Some standard content:
Chemical Industry Standard of the People's Republic of China
HG/T2544-93
Industrial p-chlorophenol
Published on September 25, 1993
Ministry of Chemical Industry of the People's Republic of China
Implemented on July 1, 1994
WChemical Industry Standard of the People's Republic of China
P-chlorophenol
Subject Content and Scope of Application
HG/T2544-93
This standard specifies the technical requirements, test methods, inspection rules and marking, packaging, transportation and storage requirements for industrial p-chlorophenol. This standard applies to p-chlorophenol produced by direct chlorination of phenol and sulfuryl chloride method. This product is mainly used in the synthesis of pesticides, medicines, dyes and other organic chemical products.
Molecular formula: CH,OCl
Structural formula:
Relative molecular mass: 128.56 (according to the international relative atomic mass in 1989) 2 Reference standards
Dangerous goods packaging mark
GB/T603 Preparation method for expressing and judging the limit value of preparations and products used in chemical reagent test methods GB1250
Determination of water content in chemical products
Karl Fischer method (general method)
GB/T6283
GB/T6678
GB/T6679
GB/T7533
3 Technical requirements
General rules for sampling of chemical products
General rules for sampling of solid chemical products
Test method for crystallization point of organic chemical products 3.1 Appearance: white or slightly yellow crystals.
3.2 The quality of industrial p-chlorophenol shall meet the requirements of the following table: Item
Ph-chlorophenol content, %
Crystallization point,
Water content, %
4 Test method
Superior quality
The reagents used in the test methods of this standard shall be analytically pure reagents unless otherwise specified. Qualified quality
The preparations and products used in the test shall be prepared in accordance with the provisions of GB/T603 unless otherwise specified. 4.1 Determination of p-chlorophenol content
4.1.1 Summary of the method
Dissolve the sample in ethyl acetate and perform sample analysis under the specified chromatographic operating conditions. Detection was performed using a hydrogen flame ionization detector and the internal standard method was used for quantification (approved by the Ministry of Chemical Industry of the People's Republic of China on September 25, 1993 and implemented on July 1, 1994). The peak area of the component to be tested was compared with the peak area of the internal standard substance to calculate the content of p-chlorophenol in the sample. 4.1.2 Reagents and Materials 4.1.2.1 Solvent: Ethyl acetate; 4.1.2.2 Standard: p-chlorophenol, purity not less than 99.5% 4.1.2.3 Internal standard: dimethyl phthalate, purity not less than 99.0%. 4.1.2.4 Chromatographic column
Stationary liquid: polycyanoalkylsiloxane (OV-225); Carrier: ChromosorbWAWDMCS, 0.15~0.18mm, b.
Chromatographic column tube: stainless steel spiral column, column length 1m, inner diameter Φ4mm; c.
Preparation and aging of chromatographic column:
Prepare the stationary phase according to the ratio of ChromosorbWAWDMCS:OV-225=100:5; dissolve OV-225 in ethyl acetate with a volume slightly larger than the volume of the carrier, and then pour the pre-weighed carrier into it and mix well. Stir gently under an infrared lamp to completely evaporate the solvent, then place in an oven at 40-60°C for 4 hours; fill the prepared stationary phase into the chromatographic column by pumping, with a filling amount of about 3g/m, and plug both ends of the column with glass fiber, then age with nitrogen for 12 hours at a nitrogen flow rate of 20ml/min at a temperature higher than 30°C; the peak width separation of difficult-to-separate substances is required to be ≥1.8; other suitable chromatographic columns can also be used if they can meet the above analysis requirements. 4.1.2.5 Carrier gas and auxiliary gas
a. Carrier gas: nitrogen, purity not less than 99.95%, dried and purified by silica gel and molecular sieve; b. Combustion gas: hydrogen, purity not less than 99.9%; c. Combustion-supporting gas: air, dried and purified by silica gel and molecular sieve. 4.1.3 Instruments and equipment
4.1.3.1 Gas chromatograph: equipped with hydrogen flame ionization detector, detection limit D<5×10-1°g/s; baseline drift number is not more than 1×10-11A/30min.
4.1.3.2 Recorder: range 10mV, or microprocessor. 4.1.3.3 Injector: 10uL.
4.1.4 Chromatographic test reference conditions, correction factor determination and chromatogram are shown in Appendix A. 4.1.5 Analysis steps
Weigh 0.5~0.6g sample and internal standard dimethyl phthalate respectively, accurate to 0.0002g. Place in a sampling bottle, add 2~3mL ethyl acetate, mix the solution evenly, and use it as a sample. Inject 1uL of sample under the selected chromatographic operating conditions, wait until the chromatographic peak is completely eluted, measure the peak areas of p-chlorophenol and internal standard respectively, and use the relative correction factor of p-chlorophenol for correction. 4.1.6 Calculation of analysis results
The p-chlorophenol content X expressed as mass percentage is calculated as follows: x=ms:A:fa×100
Wherein: A—peak area of internal standard;
Ai—peak area of p-chlorophenol;
ms——mass of internal standard, g;
m——mass of sample, g;
fs is the relative correction factor of p-chlorophenol and internal standard. Take the arithmetic mean of the results of two parallel determinations as the determination result, and the difference between the results of two parallel determinations shall not be greater than 0.4%. 4.2 Determination of crystallization point
The sampling amount is about 15g. Determine according to the method specified in GB/T7533. The sample is directly determined without drying. 2
HG/T254493
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 be greater than 0.2℃. 4.3 Determination of moisture
The sampling volume is about 15g. Determine according to the method specified in Chapter 6 "Visual Method" or Chapter 7 "Direct Coulometric Titration" of GB/T6283. 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 be greater than 0.01%. 5 Inspection rules
5.1 Parachlorophenol shall be inspected by the quality inspection department of the manufacturer. The manufacturer shall ensure that all technical indicators of all products shipped meet the requirements of this standard. Each batch of products shipped shall be accompanied by a quality certificate in a certain format. The quality certificate includes the following contents: product name, product grade, batch number, net weight, factory date and this standard number. 5.2 After receiving parachlorophenol, the user unit has the right to accept it in accordance with the provisions of this standard. 5.3 Sampling
5.3.1 The number of sampling units shall be selected in accordance with the provisions of Article 6.6.1 and Chapter 10 of GB/T6678. 5.3.2 Sampling method: Sampling shall be carried out in accordance with the method specified in 2.3.1 of GB/T6679. The sampling volume of each barrel shall not be less than 20g, and the total sampling volume shall not be less than 200g.
5.4 After the taken samples are fully mixed and divided, they shall be divided into two clean and dry glass bottles in equal amounts, sealed, and labeled with the product name, batch number, grade, sampling date and name of the sampler. One bottle shall be sent to the laboratory for inspection, and the other bottle shall be kept in a cool and dry place for 3 months for future reference.
5.5 The determination of the test results shall be determined in accordance with the rounded value comparison method in GB1250. If one of the indicators in the test results does not meet the requirements of this standard, samples should be taken from twice the amount of packaging units for re-testing. Even if only one indicator in the re-test results does not meet the requirements of this standard, the entire batch of products shall be unqualified.
5.6 Industrial para-chlorophenol is based on the amount of products produced by each distillation kettle as a batch. 5.7 If the product has been stored in the factory for more than half a year, it should be re-tested before leaving the factory. 5.8 When the supply and demand parties have disputes over product quality, they shall be resolved through negotiation or by arbitration by a national arbitration institution agreed by both parties. 6 Marking, packaging, transportation and storage
6.1 The packaging container shall be firmly marked, including the manufacturer's name, product name, trademark, product grade, product gross weight, net weight, product batch number and this standard number, as well as the "toxic" mark specified in GB190. 6.2 Industrial para-chlorophenol is packaged in clean and dry tin barrels or plastic barrels, with a net weight of 250kg, 200kg or 50kg per barrel. 6.3 Industrial p-chlorophenol should be stored in a ventilated and dry place to prevent exposure to sunlight and moisture. The transportation process should comply with the regulations on the transportation of dangerous goods. 3
WA1 Typical working conditions for chromatographic test
Chromatographic column temperature: 175℃;
Detection chamber temperature: 230℃;
Vaporization chamber temperature: 240℃;
Carrier gas flow rate: 20ml/min;
Hydrogen flow rate: 45ml/min;
HG/T2544-93
Appendix A
Operating conditions for p-chlorophenol content determination-gas chromatography (reference)bzxz.net
Air flow rate: 450ml/min;
Injection volume:
luL.
In order to obtain the best separation conditions, the working conditions of different types of chromatographs can be reasonably changed. A2
Typical spectrum of industrial p-chlorophenol and its impurities (see Figure A1)
Retention time (TR) and relative correction factor (fa) of each componentA3
See Table A1
Component name
O-chlorophenol
2.4-Dichlorophenol
p-chlorophenol
Dimethyl phthalate
A4 Determination of relative correction factor
TR(min)
Weigh 0.50.6g of p-chlorophenol standard and internal standard dimethyl phthalate respectively, accurate to 0.0002g. Place in a small sampling bottle, add 2-3ml of ethyl acetate to mix the solution evenly, and obtain a calibration mixture. Inject the mixture under the selected chromatographic operating conditions and perform chromatographic analysis. The concentration or amount of the injected calibration mixture is basically the same as the amount of the component contained in the sample to be tested. After the chromatographic peaks have finished eluting, measure the peak areas of the standard and internal standard respectively. Calculate the correction factor fs of the component as follows. fa
Wherein: A—peak area of internal standard substance;
Ar——peak area of component i;
-mass of dimethyl phthalate containing internal standard substance in the calibration mixture, g; -mass of component 1 in the calibration mixture,. m
Relative correction factor should be re-measured every two weeks and can be re-measured at any time if necessary. 4
bzsoso：coDAdditional instructions:
HG/T2544—93
a—ethyl acetate; b—o-chlorophenol; c—phenol; d—2.4-dichlorophenol; e—o-chlorophenol; f dimethyl phthalate This standard is 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 jurisdiction of the Beijing Institute of Chemical Industry of the Ministry of Chemical Industry. This standard was drafted by Jiangsu Jianhu County Organic Chemical Factory. Qingdao Jiaonan Chemical Factory and Shanghai Zhongli Chemical Factory participated in the drafting. The main drafters of this standard are Gu Renjun, Lin Huaming, Zhang Yinhua and Tao Yeqiang.
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