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Chemical Industry Standard of the People's Republic of China
HG/T2543-93
Industrial Chloromethyl Methyl Ether
Published on September 25, 1993
Ministry of Chemical Industry of the People's Republic of China
Implemented on July 1, 1994
W Chemical Industry Standard of the People's Republic of China
Industrial Chloromethyl Methyl Ether
Subject Content and Scope of Application
HG/T2543-93
This standard specifies the technical requirements, test methods, inspection rules and marking, packaging, transportation and storage of industrial chloromethyl methyl ether. This standard applies to chloromethyl methyl ether obtained by passing hydrogen chloride gas into methanol and formaldehyde solution. This product is mainly used in the production of anion exchange resin.
Molecular formula: CICH2OCH3
Structural formula:
Relative molecular mass: 80.50 (according to the international relative atomic mass in 1989) 2 Reference standards
Dangerous goods packaging mark
GB191 Pictorial mark for packaging storage and transportation
GB/T601
GB/T603
GB1250
Chemical reagent titration analysis (volume analysis) Preparation of standard solution for chemical reagent test method Methods of expressing and determining the preparation limit values of preparations and products usedGeneral rules for determination of density and relative density of chemical products GB/T4472
GB/T6678
GB/T6680
GB/T7534
3 Technical requirements
General rules for sampling of chemical products
General rules for sampling of liquid chemical products
Determination of boiling range of volatile organic liquids for industrial use 3.1 Appearance: Light yellow liquid with the pungent odor of formaldehyde and hydrogen chloride. 3.2 Industrial chloromethyl methyl ether shall meet the requirements of the following table: Item
Total chlorine content, %
Density, p20g/cms
Steamed stuffing test, 0℃, 101.325kPa
55~59.5℃Distilled volume, ml
Published by the Ministry of Chemical Industry of the People's Republic of China on September 25, 1993
Qualified products
1.065~1.075
Implemented on July 1, 1994
W.4 Test method
HG/T2543-93
The reagents and water used in this standard shall be analytically pure reagents and distilled water or water of equivalent purity unless otherwise specified. The standard solutions, preparations and products used in this standard are prepared in accordance with GB/T601 and GB/T603 unless otherwise specified. 4.1 Appearance
4.1.1 Visual inspection
4.2 Determination of total chlorine
4.2.1 Summary of the method
After the organic chlorine in the sample is converted into inorganic chlorine by sodium hydroxide treatment, a known excess of silver nitrate standard titration solution is added, and the excess silver nitrate standard titration solution is back-titrated with ammonium thiocyanate standard titration solution using ammonium ferric vanadium as an indicator. When the end point is reached, the excess ammonium thiocyanate standard titration solution and the ammonium ferric vanadium indicator form a brick-red precipitate to indicate the end point. The reaction equation is as follows:
CI-+AgtAgCl
Ag+ (remaining amount)+SCN-AgSCN
Fe8++3SCN-Fe(SCN)★
4.2.2 Reagents and materials
4.2.2.1 Nitrobenzene;
4.2.2.2 Nitric acid solution: 1+3;
4.2.2.3 Sodium hydroxide solution: 100g/L
Brick red
4.2.2.4 Standard silver nitrate titration solution: c(AgNOs) = 0.1mol/L; 4.2.2.5 Standard ammonium thiocyanate titration solution: c(NHSCN) = 0.1mol/L; 4.2.2.6 Ammonium ferric sulfate indicator solution: 80g/L. 4.2.3 Instruments
General laboratory instruments
4.2.3.1 Volumetric flask: 50mL;
4.2.3.2 Brown burette: 50mL;
4.2.3.3 Pipette: 20mL, 10mL, 1mL. 4.2.4 Analysis steps
Measure 20mL of sodium hydroxide solution (4.2.2.3) in a 50mL volumetric flask and weigh it to the accuracy of 0.0001g. Quickly add 0.5mL of sample, stopper it and shake it vigorously until the white smoke in the flask disappears. After about 10 minutes, weigh it to the accuracy of 0.0002g. Add water to dilute to the scale. This liquid is liquid A.
Put 50mL of water in a conical flask, then draw 10.00mL of A solution into the conical flask, add 5mL of nitric acid solution (4.2.2.2), 5mL of nitrobenzene (4.2.2.1), drop 25.00mL of silver nitrate standard titration solution (4.2.2.4), add 2mL of ammonium ferric sulfate indicator (4.2.2.6), then titrate with ammonium thiocyanate standard titration solution (4.2.2.5) until brick red just appears. 4.2.5 The total amount of chlorine expressed as mass percentage (x) is calculated according to the following formula: x(cV))X0.03545x100
_1×17.72bzxZ.net
Wherein: Ci——actual concentration of standard silver nitrate titration solution, mol/L, C2
actual concentration of standard ammonium thiocyanate titration solution, mol/L; Vi——volume of standard silver nitrate titration solution, mL; V2—volume of standard ammonium thiocyanate titration solution consumed, mL; 2
m——mass of the sample, g;
HG/T2543-93
0.03545—mass of chlorine in grams equivalent to 1.00mL of standard ammonium thiocyanate titration solution c(NH,SCN)=1.000mol/LJ.
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 0.1%. 4.3 Determination of density
Measure according to the density meter method in Section 2.3.3 of GB/T4472. 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 0.001g/cm. 4.4 Distillation test
Record the distillation volume between 55 and 59.5℃, and control the cooling water outlet temperature to <15℃. Other operating conditions shall be carried out in accordance with Article 4 of GB/T7534. 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 1mL. 5 Inspection rules
5.1 Industrial chloromethyl methyl ether shall be inspected by the quality supervision and inspection department of the manufacturer. The manufacturer shall ensure that the technical indicators of the products leaving the factory meet the requirements of this standard and attach a quality certificate in a certain format. The content includes: product name, product grade, product batch number, net weight, date of manufacture and the standard number.
5.2 The user has the right to accept the product according to the technical requirements, inspection rules and test methods specified in this standard. 5.3 The weight of each batch of products shall not exceed 5t. When packed in a tank truck, one tank truck shall be considered as one batch. 5.4 Sampling
5.4.1 The number of sampling units shall be sampled in accordance with the provisions of Section 6.6 and Chapter 10 of GB/T6678. 5.4.2 When industrial chloromethyl methyl ether is packaged in barrels, sampling shall be carried out in accordance with the provisions of Section 2.1.3 of GB/T6680. When packed in a tank truck, sampling shall be carried out in accordance with the provisions of Section 2.3.1 of GB/T6680.
5.5 Mix the samples and take 1000mL of the samples into two clean and dry bottles with ground stoppers. Label the bottles. The content of the labels includes: product name, batch number, grade, sampling date and sampler. One copy shall be sent to the inspection room for inspection, and one copy shall be kept for future reference. If the user has no objection within one week after receiving the product, the sample can be destroyed.
5.6 The inspection result shall be determined by the rounded value comparison method. If one of the indicators in the inspection result does not meet the requirements of this standard, a sample shall be taken from twice the amount of packaging for re-inspection. Even if only one indicator does not meet the requirements of this standard in the re-inspection result, the entire batch of products shall be unqualified. 5.7 The user of the product shall immediately inspect and accept the goods according to the provisions of this standard after the goods arrive. When the supply and demand parties have objections to the product quality, they shall raise them in time, and the two parties shall negotiate to resolve them or ask the arbitration unit to conduct arbitration analysis. 6 Marking, packaging, transportation and purchase and storage
6.1 The products shall have product markings, including: manufacturer name, trademark, product grade, product batch number, production date, standard number, and product net weight.
6.2 The packaging container shall be painted with the "anti-corrosion" mark specified in GB190 and the "upward" mark specified in GB191. 6.3 Industrial chloromethyl methyl ether is packaged in polyvinyl chloride barrels or polyvinyl chloride tank trucks. 6.4 It is packaged in polyvinyl chloride barrels, with the net weight of each barrel not exceeding 200kg.5 During transportation, the product should be handled with care and violent impact is strictly prohibited to prevent the package from breaking. If the package breaks or leaks, flush it with plenty of water.
6.6 Cover it with a bitter cloth during transportation. 6.7 The product should be stored in a cool, ventilated and dry warehouse, isolated from fire sources, and protected from sunlight and rain. 3
HG/T2543—93
Appendix A
Determination of total chlorine content of chloromethyl methyl ether—neutralization method (reference)
The purpose of setting up this method is mainly to reduce the pollution of chloromethyl methyl ether and nitrobenzene to the environment. This method is provided for users' reference. This method is applicable to chloromethyl methyl ether obtained by passing hydrogen chloride gas into methanol formaldehyde solution. A1 Method Summary
Chloromethyl methyl ether decomposes into methanol, formaldehyde and hydrochloric acid in water. Hydrochloric acid ionizes into hydrogen ions and chloride ions in water. The concentration of hydrogen ions is titrated with sodium hydroxide standard titration solution, and the chlorine content in chloromethyl methyl ether is calculated. A2 Reagents and Solutions
A2.1 Standard sodium hydroxide titration solution: c(NaOH)=0.1mol/L; A2.2 Phenolphthalein indicator solution: 10g/L.
A3 Analysis Steps
Take 20mL of freshly boiled and cooled distilled water in a 50mL volumetric flask, weigh it to an accuracy of 0.0002g, quickly add 1mL of sample, stopper it and shake it vigorously until the white smoke in the flask disappears. After about 10 minutes, weigh it to an accuracy of 0.0001g, and dilute it to the scale with water. This solution is solution A.
Add 50ml of water to a conical flask, then add 10.0ml of solution A, add 2 drops of phenolphthalein indicator, and titrate with sodium hydroxide standard titration solution until pink just appears, and keep it for 15s without fading as the end point. A4 Expression and calculation of analysis results
The total amount of chlorine expressed as mass percentage (x) is calculated as follows: X=c·VX0.03545
c——actual concentration of sodium hydroxide standard titration solution, mol/L; where:
V——volume of sodium hydroxide standard titration solution consumed, mL; m——mass of sample, g;
0.03545——mass of chlorine expressed in grams equivalent to 1.00ml sodium hydroxide standard titration solution [c(Na0H)=1.000mol/].
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 0.1%. Additional Notes:
This standard was proposed by the Science and Technology 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 was drafted by Shenyang Chemical Plant No. 4 and Shenyang Fertilizer Plant, and Liuquan Chemical Plant and Dandong Donggang Organic Chemical Plant participated in the drafting. The main drafters of this standard are Zhao Liyan and Zhao Tong.
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