Some standard content:
Chemical Industry Standard of the People's Republic of China
HG/T2547-93
Industrial chloroethanol solution
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 chloroethanol solution
Subject content and scope of application
HG/T2547-93
Replaces HG2-453-66 (83)
This standard specifies the technical requirements, test methods, inspection rules and marking, packaging, transportation, storage, etc. of industrial chloroethanol solution. This standard applies to chloroethanol solution, an azeotrope synthesized from ethylene, chlorine and water and prepared by distillation.
Molecular formula: C,H.OCl
Structural formula:
Relative molecular mass: 80.51 (according to the 1989 international relative atomic mass) 2 Reference standards
GB/T 601
Preparation of standard solutions for titration analysis (volume analysis) Chemical reagents
GB/T603 Preparation of preparations and products used in chemical reagent test methods GB1250 Expression and determination methods of limit values GB/T6678 General rules for sampling of chemical products
General rules for sampling of liquid chemical productsbzxZ.net
GB/T6680
3 Technical requirements
3.1 Appearance: light yellow or yellow liquid.
3.2 The quality of chloroethanol solution shall meet the requirements in the following table. %
Chloroethanol content
Dichloroethane content
Acidity (in HCI)
Test method
The reagents and water used in this standard, unless otherwise specified, are analytically pure reagents and distilled water or water of equivalent purity. The standard solutions, preparations and products used in this standard are prepared in accordance with the provisions of GB/T601 and GB/T603 unless otherwise specified.
4.1 Determination of chloroethanol content
Approved by the Ministry of Chemical Industry of the People's Republic of China on September 25, 1993 and implemented on July 1, 1994
W.bzsoso.coD4.1.1 Summary of the method
HG/T2547-93
Chloroethanol is hydrolyzed into chloride ions in a weak alkaline medium and titrated with a standard silver nitrate titration solution using potassium chromate as an indicator. 4.1.2 Reagents and solutions
Sodium carbonate solution: 5g/L
Nitric acid solution: 20g/L;
Potassium chromate solution: 50g/L;
Phenol indicator solution: 10g/L,
Silver nitrate standard titration solution: c(AgNOs)=0.1mol/L. e.
4.1.3 Instruments and equipment
General laboratory instruments and equipment.
4.1.4 Analysis steps
Use a weighing bottle to weigh 12.5~13g of the laboratory sample, accurate to 0.0002g, transfer it to a 250mL volumetric flask, rinse the weighing bottle with about 100mL of water several times, transfer it to the volumetric flask and rinse it with water to the scale, and shake it well. Use a pipette to draw 10mL of the test solution into a 250mL standard ground-mouth conical flask, add 50mL of sodium carbonate solution, connect a standard ground-mouth condenser, pass cooling water, place in a boiling water bath for 30min, take it out, cool it slightly, rinse the condenser with about 10mL of water, remove the standard ground-mouth conical flask, cool it to room temperature, add 2 to 3 drops of phenolic indicator solution, neutralize it with nitric acid solution until the red color just disappears, add 2mL of potassium chromate indicator solution, and titrate with silver nitrate standard titration solution until the red brown color is the end point. At the same time, perform a blank test.
4.1.5 Calculation of analysis results
The mass percentage content Xi of chloroethanol is calculated according to formula (1): (Vi-V)·cX0. 080 51X1002. 21XsX
m×250
(Vi-Vo）·cX201.275
Wherein: V1——the volume of silver nitrate standard titration solution consumed by the sample, mL; -2.21X3
——the volume of silver nitrate standard titration solution consumed by the blank test, mL; Vo
the actual concentration of silver nitrate standard titration solution, mol/L; (1)
——the mass of the laboratory sample weighed, g;
0.08051——the mass of chloroethanol in grams equivalent to 1.00mL of silver nitrate standard titration solution [c(AgNO:)=1.000mol/L);
2.21——the coefficient for converting hydrogen chloride to chloroethanol; Xs——acidity (4.3.5).
The arithmetic mean of the results of two parallel determinations is taken as the determination result. The difference between the two parallel determination results shall not exceed 0.2%. 4.2 Determination of dichloroethane content
4.2.1 Method summary
In a strong alkaline alcohol solution, dichloroethane, chloroethanol and acid in the sample are hydrolyzed and neutralized respectively. Chloride ions are generated, and potassium chromate is used as an indicator solution and titrated with silver nitrate standard titration solution to calculate the content of dichloroethane in the laboratory sample. 4.2.2 Reagents and solutions
Potassium hydroxide;
Ethanol solution: 550g/L;
c. Nitric acid solution: 200g/L;
W. Potassium chromate indicator solution: 50g/L;
e. Phenolphthalein indicator solution: 10g/L;
HG/T2547—93
f. Standard silver nitrate titration solution: c(AgNOs)=0.1mol/L. 4.2.3 Analysis steps
Use a pipette to draw 10 mL of the test solution prepared from the laboratory sample in (4.1.4) into a 250 mL standard ground-mouth conical flask, add 30 mL of ethanol solution and 4 g of potassium hydroxide, connect a standard ground-mouth condenser, pass cooling water, reflux in a boiling water bath for 1 h, take it out, cool it slightly, rinse the condenser with about 10 mL of water, remove the standard ground-mouth conical flask, cool it to room temperature, add 2 to 3 drops of phenol anhydride indicator solution, neutralize it with nitric acid solution until the red color just disappears, add 2 mL of potassium chromate indicator solution, and titrate with silver nitrate standard titration solution until the red color is reddish brown as the end point. At the same time, perform a blank test.
4.2.4 Calculation of analysis results
The mass percentage of dichloroethane X2 is calculated according to formula (2): X2-{(VV)-(V--Vo)·oX0. 099×100m×250
[(Vs-V2)-(V.-Vo))·cX247.5m
Wherein: V:——the volume of the standard silver nitrate solution consumed by the sample, mL; V2—the volume of the standard silver nitrate solution consumed in the blank test, mL; Vi—the volume of the standard silver nitrate solution consumed when titrating the chloroethanol sample, mLV. —The volume of silver nitrate standard titration solution consumed in the blank test of monochloroethanol, mL; the actual concentration of silver nitrate standard titration solution, mol/L; m
-the mass of the weighed sample, g;
the mass of dichloroethane equivalent to 1.00mL silver nitrate standard titration solution [c (AgNO) = 1.000mol/L] expressed in grams.
The arithmetic mean of the results of two parallel determinations is taken as the determination result, and the difference between the two parallel determination results shall not be greater than 0.25%. 4.3 Determination of acidity
4.3.1 Summary of the method
The acid in the sample is titrated with sodium hydroxide standard titration solution using phenolic acid as the indicator solution. 4.3.2 Reagents and solutions
a. Phenolic indicator solution: 10g/L;
b. Sodium hydroxide standard titration solution: c (NaOH) = 0.01mol/L. 4.3.3 Instruments and equipment
General laboratory instruments and equipment.
4.3.4 Analysis steps
Add 30mL of water and 2-3 drops of phenol indicator solution to a conical flask, and titrate with sodium hydroxide standard titration solution until it turns slightly red. Then weigh 5.0g of laboratory sample, accurate to 0.1g, and titrate with sodium hydroxide standard titration solution until the slightly red color does not disappear for 30s. This is the end point. 4.3.5 Calculation of analysis results
Acidity (HCI) X expressed as a percentage by mass: Calculate according to formula (3): Xs = V·cX0. 036 5X100
(3)
HG/T2547-93
Wherein: V is the volume of the standard sodium hydroxide titration solution consumed by the laboratory sample, mL; c is the actual concentration of the standard sodium hydroxide titration solution, mol/L; m is the mass of the laboratory sample, g;
0.0365 is the mass of hydrogen chloride in grams equivalent to 1.00 mL of the standard sodium hydroxide titration solution [c (Na0H) = 1.000 mol/L].
Take the arithmetic mean of the results of two parallel determinations as the determination result. The difference between the two parallel determination results shall not be greater than 0.003%. 5 Inspection rules
5.1 Chloroethanol solution shall be inspected by the quality supervision and inspection department of the manufacturer. The manufacturer shall ensure that all technical indicators of the products shipped meet the requirements of this product standard and attach a quality certificate in a certain format. The content of the quality certificate includes product name, batch number, net weight, date of shipment and the standard number. 5.2 Provisions on product batches at the time of shipment: For products packaged in tank trucks, each tank truck is a batch, and for products packaged in barrels, any number of the same quality is a batch.
Sampling method and sampler: Sampling and sampler of barreled products shall be carried out in accordance with the provisions of 2.1.3 of GB/T6680. Sampling and sampler of products packaged in tank trucks shall be carried out in accordance with the relevant provisions of 2.3.1 of GB/T6680. For the number of sampling units for large barrel packaging, the number shall be in accordance with Article 6.6 of GB/T6678. The sampling volume of each batch shall not be less than 500mL. After fully mixing, the samples shall be divided into two clean and dry wide-mouth bottles, sealed, labeled and marked with product name, batch number, sampling date and sampler. One bottle shall be sent to the quality inspection department for inspection, and the other bottle shall be kept for two months for future reference. 5.3 The inspection results shall be determined according to the rounded value comparison method of GB1250. If one of the indicators in the inspection results does not meet the requirements of this standard, samples shall be taken from the packaging of twice the amount for re-inspection. If only one indicator in the re-inspection results does not meet the requirements of this standard, the entire batch of products shall be unqualified.
5.4 The user unit has the right to accept the product quality according to this standard. When the supply and demand parties have objections to the product quality, they shall promptly raise the issue and resolve the issue through negotiation or ask the arbitration unit to conduct arbitration analysis. 6 Marking, packaging, transportation and purchase and storage
6.1 Clearly and firmly mark the manufacturer name, product name, product batch number, production date, this standard number and product net weight on the packaging barrel with paint.
6.2 This product is packaged in iron barrels or railroad tank cars. When packaged in iron barrels, the net weight of each barrel is 200kg, and the weight difference is allowed to be ±0.5kg. 6.3 During transportation and handling, avoid violent impact, avoid cracking of the barrel skin weld, and prevent rain and sun. 6.4 This product should be stored in a dry, well-ventilated warehouse or shed. Additional remarks:
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 jurisdiction of the Beijing Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Jinxi Chemical General Plant. The main drafters of this standard are Gao Fenglin and Wang Huilin. 4
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