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Chemical Industry Standard of the People's Republic of China
HG2027-91
Industrial Benzyl Chloride
Published on June 26, 1991
Published by the Ministry of Chemical Industry of the People's Republic of China and implemented on January 1, 1992
Chemical Industry Standard of the People's Republic of China
Subject Content and Scope of Application
HG2027-91
This standard specifies the technical requirements, test methods, inspection rules, marking, packaging, transportation and storage of industrial benzyl chloride. This standard applies to industrial benzyl chloride obtained by chlorination, distillation and purification of toluene. This product is mainly used as raw materials for medicine, pesticides, spices, dyes, plastics and chemical additives.
Molecular formula C, H, CI
Structural formula
Relative molecular mass 126.56 (according to the international relative atomic mass in 1987)2
Cited standards
GB1250
GB4472
GB6283
GB6678
GB6680
GB6682
GB8170
GB9722
3 Technical requirements
3.1 Appearance
Dangerous goods packaging Marking
Packaging, storage and transportation pictorial marking
Preparation of standard solutions for titration analysis (volumetric analysis) of chemical reagents Preparation of preparations and products used in test methods of chemical reagents Methods of expressing and determining limit values General rules for determination of density and relative density of chemical products Determination of water content in chemical products Karl Fischer method (general method) General rules for sampling of chemical products
General rules for sampling of liquid chemical products
Specifications for water used in laboratories
Rules for rounding off values
General rules for gas chromatography of chemical reagents
Colorless or slightly yellowish transparent liquid.
3.2 The quality of industrial benzyl chloride shall meet the requirements of Table 1: Table 1
Water content, %
Density po20g/cm
Acidity (in HCI), %
Non-volatile matter, %
Approved by the Ministry of Chemical Industry of the People's Republic of China on June 28, 1991Superior product
1.0991.105
First-class product
1.099~1.105
Qualified Product
1.097~1.107
1992-01-01Implementation
Purity, %
Total amount of impurities\, %
HG2027-91
Continued Table 1
Superior product
First-class product
Qualified product
Note: 1) This item includes chromatographic impurities such as toluene, benzaldehyde, o-(or m-)chlorotoluene, 2,4-dichlorotoluene and benzyldichloro (dichloromethylbenzene). 4 Test method
The reagents used in the test method of this standard are analytical pure reagents unless otherwise specified; the experimental water should comply with the third-grade water in GB6682.
The standard solutions, preparations and products required in the test are prepared according to the methods specified in GB601 and GB603 unless otherwise specified. 4.1 Determination of moisture
4.1.1 Analysis steps
Measure 10.0mL sample and titrate directly according to the method specified in GB6283. 4.1.2 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.005%. The arithmetic mean shall be taken as the determination result. 4.2 Determination of density
4.2.1 Analysis steps
Perform according to the method specified in Article 2.3.3 of GB4472. 4.2.2 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.0005g/cm3. The arithmetic mean shall be taken as the determination result. 4.3 Determination of acidity
4.3.1 Reagents and solutionsWww.bzxZ.net
4.3.1.1 Anhydrous ethanol;
4.3.1.2 Phenol indicator solution: 10g/L;
4.3.1.3 Standard titration solution of sodium hydroxide: c(NaOH)=0.1mol/L; 4.3.2 Analysis steps
Weigh 10g of the sample (accurate to 0.1g), put it into a 250mL conical flask, add 100mL of anhydrous ethanol, add 2~3 drops of phenol indicator solution, mix thoroughly, and titrate with standard titration solution of sodium hydroxide to a slightly reddish end point. At the same time, perform a blank test. 4.3.3 Calculation of results
The mass percentage X of acidity (in terms of HCl) is calculated according to formula (1): 0. 036 46Xc(VV)×100
Wherein: 0.03646-
6 is the mass of hydrochloric acid equivalent to 1.00mL of sodium hydroxide standard titration solution (c(Na0H)=1.000mol/L), expressed in grams;
the concentration of sodium hydroxide standard titration solution (4.3.1.3), mol/L; V
-the volume of sodium hydroxide standard titration solution consumed by the sample, mL; V1 is the volume of sodium hydroxide standard titration solution consumed by the blank test, mL; m
4.3.4 Allowable difference
The mass of the sample, 8.
The difference between the results of two parallel determinations shall not exceed 0.005%, and the arithmetic mean shall be taken as the determination result. 4.4 Determination of non-volatile matter
4.4.1 Test device
The test device is shown in Figure 1:
HG2027-91
Figure 1 Test device for determination of non-volatile matter
1-gathering port; 2-nitrogen outlet 3-quartz tube; 4-quartz boat; 5-heating box; 6-nitrogen inlet; 7-thermometer insertion port; 8-rubber plug; 9-heating furnace 4.4.1.1 Tube type electric furnace: equipped with a temperature regulator that can be adjusted within the range of 100-400℃. 4.4.1.2 Quartz tube: tube length 450mm, outer diameter 5mm, wall thickness 2mm. 4.4.1.3 Sample boat: made of hard glass or quartz, with a volume of about 3mL. Its outer dimensions should be such that the boat can be freely placed in the quartz tube, and a small hole is left at one end of the boat so that the sample boat can be taken out of the furnace with a hook. 4.4.2 Analysis steps
Add 1.0~1.2g of sample (accurate to 0.1g) to a cleaned and dried sample boat, then carefully place it in a quartz tube preheated to 182±2℃, introduce nitrogen at a flow rate of 600mL/min, and introduce the tail gas into an absorption bottle filled with sodium hydroxide alcohol solution for bubbling absorption for 15min. Then take out the sample boat and place it in a dryer to cool for 45min, and then weigh it (accurate to 0.0002g).
4.4.3 Result calculation
The mass percentage of non-volatile matter X2 is calculated according to formula (2): mlx100
Where: X2 non-volatile matter content, %;
-mass of the residue after volatilization, g;
mass of the sample,.
4.4.4 Allowable difference
The difference between two parallel determination results shall not exceed 0.02%, and the arithmetic mean shall be taken as the determination result. 4.5 Determination of purity and impurity content
4.5.1 Reagents and materials
Toluene: chromatographically pure;
O-(or m-)chlorotoluene: chromatographically pure;
Benzaldehyde;
Taro chloride: chromatographically pure;
2,4-dichlorotoluene: chromatographically pure;
f. Dichlorobenzene
Nitrogen: purity not less than 99.9%;
Hydrogen: purity not less than 99.9%;
Air: purified;
Toluene.
Instruments and equipment
HG2027-91
Gas chromatograph: Any type of gas chromatograph whose sensitivity and stability meet the relevant provisions of GB9722. 4.5.2.1
Chromatographic column:
Column tube: Hard glass column, 2m long, 4mm inner diameter; Support: Acid-washed 101 white support (0.180.25mm) (8060 mesh); Stationary liquid: Apizone L and silicone oil (V);
Preparation and aging of chromatographic column:
The column is prepared according to the ratio of acid-washed 101 white support: Apizone L: silicone oil (V) = 100:7:12. Dissolve Apizone L and silicone oil (V) in toluene with a volume slightly larger than that of the carrier (when it is cold, it can be slightly heated, but the temperature should not be greater than 80°C), then pour the weighed carrier into it, mix, and then gently stir under an infrared lamp to completely evaporate the solvent, and then place it in an oven at 120°C to dry for 2~3 hours.
The carrier coated with the stationary liquid is loaded into the chromatographic column by pumping, with a loading amount of about 4g/m, and the two ends of the column are plugged with glass fiber, and then aged for 24 hours with nitrogen gas at a nitrogen flow rate of 10ml/min at a temperature higher than 30°C.4.5.2.3Micro-injector: 10μl.
4.5.2.4 Detector: hydrogen flame ionization detector. 4.5.2.5 Recorder or microprocessor.
4.5.3 Chromatographic operating conditions
Column temperature: 135145℃;
Detection temperature: 200℃;
Vaporization temperature: 200℃;
Carrier gas: nitrogen flow rate: 30ml/min;
Hydrogen flow rate: 30ml/min;
Air flow rate: 400~500ml/min;
Injection volume: 0.2μl.
4.5.4 Analysis steps
The instrument should be operated according to the instruction manual, and the operating conditions should be carried out according to the provisions of Article 4.5.3. Samples can be injected after the baseline of the instrument is stable, and the peak area measurement should be carried out after all the peaks of each component have flowed out. The retention time (ts) and relative retention time (Rls) of each component and the relative correction factor (f) are shown in Table 2. The typical chromatogram of industrial benzyl chloride and its impurities is shown in Figure 2.
o-(m-)chlorotoluene
benzaldehyde
benzyl chloride
2,4-dichlorotoluene
dichlorobenzene
HG2027-—-91
tr/man
Note: The data in the table may be slightly different when measured using different instruments. 5
Figure 2 Typical chromatogram of industrial chlorinated taro and its impurities 1—Solvent peak (ethanol); 2—Toluene; 3—O-(m-)chlorotoluene; 4—Benzaldehyde; 5—Chloride; 6—2,4-Dichlorotoluene; 7—Dichlorobenzene 4.5.5
Result calculation
The mass percentage X of the purity of benzyl chloride: calculated according to formula (3): f
HG2027-—91
Xs-→·A+Zr,·A,·fi
（100-WX）
Impurities in benzyl chloride The mass percentage X is calculated according to formula (4): ZrAfi
X,=A+ZA
In formulas (3) and (4):
—signal attenuation ratio of benzyl chloride;
A—peak area of benzyl chloride;
—signal attenuation ratio of each impurity;
A—peak area of each impurity;
f—relative correction factor of each impurity;
W—water content of benzyl chloride measured in Article 4.1,%; X—non-volatile matter content measured in Article 4.4,%. 4.5.6 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.2%, and the arithmetic mean shall be taken as the determination result. 5 Inspection rules
(3)
5.1 Industrial benzyl chloride shall be inspected by the technical inspection department of the manufacturer, and the manufacturer shall ensure that all products leaving the factory meet the requirements of this standard. Each batch of industrial chlorinated ... If even one index of the re-test result does not meet the requirements of this standard, the whole batch of products shall be judged as unqualified. 5.6 When the supply and demand parties have objections to the product quality, the provisions of the "Interim Measures for National Product Quality Arbitration Inspection" shall apply. 5.7 The judgment of the test results shall be carried out according to the rounded value comparison method in GB1250, and the rounding shall be carried out according to GB8170. 6 Marking, packaging, transportation, storage
6.1 Marking
The packaging container shall be painted with a firm mark, which includes the manufacturer's name, product name, trademark, standard number, production date, grade mark, product gross net weight, and the toxic mark in GB190 and the mark of afraid of moisture, handle with care, and afraid of heat in GB191. 6.2 Packaging
Industrial benzyl chloride should be packaged in iron drums lined with polyethylene, or other suitable materials. 6.3 Transportation and storage
Industrial benzyl chloride should be stored in a cool and dry place; avoid rain, high temperature and fireworks during transportation. The validity period of this product is six months from the date of leaving the factory. 6
Additional instructions:
HG2027-91
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 technical jurisdiction of the Beijing Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Wuhan Organic Synthesis Chemical Plant and Jiangsu Lianyungang Chemical Plant. The main drafters of this standard are Wang Zhendong, Li Yun, Wang Zhulan, Yu Huaidao and Li Zhenrong. This standard refers to the Japanese Industrial Standard JISK4125-1983 "Taro Chloride". 75 If one of the indicators in the test results does not meet the requirements of this standard, samples should be taken from the packaging barrels with twice the amount for re-testing. If even one of the indicators in the re-test results does not meet the requirements of this standard, the entire batch of products shall be judged as unqualified. 5.6 When the supply and demand parties have objections to the product quality, they shall be handled in accordance with the provisions of the "Interim Measures for National Product Quality Arbitration Inspection". 5.7 The judgment of the test results shall be carried out according to the rounded value comparison method in GB1250, and the rounding shall be carried out according to GB8170. 6 Marking, packaging, transportation, storage
6.1 Marking
The packaging container shall be painted with a firm mark, which includes the manufacturer's name, product name, trademark, standard number, production date, grade mark, product gross net weight, as well as the toxic mark in GB190 and the marks such as afraid of moisture, handle with care, and afraid of heat in GB191. 6.2 Packaging
Industrial benzyl chloride shall be packaged in iron drums lined with polyethylene, or other suitable materials. 6.3 Transportation and storage
Industrial taro chloride should be stored in a cool and dry place; avoid rain, high temperature and fireworks during transportation. The validity period of this product is six months from the date of leaving the factory. 6
Additional instructions:
HG2027-91
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 technical jurisdiction of the Beijing Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Wuhan Organic Synthesis Chemical Plant and Jiangsu Lianyungang Chemical Plant. The main drafters of this standard are Wang Zhendong, Li Yun, Wang Zhulan, Yu Huaidao and Li Zhenrong. This standard refers to the Japanese Industrial Standard JISK4125-1983 "Taro Chloride". 75 If one of the indicators in the test results does not meet the requirements of this standard, samples should be taken from the packaging barrels with twice the amount for re-testing. If even one of the indicators in the re-test results does not meet the requirements of this standard, the entire batch of products shall be judged as unqualified. 5.6 When the supply and demand parties have objections to the product quality, they shall be handled in accordance with the provisions of the "Interim Measures for National Product Quality Arbitration Inspection". 5.7 The judgment of the test results shall be carried out according to the rounded value comparison method in GB1250, and the rounding shall be carried out according to GB8170. 6 Marking, packaging, transportation, storage
6.1 Marking
The packaging container shall be painted with a firm mark, which includes the manufacturer's name, product name, trademark, standard number, production date, grade mark, product gross net weight, as well as the toxic mark in GB190 and the marks such as afraid of moisture, handle with care, and afraid of heat in GB191. 6.2 Packaging
Industrial benzyl chloride shall be packaged in iron drums lined with polyethylene, or other suitable materials. 6.3 Transportation and storage
Industrial taro chloride should be stored in a cool and dry place; avoid rain, high temperature and fireworks during transportation. The validity period of this product is six months from the date of leaving the factory. 6
Additional instructions:
HG2027-91
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 technical jurisdiction of the Beijing Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Wuhan Organic Synthesis Chemical Plant and Jiangsu Lianyungang Chemical Plant. The main drafters of this standard are Wang Zhendong, Li Yun, Wang Zhulan, Yu Huaidao and Li Zhenrong. This standard refers to the Japanese Industrial Standard JISK4125-1983 "Taro Chloride". 7
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