Some standard content:
Chemical Industry Standard of the People's Republic of China
HG/T2560-94
Ethane
Published on February 9, 1994
Ministry of Chemical Industry of the People's Republic of China
Implemented on June 1, 1994
W Chemical Industry Standard of the People's Republic of China
Subject Content and Scope of Application
HG/T2560-94
This standard specifies the technical requirements, test methods, inspection rules, as well as marking, packaging, transportation and storage of industrial ethyl bromide. This standard applies to industrial ethyl bromide synthesized from ethanol and bromine or hydrobromic acid as raw materials. This product is mainly used as an ethylating agent in the pharmaceutical industry and organic synthesis, and can also be used as a refrigerant and solvent, etc. Molecular formula: C,HsBr
Relative molecular mass: 108.97 (according to the international relative atomic mass in 1989) 2 Reference standards
GB190 Dangerous goods packaging mark
GB/T603
GB/T1250
GB/T4472
GB/T6283
Preparation method of preparations and products used in chemical reagent test methods and methods of expression and determination of chemical product density and relative density determination general rules Determination of water content in chemical products Karl Fischer method (General method) GB/T6324.2 General method for determination of dry residue after evaporation of volatile organic liquids on a water bath GB/T6678
GB/T6680
GB/T9722
3 Technical requirements
3.1 Appearance:
General rules for sampling of chemical products
General rules for sampling of liquid chemical products
General rules for gas chromatography of chemical reagents
Colorless or slightly yellowish transparent liquid. www.bzxz.net
3.2 Industrial ethyl bromide shall meet the requirements of the following table: Item
Density (pao), 8/cm3
Ethyl bromide content, %
Evaporation residue, %
Water, %
Acidity test
Approved by the Ministry of Chemical Industry of the People's Republic of China on February 9, 1994Superior product
First-class product
1.430~1.470
Qualified product
Implemented on June 1, 1994
W.4 Test method
HG/T2560—94
The reagents and water used in this standard, unless otherwise specified, are analytical reagents and distilled water or water of equivalent purity. The preparations and products used in this standard, unless otherwise specified, are prepared in accordance with the provisions of GB/T603. 4.1 Determination of density
Carry out in accordance with the provisions of Article 2.3.3 Densitometer method in GB/T4472. The arithmetic mean of the results of two parallel determinations shall be taken as the determination result, and the difference between the two parallel determination results shall not exceed 0.0005g/cm. 4.2 Determination of ethyl bromide content
4.2.1 Reagents and materials
a. Acetone;
Ether, chromatographic grade;
Ethanol, chromatographic grade;
Ethyl bromide, purity ≥99.9%;
Carrier gas: hydrogen or hydrogen, purity ≥99.9%. 4.2.2 Instruments and equipment
4.2.2.1 Gas chromatograph
Any type of gas chromatograph equipped with a thermal conductivity detector, whose sensitivity and stability meet the relevant provisions of GB/T9722. 4.2.2.2 Chromatographic column
Column tube: stainless steel tube with inner diameter @4mm and length of 2m; b.
Stationary liquid: polyethylene glycol 20M;
Carrier: silanized white diatomaceous earth 101 carrier, particle size 0.18~0.25mm (80~60 mesh); c.
Preparation and aging of chromatographic column
Prepare according to the ratio of carrier: polyethylene glycol 20M=100:10. Weigh 2.0g polyethylene glycol 20M, put it in a beaker, add appropriate amount of acetone to make it fully dissolved, slowly pour 20.0g carrier into it and evenly immerse it. Evaporate on a water bath until dry. Pre-treat the column tube according to the relevant provisions of GB/T9722, install the column by decompression method, plug the two ends of the column with glass wool, connect the inlet end to the vaporization chamber, and do not connect the outlet end to the detector. Pass nitrogen at a flow rate of 10mL/min for aging. The aging temperature is 150℃ until a stable baseline is obtained under the test conditions.
4.2.2.3 Micro-injector: 0.5μL, 1.0μL or 2.0μL. 4.2.2.4 Data processor or integrator
4.2.3 Chromatographic test reference conditions, relative retention values of each component, relative correction factor and typical chromatogram are shown in Appendix A and Figure A1. 4.2.4 The determination method of relative correction factor is shown in Appendix B. 4.2.5 Analysis steps
Operate the chromatograph according to the instruction manual. Refer to Appendix A for operating conditions. Samples can be injected after the instrument baseline is stable. Use a data processor or integrator to process the calculation results.
4.2.6 Quantitative method adopts the correction area normalization method. 4.2.7 Expression and calculation of analysis results
The content X of bromoethane expressed as mass percentage is calculated according to formula (1): X-100—X1-EX,
X100·
W.bzsoso.coIWhere: X,——the moisture content measured in 4.4, %X——the content of a certain impurity component, %:
Ar——the peak area of a certain impurity chromatographic peak; HG/T2560—94
f——the relative correction factor of a certain impurity chromatographic peak. 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 0.2%. 4.3 Determination of evaporation residue
Take 50.0mL of sample, and the rest shall be carried out according to the provisions of GB/T6324.2. 4.4 Determination of moisture
Take 10.0mL of sample, and the rest shall be carried out in accordance with the provisions of GB/T6283. The arithmetic mean of the results of two parallel determinations shall be taken as the determination result, and the difference between the two parallel determination results shall not exceed 0.03%. 4.5 Acidity test
Take 5.0mL of sample in a 20mL test tube, add 5.0mL of water without carbon dioxide, shake the test tube, add 1 drop of 1g/L methyl orange indicator solution, and if the aqueous solution is yellow, it is judged to be qualified. 5 Inspection rules
5.1 Industrial ethyl bromide shall be inspected by the quality supervision and inspection department of the manufacturer, and the manufacturer shall ensure that each batch of products shipped from the factory meets the requirements of this standard. Each batch of products shipped from the factory shall be accompanied by a quality certificate in a certain format, including: manufacturer name, product name, batch number, production date, product quality and this standard number. 5.2 The products produced in each shift are considered as a batch.
5.3 Sampling shall be carried out in accordance with the method specified in Article 2 of GB/T6678 and GB/T6680. The sampling volume shall not be less than 250mL. Divide the sample into two equal parts, put them into clean and dry glass bottles, cover them tightly and seal them, and affix labels. The label shall indicate the product name, batch number, sampling date and sampler. One bottle is for inspection and the other bottle is kept for future reference. 5.4 If one of the indicators in the inspection results does not meet the requirements of this standard, re-sampling shall be carried out from twice the amount of packaging. Even if one of the indicators in the re-inspection results still does not meet the requirements of this standard, the entire batch of products shall be unqualified. 5.5 The user has the right to accept the product quality in accordance with this standard. During the storage period, if the supply and demand parties have objections to the product quality, they shall negotiate to resolve the dispute or ask the arbitration unit to conduct arbitration analysis in accordance with this standard. 5.6 The inspection results shall be determined in accordance with the GB/T1250 rounded value comparison method. 6 Marking, packaging, transportation and storage
6.1 The markings that should be painted on the packaging barrels of industrial ethyl bromide include: product name, factory name, factory address, product net weight, batch number, trademark, production date, this standard number and the toxic signs specified in GB190. 6.2 Industrial ethyl bromide should be packaged in clean and dry galvanized iron barrels. The net weight of each barrel is 250kg. 6.3 There should be a cover during transportation to prevent exposure to the sun. 6.4 Industrial ethyl bromide should be stored in a cool, ventilated place, isolated from heat sources. Under the above conditions, the product has a storage period of 6 months. 7 Safety
Ethyl bromide has the smell of chloroform and is toxic. Avoid contact with the skin and prevent inhalation into the human body through the mouth and nose. 3
W.bzsosO.coI A1
Chromatographic test reference conditions
Column temperature: 70℃;
Vaporization chamber temperature: 100℃;
Detector temperature: 100℃,
HG/T2560—94
Appendix A
Content determination chromatographic test reference conditions and typical chromatograms (supplement)
Carrier gas flow rate: 30~40mL/min,
Injection volume: 0.4~2.0μL.
Relative retention value (ri) and relative correction factor (f) of each component Component
Ethyl chloride
Ethyl bromide
Retention time and spectrum will change accordingly, but should have appropriate separation. The analysis conditions can be adjusted appropriately, 1
B1 Determination method of correction factor
HG/T2560-94
Figure A1 Typical chromatogram of industrial ethyl bromide sample analysis 0-air; 1-ether, 2-chloroethane; 3-bromoethane; 4-ethanol Appendix B
Determination method of correction factor
Supplement)
Use a clean, dry, sealable ground-mouth bottle, and prepare several standard test solutions with similar components and contents to those in the sample by accurate weighing, and perform the test under the same test conditions as the sample. B2 Relative correction factor calculation formula
fr-A,·m
Wherein: f——Correction factor of each component relative to the main body, A—peak area of the main substance;
At——peak area of component i;
m——mass of the main substance, g,
mass of component i, g.
Relative correction factor needs to be calibrated regularly. If any change is found, it needs to be re-measured. B3
Wo
Additional instructions:
HG/T2560—94
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 under the technical supervision of the Beijing Chemical Research Institute of the Ministry of Chemical Industry. This standard is drafted by Lianyungang Seawater Chemical Plant No. 1. The main drafters of this standard are Zhang Gengzhu, Su Changliu and Liu Maochun. This standard refers to "OCT2658—86 "Industrial Ethyl Bromide".
Tip: This standard content only shows part of the intercepted content of the complete standard. If you need the complete standard, please go to the top to download the complete standard document for free.