiar with and comply with the safety requirements of GB/T3723 for sampling.
The total amount of the sample shall not be less than 500g. The selected samples shall be mixed and put into two clean, dry bottles with ground stoppers in equal amounts, and labeled. One bottle is for inspection and the other is sealed and stored for future reference. The shelf life is 2 months. 5.3 The inspection results shall be determined in accordance with the rounded value comparison method of GB/T1250. If one indicator does not meet the requirements of this standard, re-sampling from twice the amount of packaging shall be carried out for re-inspection. If the re-inspection result shows that only one indicator does not meet the requirements of this standard, the entire batch of products shall be unqualified.
5.4 The user has the right to inspect and accept the product quality according to this standard. During the storage period, if the supply and demand parties have any objections to the product quality, they shall promptly raise them and the two parties shall negotiate to resolve them or ask the arbitration unit to conduct arbitration. 6 Marking, packaging, transportation and purchase and storage
6.1 Each package shall be painted with a clear and firm mark of the manufacturer's name, address, product name, trademark, product grade, product batch number, production date, this standard number and product net weight, and shall have the "flammable liquid" and "toxic" marks specified in GB190. 6.2 The product shall be packaged in dry and clean iron drums (net weight of each drum is 250kg) or tank trucks. 6.3 During transportation, it shall be handled with care to avoid damage caused by collision with hard materials, and avoid sun exposure and rain. 6.4 The product shall be stored in a dry, ventilated warehouse with a temperature below 35℃ and fireproof and explosion-proof. The storage period is 2 months from the date of leaving the factory.
W.bzsoso.coIHG/T2662—95
Appendix A
Typical chromatogram of main content low-boiling and high-boiling substances (reference)
Figure A1 Typical chromatogram (3-meter column low boiling)
1—Ethylene chloride, 2—Venelide chloride, 3-trans-1,2-dichloroethylene, 4—Carbon tetrachloride, 5—Dichloromethane, 6—Benzene, 7—Trichloroethylene, 8—Trichloromethane; 9—1,2-Dichloroethane 5
6
Carbon tetrachloride
Dichloromethane
Trichloroethylene
Trichloromethane
Dichloropropane
Trichloroethane||tt ||HG/T2662—95
Figure A2 Typical chromatogram (1 meter column high boiling)
1—1,2-dichloroethane, 2—trichloroethane; 3—n-dodecane Appendix B
Relative mass correction factors of low-boiling and high-boiling impurities to internal standard (reference)
Relative mass correction factors
Dodecane
Ethyl chloride
Vinylidene chloride
Trans-1,2-dichloroethylene
HG/T2662—95
Relative mass correction factors
Since there is no standard sample, the relative mass correction factor of ethyl chloride, vinylidene chloride and trans-1,2-dichloroethylene is calculated as 1. Appendix C
Determination of water content in 1,2-dichloroethane Chromatographic operation reference conditions and typical chromatogram (reference)
Chromatographic operation reference conditions
Chromatographic column: 3m long, 3mm inner diameter
Filling material: Shangshi 407 organic carrier, particle size 0.180~0.250mm (60~80 mesh) Column temperature: 130℃;
Detection chamber temperature: 150℃;
Vaporization chamber temperature: 160℃;
Carrier gas (H2) flow rate: 25mL/min;
Detector: thermal conductivity detector;
Injection volume: 8μL.
Typical chromatogram
Additional instructions:
HG/T2662-95
Figure c1 Typical chromatogram
1-1,2-dichloroethane, 2-water
This standard is proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is technically managed by the Beijing Chemical Research Institute of the Ministry of Chemical Industry. This standard is drafted by the Changzhou Petrochemical Plant in Jiangsu. The main drafters of this standard are Shan Bingwu and Gao Shundi. This standard is equivalent to TOCT1942-86. From the date of implementation of this standard, the original ministerial standard HG2-1438-81 "Industrial 1,2-dichloroethane" of the People's Republic of China will be invalid. w.bzsoso: com2-Dichloroethane, 2-trichloroethane; 3-n-dodecane Appendix B
Relative mass correction factors of low-boiling and high-boiling impurities to internal standard (reference)
Relative mass correction factors
Dodecane
Ethyl chloride
Vinylidene chloride
Trans-1,2-dichloroethylene
HG/T2662—95
Relative mass correction factors
Since there is no standard sample for ethyl chloride, vinylidene chloride and trans-1,2-dichloroethylene, the relative mass correction factor is calculated as 1. Appendix C
Determination of water content in 1,2-dichloroethane Chromatographic operation reference conditions and typical chromatogram (reference)
Chromatographic operation reference conditions
Chromatographic column: 3m long, 3mm inner diameter
Filling material: Shangshi 407 organic carrier, particle size 0.180~0.250mm (60~80 mesh) Column temperature: 130℃;
Detection chamber temperature: 150℃;
Vaporization chamber temperature: 160℃;
Carrier gas (H2) flow rate: 25mL/min;
Detector: thermal conductivity detector;
Injection volume: 8μL.
Typical chromatogram
Additional instructions:
HG/T2662-95
Figure c1 Typical chromatogram
1-1,2-dichloroethane, 2-water
This standard is proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is technically managed by the Beijing Chemical Research Institute of the Ministry of Chemical Industry. This standard is drafted by the Changzhou Petrochemical Plant in Jiangsu. The main drafters of this standard are Shan Bingwu and Gao Shundi. This standard is equivalent to TOCT1942-86. From the date of implementation of this standard, the original ministerial standard HG2-1438-81 "Industrial 1,2-dichloroethane" of the People's Republic of China will be invalid. w.bzsoso: com2-Dichloroethane, 2-trichloroethane; 3-n-dodecane Appendix B
Relative mass correction factors of low-boiling and high-boiling impurities to internal standard (reference)
Relative mass correction factors
Dodecane
Ethyl chloride
Vinylidene chloride
Trans-1,2-dichloroethylene
HG/T2662—95
Relative mass correction factors
Since there is no standard sample for ethyl chloride, vinylidene chloride and trans-1,2-dichloroethylene, the relative mass correction factor is calculated as 1. Appendix C
Determination of water content in 1,2-dichloroethane Chromatographic operation reference conditions and typical chromatogram (reference)
Chromatographic operation reference conditions
Chromatographic column: 3m long, 3mm inner diameter
Filling material: Shangshi 407 organic carrier, particle size 0.180~0.250mm (60~80 mesh) Column temperature: 130℃;
Detection chamber temperature: 150℃;
Vaporization chamber temperature: 160℃;
Carrier gas (H2) flow rate: 25mL/min;
Detector: thermal conductivity detector;
Injection volume: 8μL.
Typical chromatogramWww.bzxZ.net
Additional instructions:
HG/T2662-95
Figure c1 Typical chromatogram
1-1,2-dichloroethane, 2-water
This standard is proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is technically managed by the Beijing Chemical Research Institute of the Ministry of Chemical Industry. This standard is drafted by the Changzhou Petrochemical Plant in Jiangsu. The main drafters of this standard are Shan Bingwu and Gao Shundi. This standard is equivalent to TOCT1942-86. From the date of implementation of this standard, the original ministerial standard HG2-1438-81 "Industrial 1,2-dichloroethane" of the People's Republic of China will be invalid. w.bzsoso: com
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