Some standard content:
National Standard of the People's Republic of China
Chlorine
Subject content and scope of application
Chlorobenzene
Benzene
GB 2404—92
Replaces GB2404- 80
This standard specifies the technical requirements, test methods, inspection rules, marking, packaging, transportation, storage and other requirements for chlorobenzene. This standard applies to fluorobenzene obtained by oxidation and purification of benzene in the presence of ferric chloride. This product is mainly used in industries such as dyes, pesticides and organic synthesis.
Structural formula:
C
Molecular formula: C,H,Cl
Relative molecular mass: 112.56 (according to the 1989 international relative atomic mass) 2 Reference standards||tt ||GB190
GB191
GB3143
GB 6283
GB 6388
GB 6678
GB 9722
3 Technology Requirements
Dangerous goods packaging mark,
Package storage pictorial mark
Liquid chemical product forehead color measurement method (Hazen unit - platinum-diamond color number) Determination of moisture content in chemical products Karl Fischer method (general method) Transportation, packaging, receipt and delivery marks
General principles for sampling of chemical products
Chemical reagents
General principles for gas chromatography
Quality requirements of chlorobenzene Comply with the requirements of Table 1:
Table 1
Item
Appearance
Moisture content, %
Acidity (based on HSO.), %||tt ||Item
Guohao Technical Supervision Bureau 1992-0 6 - 2 9 approved 478
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Superior grade product
Indicator
First-class product
mark
qualified product
is a colorless or slightly yellow transparent liquid at 20℃ (its color must not be deeper than No. 40)
0.05
0.001
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0.10
0.001
0.15
0.001
1993-05-01 Implement
chlorobenzene content, %
benzene content, %\
difluorobenzene content, %
item
from
Note: 1) Benzene content includes all impurities before the benzene and chlorobenzene peaks. GB 2404-—92
Continued Table 1
Excellent products
99.8
0. 05
0. 15
2) The dichlorobenzene content includes dichlorobenzene, o-chlorotoluene and all other impurities after the oxygen benzene peak. 4 Test methods
4.1 Determination of appearance
Determine the color of chlorobenzene according to the provisions of GB3143. 4.2 Determination of moisture
4.2.1 Method principle
refers to
first-class product
99.5
0.15
0.35||tt| |Standard
Qualified product
99.0
0.20
0.65
This method uses water, iodine and dichloride in the presence of methanol and pyridine. Sulfur reacts quantitatively to quantitatively determine the moisture in chlorobenzene. 4.2.2 Instruments
Instrument and installation see GB6283.
4.2.3 Reagent
Karl Fischer reagent (preparation shall be carried out according to the provisions of GB6283 4.12) or Karl Fischer modified reagent (preparation please refer to Appendix A)
Trichloro Methane anhydrous methanol (3+1) mixed reagent. 4.2.4 Calibration of the titer of Karl Fischer reagent (or Karl Fischer modified reagent) 4. 2. 4. Determination of the mass (m) of 1 5 uL pure water. Use a 10 μL microsyringe to accurately draw 5 μL of pure water. Weigh the mass (accurate to 0.000 2g), repeat twice, and take the arithmetic mean as the mass of 5 μL pure water.
4.2.4.2 Blank test
Use a pipette to absorb 25mL of chloroform anhydrous methanol (3+1) mixed reagent into the reactor, cap the bottle stopper, turn on the power, and turn on the electromagnetic Stirrer, use Karl Fischer reagent or Karl Fischer modified reagent to titrate the trace amount of water in the solution, titrate until the ammeter pointer produces a large deflection and remains unchanged for 1 minute as the end point (do not record the volume of the consumed reagent, do not drain it solution). 4.2.4.3 Calibration
Add 5uL water into the reactor with 10μL microinjection, cap the bottle stopper, and continue to titrate with Karl Fisher reagent or Karl Fisher modified reagent until the ammeter pointer stays at the end point of the blank test position and keep it unchanged for 1 minute as the end point. Record the amount of Karl Fischer reagent V and drain the waste liquid.
4.2.4.4 Calculation of titer
The titer T of Karl Fischer reagent or Karl Fischer modified reagent is calculated according to formula (1): T=V
m| |tt|| In the formula: T—-The titer of Karl Fischer reagent·g/mL, the mass of 5 μL pure water, g:
V—The Karl Fischer reagent consumed during calibration or Volume of Karl Fischer's modified reagent, mL. Repeat twice and take the arithmetic mean as the titer of the reagent. The titer of the reagent is calibrated once a day.
4.2.5 Analysis steps
4.2.5.1 Blank test
Same as 4.2.4.2.
4.2.5.2 Determination of moisture in the sample
GB 2404-92
Use a 25mL pipette to absorb 25ml of the sample and inject it into the reactor (into the solution after the blank test), Continue to titrate with Karl Fischer reagent (or Karl Fischer modified reagent) under stirring until the ammeter pointer stays at the end point of the blank test titration and remains unchanged for 1 minute. bZxz.net
4.2.6 Calculation
The mass percentage of moisture in chlorobenzene is calculated according to formula (2): V,T
wv,i.1i×100
where: u-
Moisture mass percentage, %;
V, the amount of Karl Fischer reagent (or Karl Fischer modified reagent) used when titrating the sample one by one, mL; Vz—added to the sample Volume, mL
1.11---The approximate density of the sample at 20°C, g/mL, T—titer of Karl Fischer reagent or Karl Fischer modified reagent), g/mL. If the difference between the two parallel measurement results is not greater than 0.005%, the arithmetic mean shall be taken as the measurement result. (2)
Note: When measuring the water content in the sample, each time the trifluoromethane anhydrous methanol (3-1) mixed reagent is added as the sample solvent, it can only be measured twice, otherwise due to the solvent in the sample Insufficient dosage will advance the end point and cause measurement errors. 4.3 Determination of acidity
4.3.1 Reagent
Congo red indicator solution: 1g/L aqueous solution.
4.3.2 Analysis steps
Use a pipette to absorb 20mL of the sample into a 250mL Erlenmeyer flask with a ground stopper, add 50mL of freshly boiled and cooled distilled water, shake vigorously for 3 minutes, and let stand After stratification, add 2 drops of Congo red indicator solution. If the upper layer does not change blue, it is qualified, that is, the acid content (calculated as H2SO.) is below 0.001%.
4.4 Determination of the content of chlorobenzene, benzene and difluorobenzene 4.4.1 Fang Qu Summary
Determination is carried out by gas chromatography, the detector is a thermal conductivity detector, and the calculation method adopts calibrated area normalization Method and use microprocessor. 4.4.2 Instrument
Required.
Gas Chromatograph: The instrument used should comply with the provisions of Chapter 5 of GB9722. Microprocessor (or integrator).
b.
Detector: Thermal conductivity detector.
c.
d． Microsyringe: 1μL, 5μ or 10μl. 4.4.3 Test conditions
． Carrier gas and flow rate: Dry and purified hydrogen is used as the carrier gas, and its purity is above 99.8%; the post-column flow rate is 55~65 mL/minc
b.Chromatography column: stainless steel column or glass column with an inner diameter of 3mm or 4mm and a length of 2000mm. c. Stationary phase: Use alkali-treated 250~180um (60~80 mesh) 6201 red diatomite as the carrier. Place 100g 6201 red diatomite in a conical flask and soak it in methanol solution with 5 potassium hydroxide added. Keep airtight for one day and night. Then evaporate to nearly dryness on a water bath, transfer to Crystal III, and bake in an oven at 100°C for 1 hour, then raise the temperature to 120-130°C and bake for 4 hours, cool and set aside. The fixative is Polyethylene 2480
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GE 2404--92
Alcohol 20000. The mass ratio of Zhou Dingbo to the carrier It's 15:100. d.
e.
f.
Column temperature: 140℃ (actual temperature).
Vaporization chamber temperature: 200℃.
Detector temperature: 200℃.
Bridge current: 160~~180mA.
g.
h.
Input volume: 1μl, depending on the sensitivity of the instrument. The maximum injection volume should not exceed 10 μL, so that each impurity peak should be clearly recorded at the selected injection volume, and the main peak height (or after attenuation) should account for more than 70% of the full scale on the recorder. The separation degree of difficult-to-separate substances is R≥1.0.
The relative retention value r. of each component is shown in Table 2.
Table 2
group
benzene
cent
rat benzene
o-chlorotoluene
|tt||p-difluorobenzene
o-dichlorobenzene
retention value min
0.85
2.64
3.50
5.09| |tt||6.59
8.08
The operating conditions can be adjusted appropriately during operation according to the performance of the specific instrument. The relative quality correction factors of each component are shown in Table 3. Table 3
Components
xin
0.81
4.4.4 Coating method of fixative
rat benzene
1.00|| tt | 4.4.5 Packing of the chromatographic column
According to the provisions of 7.1.3 in (39722). The filling amount is about 6g/m. 4.4.6 Aging of the chromatographic column
Relative retention value r.5|| tt||0.32
1.00
1.33
1.93
2.50
3.06
p-dichlorobenzene
1. 06 | | tt | After the aging study, gradually cool down in the carrier gas flow to prevent the carrier from agglomerating. 4.4.7 Instrument attenuation ratio calibration method | .8.1 Injection
When the instrument is turned on for a certain period of time and all parameters reach the values ??specified in this standard, use a clean and dry microsyringe to inject samples. Chromatographic legend: Use standard samples according to the test conditions shown in 4.4.3. The chromatogram produced is as follows: 481
:bzse
|tt||4.4.8.2 Quantitative method
GB2404
3
92||tt ||9 retention time (min)
1-benzene, 2-chlorobenzene 3-o-chlorotoluene; 4-m-dichlorobenzene, 5 p-dichlorobenzene t6-o-dichlorobenzene||tt| |Measurement of peak area: carried out with a emblem processor. a.
Quantitative method: use the correction area normalization method. The correction factors of each component use the values ??given in Table 3, except for the components before the chlorobenzene peak. The correction b.
factors are all calculated using the correction factor of benzene, and the correction factors of the unknown components between the chlorobenzene peak and the m-dichlorobenzene peak are calculated using the correction factor of o-chlorotoluene. :
The mass percentage of each component is calculated according to formula (3): A· f.
Z(A..) ×(100 - w)
r||tt. ||In the formula: Peak area of ??i, mm\,
f—relative mass correction factor of component i, GB2404-92
w—moisture mass percentage measured in 4.2, %. Two parallel measurements. Requirements for difference in results:
Chlorobenzene: no more than 0.05%
Benzene: no more than 0.01%;
Dichlorobenzene: no more than 0.01%
5 inspection. Rules
5.1 Chlorobenzene shall be sampled and inspected by the quality inspection department. 5.2 The manufacturer shall ensure that all chlorobenzene shipped from the factory shall comply with the requirements of this standard, and shall be accompanied by a quality certificate in a fixed format. 5.3 The user shall comply with this standard. 5.4 The weight of each batch shall not exceed 60t. 5.5 Sampling:
5.5.1 For chlorobenzene shipped in tank trucks, take samples from the inlet on the top of the tank truck using a glass bottle with a lead bob (or place the bottle in a weighted cage). Place the loose mouth of the sampling bottle into the tank car and collect representative samples from top to bottom. 5.5.2 When transporting fluorobenzene in iron barrels, the number of sampling barrels selected should comply with the provisions of 6.6.1 in GB6678. The sample is made of a glass tube with a diameter of 20 mm and a whistle at one end. Insert it into the bottom of the barrel at a speed where the liquid level inside and outside the tube is equal. Press the mouth of the tube with your thumb and take it out. 5.5.3 Divide the sample: Combine the collected samples together, mix carefully, take out no less than 500mL of sample and put it into a clean, dry glass bottle with a ground stopper. A label should be attached to the bottle to indicate: manufacturer name, product name, grade, batch number and sample date for analysis. 5.5.4 If any indicator in the inspection results does not meet the requirements of this standard, resampling should be taken from the tank car (or double the number of barrels) for verification. If the verification results still do not meet the requirements of this standard, the entire batch of chlorobenzene cannot be accepted. 6 Marking, packaging, transportation and storage
6. 1 Packaging Fluorobenzene should be shipped in special tank trucks or iron drums. When packed in quick barrels, the net weight of each barrel is 200 kg. 6.2 Packaging containers should be painted with firm markings. The content includes: manufacturer name, product name, production date, batch, trademark, net weight, and the signs of Figure 5 in GB190 and Figures 1~5 in GB6388. When shipping the tanker, you can write it down on the delivery note and print the above items on kraft paper, put it in a plastic clip, and hang it firmly at a specific position on the truck. 6.3 This product is a second-level flammable liquid and is easily volatile. It should be stored in a no-fire area, isolated from fire sources, and prevented from being exposed to sunlight or stored in a place with high temperature.
6.4 Storage and transportation must comply with GB191 and the relevant regulations of my country’s railway department on the storage and transportation of dangerous goods. 483
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A1 reagent
GB 2404—92
Appendix A
Karl Fischer improvement Preparation of reagents
(supplement)
A1.1 Dry iodine: Place sublimated iodine in a sulfuric acid desiccator for more than 48 hours. A1.25A molecular sieve: particles with a diameter of 3~5mm, used as desiccant. Roast at 500°C for 2 hours before use and cool in a dryer equipped with molecular sieves. Used molecular sieves can be washed with water, dried, and roasted before use. A1.3 Anhydrous methanol (GB683), if the moisture content is greater than 0.05%, it needs to be processed as follows: Preparation of anhydrous methanol: Add about 50g of 5A molecular sieve A1.2 to 500mL of methanol, plug the bottle and place it Leave it overnight. When using, aspirate the supernatant.
A1.4 Anhydrous sodium iodide: After drying at 120℃, store in a sealed bottle. A1.5 Anhydrous sodium acetate.
A1.6 Sulfur dichloride: Prepared by compressing gas or using sodium bisulfite: Put the paste aqueous solution of sodium bisulfite in a branch flask, and drip concentrated sulfuric acid to generate sulfur dioxide. Sulfur dioxide needs to be dehydrated and dried. A2 device
See GB 6283.
Preparation of A3 Karl Fischer modified reagent
Place 63g dry iodine in a clean and dry 1L brown narrow-mouth bottle, add 600mL anhydrous methanol, 25g anhydrous sodium iodide and 85g anhydrous Sodium acetate, cork the bottle, and shake until all iodine is dissolved (Solution A). Pour sulfur dioxide into a stoppered bottle containing no less than 90 mL of anhydrous methanol and cooled with an ice-water bath, so that the concentration of sulfur dioxide is 256g/L (solution B).
Add 90mL of solution B (containing 23g of the dioxide bowl) or directly pass dry sulfur dioxide gas into solution A, then dilute to 1L with methanol, homogenize and place in a dark place for later use.
Additional notes:
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical jurisdiction of Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard is drafted by Tianjin Chemical Plant. The main drafters of this standard are Guo Zhiying, Chen Yaqing and Liu Penglan. This standard refers to the Japanese Industrial Standard JISK4102-83 "Industrial Chlorobenzene". 18.4
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