Some standard content:
National Standard of the People's Republic of China
Liquid sulphur dioxide
Liquid sulphur dioxide
1 Content and scope of application
GB/T 3637-93
Replaces CB363783
This standard specifies the technical requirements, test methods, inspection rules, and requirements for marking, packaging, transportation, storage and safety of liquid sulphur dioxide.
This standard applies to liquid sulphur dioxide for industrial use. The product is mainly used for the manufacture of sulfites and as a raw material for organic synthesis industries such as nylon, dyes, and synthetic detergents. It can also be used as a refrigerant, preservative, etc. The molecular formula is: SO
Relative molecular mass: 64.06 (according to the international relative atomic mass in 1989) 2 Reference standards
GB602 Preparation of standard solutions for determination of impurities in chemical reagents GB603 Preparation of preparations and products used in test methods for chemical reagents GB 1250
Expression and determination methods of limit values GB/T 6283
GB6682
GB 7144
GB10478
GB12268
3 Technical requirements
Determination of water content in chemical products Karl Fischer method (general method) Specifications and test methods for water used in analytical laboratories Gas cylinder color marking
Technical conditions for liquefied gas railway tank cars
List of dangerous goods
Liquid sulfur dioxide should meet the following requirements: Standard
Sulfur dioxide (SO, %
Residue,
Water, for
Arsenic (As),
Superior quality
0.000 604
White or slightly yellow liquid
Qualified products
Note: 1) Liquid sulfur dioxide produced directly from sulfur as raw material should be tested. Under normal conditions, test every time. Approved by the State Administration of Technical Supervision on August 19, 1993 and implemented on July 1, 1994
4 Test method
GB/T 3637--93
Unless otherwise specified, the reagents and water used in this standard are analytically pure reagents and grade 3 water in accordance with GB6682. 4.1 Appearance
Determined by visual inspection.
4.2 Determination of sulfur dioxide content
4.2.1 Summary of method
This standard uses the method of deducting the total content of impurities (residue, water, arsenic) to calculate the content of liquid sulfur dioxide. 4.2.2 Expression of separation results
The liquid sulfur dioxide content (X,) expressed as mass percentage is calculated according to formula (1): X, - 100 - (X, + X, + X)-..
Where: X, is the mass percentage of water determined according to 4.3; X—the mass percentage of residue determined according to 4.4; X,—the mass percentage of arsenic determined according to 4.5. 4.3 Determination of moisture
4.3.1 Sampling
4.3.1.1 Sampling by steel cylinder arbitration method
a. Sampling from liquid sulfur dioxide steel cylinder:-.-(1)
Connect a 1L sampling steel cylinder to the sampling pipeline at the outlet of the liquid sulfur dioxide steel cylinder. The connection must not leak. Then open the valve and replace all the remaining gas in the small steel cylinder with oxidizing gas. Continue ventilation for about 10 minutes and then remove the steel cylinder. Install the removed steel cylinder with a right-angle elbow (see Figure 1). Before each sampling, place the angle elbow with a screw phase in an oven at 100-110℃ for drying.
Figure 1 Angle elbow
b. Sampling from tank truck filling line
When liquid sulfur dioxide is shipped by tank truck, sampling can be performed on the production filling line. The sampling device is installed as shown in Figure 2. GB/T 3637—93
[Return chlorine system negative pressure temporary
SO, Origin
Figure 2 Sampling pipeline connection diagram
BI,B,,Bs—operating valve; B.,B5—cylinder connector Figure 2 shows a sampling device from a tank truck to a small-capacity cylinder, which is composed of operating valves B, and B2.B., and cylinder connectors B, and B, are also connected to the pipeline. When the device is not working, valves B, B, and B, should be closed. When preparing to sample, connect the cylinder according to the line shown in Figure 2. Close the cylinder valves B, and B, before sampling. Then open valves B, B, and B, in turn to replace the residual gas in the pipe with sulfur dioxide from the tank truck, then close valve B, and then open cylinder B, B;. After about 20 minutes (you can see the white box or water outside the cylinder), close valves B and B according to the softness, open B to extract the remaining gas in the pipe, and then close valves B2, B, to remove the cylinder.
After the cylinder is removed, it should be fixed in a horizontal position and screwed with a right-angle elbow with a nut welded on it (see Figure 1). Before each sampling, place the right-angle elbow in an oven at 100-110℃ for drying.
4.3.1.2 Sampling with glass bottles
Open the mixing port of the steel cylinder or tank truck, release the residual gas on the sampling tube, and after venting for a few minutes, use a 500mL narrow-necked grinding glass bottle that has been dried to directly sample. When the sample fills the bottle, quickly cover it with a ground-mouth bottle cap to prevent the escape of carbon dioxide. 4.3.2 Specifications
4.3.2.1 Summary of methods
Same as Chapter 2 and Chapter 3 of GB/T 6283.
4.3.2.2 Reagents and materials
See GB/T 6283 Sections 4.1.4.3, 4.4.4.9, 4.11, and 4.12. 4.3-2.3 Apparatus
See GB/6283 Sections 5.1,
4.3.2. 4 Analysis steps
a. Calibration of Karl Fischer reagent
Perform the operation according to Article 6.2.1 of GB/T6283. b. Direct coulometric titration:
When using a moisture meter, add 25ml of methanol to the titration container, and use Karl Fischer reagent to titrate the trace water in methanol until the ammeter produces the same deflection as during calibration and remains unchanged for 1 minute as the end point (do not record the volume of Karl Fischer reagent consumed). In the fume hood, prepare a 100ml conical flask that has been dried to an accuracy of 0.1g, and then quickly weigh 40g of liquid sulfur dioxide (accurate to 1.0g). Immediately transfer it to the titration container and titrate to the end point with Karl Fischer reagent as described above.
Daytime method
G/T 3637-93
When using the moontime method, follow Article 6 of GB/T 6283 The determination method is the same as above. The solution is titrated until the color changes from yellow to amber. 4.3.3 Expression of analysis results
The water content (X,) expressed as a percentage of mass is calculated according to formula (2): VT
Xx0o × 100
Wherein: V-
The volume of the Karl Fischer reagent consumed when titrating the sample, 1.0 mg/mL; T——The water equivalent of the Karl Fischer reagent. mg/mL; K-The mass of the sample, K
4.3.4 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. 2
The absolute difference of the determination results is not more than 0.002% for superior products, not more than 0.002% for first-class products, and not more than 0.02% for qualified products. 4.4 Residue Determination of
4.4.1 Summary of the method
The sample is evaporated in a boiling water bath until the smell of sulfur monoxide disappears, then cooled in a desiccator and weighed. 4.4.2 Apparatus
4.4.2.1 Water bath.
4.4.2.2 100mL conical flask.
4.4.3 Analysis steps
In a fume hood, quickly weigh about 100g of the sample in a conical flask that has been weighed to a constant weight (weighing to 0.0001g), accurately add 1.0g, and place it in a boiling water bath to evaporate to dryness until no sulfur dioxide smell escapes. After steaming, wipe the external moisture of the conical flask with filter paper and place it in a desiccator to cool for 30 minutes. Weigh it to an accuracy of 0.0001g. 4.4.4 Analysis results
The residue content (X,) expressed as mass percentage is calculated according to formula (3): X,=
Where: mi
Frl 2
Mass of bottle plus residue + area
"Mass of empty bottle·g:
Mass of sample, g.
4.4-5 Allowable difference
The calculated mean of the parallel determination results is taken as the determination result.12
The absolute difference of the parallel determination results: the superior product is not more than 0.002%, the first-class product is not more than 0.002%, and the qualified product is not more than 0.02%.4.5 Determination of arsenic content
4.5.1 Summary of the method
In the hydrochloric acid medium, metallic zinc is reduced to arsenic hydrogen,The reaction of hydrogen iodide and mercuric bromide produces a brown arsenic spot, which is compared with the standard spot to determine the arsenic content.
4.5.2 Reagents and materials
4.5.2.1 Arsenic-free metallic zinc (GB2304). 4.5.2.2 Hydrochloric acid (B 622).
GB/T 3637-93
4.5.2.3 Potassium iodide (GB1272) solution: 150 g/L. 4.5.2.4 Stannous chloride (GB638) solution: 400 g/L. Dissolve 40 tin (GB638) chloride in 100 mL of hydrochloric acid with a concentration (HCl) of 9 mol/L.
4.5.2.5 Lead acetate (HG3074): 200 g/L solution. 4.5.2.6 Lead acetate cotton: Soak the absorbent cotton with the solution in 4.5.2.5, take it out and drain it, dry it at room temperature and store it in a sealed container. 4.5.2.7 Mercuric bromide test paper. Prepare according to GB603. 4.5.2.8 Arsenic standard solution (1 mL. Containing 10 pμg): Prepare according to GR 602 and dilute it 1 time for use. This solution should be prepared before use. 4.5.3 Instrument
Arsenic determination instrument, as shown in Figure 3:
HRBr+test paperbZxz.net
Rubber pad
Tube frequency head rescue diagram
HgBr distance
Degradation
Lead acetate cotton
No zinc reduction
Figure 3 Arsenic determination instrument
4.5.4 Analysis steps
4.5.4 .1 Preparation of standard color spots
Pick 0.0.20.0.40, 0.60:1.00ml of arsenic standard solution respectively and place it in the conical bottle of the determination instrument. Add 5ml of hydrochloric acid and 25ml of water, 5ml of potassium iodide solution and 2ml of tin oxide solution, shake well. Let it stand for 15min, add 2g of arsenic-free zinc particles, connect the instrument according to the instructions, place it in a dark place, and let the reaction proceed for 45min. Take out the mercuric bromide test paper and mark the corresponding arsenic disc. Soak it with molten paraffin and place it in a desiccator.
4.5.4.2 Determination
Determine the arsenic content in the conical bottle used for the determination of the residue (4.1). The following analysis steps are carried out according to 4.5.4.] from "add 6:1 hydrochloric acid" to "take out the bromide test paper". The obtained color spot is compared with the standard color spot to measure the arsenic mass. 4.5. 5 Expression of analysis results
Express the arsenic content (X,) in mass percentage. Calculate X, according to formula (4) - m × 10 #
The arsenic spot in the sample is equivalent to the content of the standard arsenic spot, μg: m—sample mass,.
5 Inspection rules
CB/T 3637- 93
5.1 Liquid sulfur monoxide should be inspected by the quality supervision and inspection department of the manufacturer to ensure that all product indicators meet the requirements of this standard.
5.2 Each batch of tank trucks or cylinders containing liquid sulfur oxide is accompanied by a quality certificate, which includes the name of the manufacturer, product name, batch number or production date, net weight or number of pieces, standard reminder number and product certificate. 5.3 Liquid sulfur diamine should be inspected in batches. The number of cylinders filled in a day is regarded as a batch, and the number of sampled cylinders is rounded up according to each batch. The number of cylinders is 5, and no less than 2 cylinders + tank trucks are required. Sampling is conducted on the basis of one tank truck as a batch. 5.4 The user has the right to accept the received sulfur dioxide in bulk according to this standard. 5.5 The rounded value comparison method specified in GH1250 shall be used to determine whether the test results meet this standard. When calculating the sulfur dioxide content in bulk, the mass percentages of residue, moisture and arsenic shall be the values before rounding. 5.6 The sampling of liquid sulfur dioxide is called sampling at the filling station, and can also be sampled at the exit of the cylinder or tank truck. 5.7 If any indicator of the test result does not meet the requirements of the technical standard, it shall be retested with twice the sampling volume. If any indicator does not meet the requirements of this standard, the whole batch of products shall be unqualified. 6 Marking, packaging, transportation and storage
6.1 The color marking of steel cylinders filled with sulfur dioxide is shown in No. 45 in Table 2 of Article 5.1 of GB7144. The surface paint color is silver-gray and has obvious black "liquid sulfur dioxide" words: the marking of tank trucks is shown in Article 10 of GB10478. The surface of the cylinder is painted with silver-gray and yellow annular color bands and has obvious blue "liquid sulfur dioxide" words. 6.2 Steel cylinders and tank trucks filled with sulfur dioxide must comply with the requirements of the national "Gas Cylinder Safety Supervision Regulations" and the requirements of the Dangerous Goods Transportation Regulations. 6.3 The amount and pressure of liquid sulfur dioxide filled in the cylinder or tank truck must comply with the gas cylinder safety supervision regulations and the filling amount of liquid sulfur dioxide shall not exceed the filling coefficient of 1.23 kg/. Calculated filling volume, 6.4 When the user returns the empty bottle or tank truck to the manufacturer, the cylinder or tank truck should have residual pressure according to relevant regulations, and it shall not be less than 0.005MPa 7 Safety requirements
7.1 Liquid sulfur monoxide is a highly corrosive and toxic liquefied gas. According to GB12268, the hazard number is 31008. The air in its production workshop [working place is allowed to have a limit concentration of 10m/m 7.2 Personnel engaged in sulfur dioxide operation should wear protective equipment and be equipped with filter-type gas masks on site. In the event of an accident, isolation gas masks, rubber work clothes and rubber gloves must be used. 7.3 Before sampling, the integrity of the sampling system must be checked, and the wind direction must be observed. Pay attention to the sulfur dioxide content in the surrounding air. The transfer of samples during inspection must be carried out in a ventilated kitchen.
7.4 When liquid sulfur monoxide splashes onto human skin and other parts, the injured part should be immediately rinsed with human water. In case of sulfur dioxide poisoning, the poisoned person should be immediately removed from the scene and placed in fresh air or sent to the hospital for emergency treatment. Additional remarks:
GB/T3637-93
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Research Institute of Nanjing Chemical Industry (Group) Company: This standard was issued by the Research Institute of Nanjing Chemical Industry (Group) Company. The main drafters of this standard are Chen Chunsong, Zhao Yifang, Zheng Jufen and Yang Jun. This standard adopts the Soviet standard F0T2918-79 (name 43 "Technical conditions for industrial liquid sulfur dioxide 31 Liquid sulfur monoxide shall be inspected by the quality supervision and inspection department of the manufacturer to ensure that all indicators of the product meet the requirements of this standard.
5.2 Each batch of tank trucks or cylinders containing liquid sulfur oxide shall be accompanied by a quality certificate, which includes the name of the manufacturer, product name, batch number or production date, product net weight or number of pieces, standard number and product certificate. 5.3 Liquid disulfur dioxide shall be inspected by batch. The number of cylinders filled in a day shall be regarded as a batch, and the number of sampled cylinders shall be calculated as 5 cylinders per batch, and the number of cylinders shall not be less than 1 tank truck. The sampling shall be conducted on the basis of one tank truck as a batch. 5.4 The user unit has the right to accept the received sulfur dioxide in accordance with this standard. 5.5 The rounded value comparison method specified in GH1250 shall be used to determine whether the inspection results meet this standard. When calculating the content of sulfur dioxide in the body, the mass percentages of residue, moisture and arsenic shall be taken as the values before rounding. 5.6 The sampling of liquid sulfur oxide is called sampling at the filling station, and can also be sampled at the exit of the cylinder or tank truck. 5.7 If even one indicator of the test result does not meet the requirements of the technical standard, a new test should be carried out with twice the sampling volume. If even one indicator does not meet the requirements of this standard, the whole batch of products shall be unqualified. 6 Marking, packaging, transportation and storage
6.1 The color marking of steel cylinders filled with sulfur dioxide is shown in No. 45 in Table 2 of Article 5.1 of GB7144. The surface paint color is silver-gray and has obvious black "liquid sulfur dioxide" words: the marking of tank trucks is shown in Article 10 of GB10478. The surface of the cylinder is painted with silver-gray and yellow annular color bands and has obvious blue "liquid sulfur dioxide" words. 6.2 Steel cylinders and tank trucks filled with sulfur dioxide must comply with the requirements of the national "Gas Cylinder Safety Supervision Regulations" and the requirements of the Dangerous Goods Transportation Regulations. 6.3 The amount and pressure of liquid sulfur dioxide filled in the cylinder or tank truck must comply with the gas cylinder safety supervision regulations and the filling amount of liquid sulfur dioxide shall not exceed the filling coefficient of 1.23 kg/. Calculated filling volume, 6.4 When the user returns the empty bottle or tank truck to the manufacturer, the cylinder or tank truck should have residual pressure according to relevant regulations, and it shall not be less than 0.005MPa 7 Safety requirements
7.1 Liquid sulfur monoxide is a highly corrosive and toxic liquefied gas. According to GB12268, the hazard number is 31008. The air in its production workshop [working place is allowed to have a limit concentration of 10m/m 7.2 Personnel engaged in sulfur dioxide operation should wear protective equipment and be equipped with filter-type gas masks on site. In the event of an accident, isolation gas masks, rubber work clothes and rubber gloves must be used. 7.3 Before sampling, the integrity of the sampling system must be checked, and the wind direction must be observed. Pay attention to the sulfur dioxide content in the surrounding air. The transfer of samples during inspection must be carried out in a ventilated kitchen.
7.4 When liquid sulfur monoxide splashes onto human skin and other parts, the injured part should be immediately rinsed with human water. In case of sulfur dioxide poisoning, the poisoned person should be immediately removed from the scene and placed in fresh air or sent to the hospital for emergency treatment. Additional remarks:
GB/T3637-93
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Research Institute of Nanjing Chemical Industry (Group) Company: This standard was issued by the Research Institute of Nanjing Chemical Industry (Group) Company. The main drafters of this standard are Chen Chunsong, Zhao Yifang, Zheng Jufen and Yang Jun. This standard adopts the Soviet standard F0T2918-79 (name 43 "Technical conditions for industrial liquid sulfur dioxide 31 Liquid sulfur monoxide shall be inspected by the quality supervision and inspection department of the manufacturer to ensure that all indicators of the product meet the requirements of this standard.
5.2 Each batch of tank trucks or cylinders containing liquid sulfur oxide shall be accompanied by a quality certificate, which includes the name of the manufacturer, product name, batch number or production date, product net weight or number of pieces, standard number and product certificate. 5.3 Liquid disulfur dioxide shall be inspected by batch. The number of cylinders filled in a day shall be regarded as a batch, and the number of sampled cylinders shall be calculated as 5 cylinders per batch, and the number of cylinders shall not be less than 1 tank truck. The sampling shall be conducted on the basis of one tank truck as a batch. 5.4 The user unit has the right to accept the received sulfur dioxide in accordance with this standard. 5.5 The rounded value comparison method specified in GH1250 shall be used to determine whether the inspection results meet this standard. When calculating the content of sulfur dioxide in the body, the mass percentages of residue, moisture and arsenic shall be taken as the values before rounding. 5.6 The sampling of liquid sulfur oxide is called sampling at the filling station, and can also be sampled at the exit of the cylinder or tank truck. 5.7 If even one indicator of the test result does not meet the requirements of the technical standard, a new test should be carried out with twice the sampling volume. If even one indicator does not meet the requirements of this standard, the whole batch of products shall be unqualified. 6 Marking, packaging, transportation and storage
6.1 The color marking of steel cylinders filled with sulfur dioxide is shown in No. 45 in Table 2 of Article 5.1 of GB7144. The surface paint color is silver-gray and has obvious black "liquid sulfur dioxide" words: the marking of tank trucks is shown in Article 10 of GB10478. The surface of the cylinder is painted with silver-gray and yellow annular color bands and has obvious blue "liquid sulfur dioxide" words. 6.2 Steel cylinders and tank trucks filled with sulfur dioxide must comply with the requirements of the national "Gas Cylinder Safety Supervision Regulations" and the requirements of the Dangerous Goods Transportation Regulations. 6.3 The amount and pressure of liquid sulfur dioxide filled in the cylinder or tank truck must comply with the gas cylinder safety supervision regulations and the filling amount of liquid sulfur dioxide shall not exceed the filling coefficient of 1.23 kg/. Calculated filling volume, 6.4 When the user returns the empty bottle or tank truck to the manufacturer, the cylinder or tank truck should have residual pressure according to relevant regulations, and it shall not be less than 0.005MPa 7 Safety requirements
7.1 Liquid sulfur monoxide is a highly corrosive and toxic liquefied gas. According to GB12268, the hazard number is 31008. The air in its production workshop [working place is allowed to have a limit concentration of 10m/m 7.2 Personnel engaged in sulfur dioxide operation should wear protective equipment and be equipped with filter-type gas masks on site. In the event of an accident, isolation gas masks, rubber work clothes and rubber gloves must be used. 7.3 Before sampling, the integrity of the sampling system must be checked, and the wind direction must be observed. Pay attention to the sulfur dioxide content in the surrounding air. The transfer of samples during inspection must be carried out in a ventilated kitchen.
7.4 When liquid sulfur monoxide splashes onto human skin and other parts, the injured part should be immediately rinsed with human water. In case of sulfur dioxide poisoning, the poisoned person should be immediately removed from the scene and placed in fresh air or sent to the hospital for emergency treatment. Additional remarks:
GB/T3637-93
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Research Institute of Nanjing Chemical Industry (Group) Company: This standard was issued by the Research Institute of Nanjing Chemical Industry (Group) Company. The main drafters of this standard are Chen Chunsong, Zhao Yifang, Zheng Jufen and Yang Jun. This standard adopts the Soviet standard F0T2918-79 (name 43 "Technical conditions for industrial liquid sulfur dioxide 3
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