Some standard content:
National Standard of the People's Republic of China
Industrial hydrogen
Subject content and scope of application
GB/T3634-1995
Replaces GB363483
This standard specifies the technical requirements, test methods, inspection rules, packaging, marking, storage and transportation as well as safety requirements for industrial hydrogen. This standard applies to compressed and uncompressed industrial hydrogen produced by water electrolysis and salt electrolysis, which is mainly used for hydrogenation of petroleum and oils, manufacture of artificial gemstones and quartz glass, and metal cutting and refining. Molecular formula: H2
Relative molecular mass: 2.016 (according to the international relative atomic mass in 1991) 2 Reference standards
Dangerous goods packaging mark
GB 190
GB4962
GB 5099
Safety technical regulations for the use of hydrogen
Seamless steel gas cylinders
GB/T5832.2 Determination of trace moisture in gas Dew point method GB 7144
3 Technical requirements
Color marking of gas cylinders
The technical indicators of industrial hydrogen shall meet the requirements of Table 1. Table 1
Hydrogen purity, 102
Oxygen radical content, 10?
Nitrogen content, 102
Dew point (
Free water
mL/bottle
Note: (i) The purity and content in the table are expressed in volume fraction (V/V). (2) Hydrogen produced by water electrolysis does not require fluorine. Approved by the State Administration of Technical Supervision on December 20, 1995. Superior product
Conforms to inspection
Conforms to inspection
Conforms to inspection
Conforms to inspection
Conforms to inspection
Conforms to inspection
Implementation on August 1, 1996
4 Test method
4.1 Hydrogen purity
GB/T 3634--1995
Hydrogen purity is expressed in volume fraction and is calculated according to formula (1): =100 (Ten 2)
Where: worm - hydrogen purity (volume fraction), 10-2; - oxygen content (volume fraction), 10-2,
42 - nitrogen content (volume fraction), 10-2. 4.2 Determination of moisture
4.2.1 Determination of free water
Determine by inversion method. Invert the hydrogen bottle vertically for 10 minutes at room temperature, slightly open the bottle valve, and let water flow into a dry and clean container at a small flow rate. When hydrogen is sprayed out, Close the bottle valve immediately and measure the amount of water flowing out with a measuring cylinder. The first-class product has no free water, and the qualified product has a water content of no more than 100mL, which meets the standard requirements.
4.2.2 Determination of water vapor content
The water content of the superior product shall be determined according to GB/T5832.2. 4.3 Determination of oxygen (argon) and nitrogen
4.3.1 Method and principle
Use gas chromatography.
Use a chromatographic column to separate the components of the sample gas and use a thermal conductivity cell to detect Measure the content of each component. When the sample gas enters the thermal conductivity cell after being separated by the chromatographic column, due to the different thermal conductivity and content of each component, it will take away different amounts of heat from the thermistor and cause changes in its resistance. Therefore, the corresponding signal is immediately given at the output end of the measuring bridge, thereby determining the content of each component. 4.3.2 Instrument
A gas chromatograph is used, and the detection limit for oxygen and nitrogen should be less than 10×10-6. The installation and commissioning of the instrument shall be carried out in accordance with the instructions. Gas The schematic flow chart of the chromatograph is shown in Figure 1
Figure 1 Schematic flow chart of gas chromatography
1 Hydrogen carrier gas bottle; 2--pressure reducing valve 3-regulating valve: 4-~drying tube; 5--pressure gauge; 6-thermal conductivity cell; 7-injector; 8 chromatographic column; 9--flow meter; 10--measuring bridge: 11-recorder 4.3.3 Determination conditions
Detector: thermal conductivity cell;
Bridge current: 150~200mA;
GB/T 3634-1995
Carrier gas purity: pure hydrogen not less than 99.99×10-2; Carrier gas flow rate: about 40mL/min;
Injection volume: 1~5mL;
Chromatographic column: 1m long, 4mm inner diameter, filled with 0.25~0.40mm 5A molecular sieve and activated. The column temperature is room temperature. f.
4.3.4 Determination steps
4.3.4.1 Startup: Start the instrument according to the manual of the gas chromatograph. Turn on the carrier gas, fully replace the system, connect the instrument power supply, and adjust the various parts of the instrument to achieve the determination conditions. After the instrument is stable, it can be measured. 4.3.4.2 Calibration: Use a standard gas whose component content is close to the corresponding component content of the sample or use pure air as a standard sample, and use the standard gas as arbitration. When using air as the standard gas, use a 1mL fixed volume tube for injection, the signal is appropriately attenuated, and the corresponding oxygen and nitrogen peak areas are measured. When using the prepared standard gas, the peak height (or peak area) can be used. Repeat the injection twice, and the relative deviation is no more than 5%. Take the average value. 4.3.4.3 Determination: Directly inject the sample gas with a fixed volume tube. After injection, observe the appearance of the oxygen peak and nitrogen peak, and measure their peak areas respectively. Repeat the injection twice, and the relative deviation is no more than 5%. Take the average value. 4.3.5 Results and treatment
4.3.5.1 The content of the measured component in hydrogen is calculated according to formula (2): shan·
Wherein: Φ—the content of the measured component in the sample gas (volume fraction), 10-2; ,—the content of the measured component in the standard gas (volume fraction), 10-?; A;—the peak area of the measured component in the sample gas, mm2; A—the peak area of the measured component in the standard gas, mm. 4.3.5.2 The arithmetic mean of two parallel determinations is taken as the determination result, and the relative deviation of the parallel determinations shall not exceed 5%. 4.4 Determination of alkali
4.4.1 Method and principle
The phenolic acid colorimetric method is adopted.
(2)
The phenolic acid indicator is red in the pH range of 8.0 to 10.0 (in alkaline solution). Therefore, the alkali in hydrogen can show red when passing through a cotton plug filled with phenolic acid indicator, and thus it can be determined. 4.4.2 Reagents and materials
Ethanol (GB/T679): chemically pure,
Sodium hydroxide (GB/T629): chemically pure, 4g/L solution; b.
Phenolic indicator: 10g/L ethanol solution, dissolve 1g phenol in 70~~80.mL50% ethanol aqueous solution, then adjust to neutral with sodium hydroxide solution, and finally dilute to 100mL with distilled water; d. Absorbent cotton;
e. Distilled water.
4.4.3 Determination steps
The determination device is shown in Figure 2.
Insert 0.15~0.20g of absorbent cotton into the glass sampling tube with tweezers, and soak it with 20~~25 drops of 10g/L phenol indicator, and then immediately connect it to the determination device (the catheter port in the rubber stopper should be 2~~5mm away from the cotton stopper). Open the sample gas valve, pass the gas through the sampling tube at a gas speed of 100mL/min, measure with a wet flowmeter, and sample 2L. If the cotton plug does not turn red, the alkali content in the hydrogen meets the test. 127
GB/T3634—1995
Figure 2 Alkali and chlorine determination device
1·Hydrogen sample cylinder, 2--pressure reducing valve; 3: three-way piston; 4---sampling tube (9cm long, 2cm inner diameter); 5---wet flowmeter 4.5 Determination of chlorine
4.5.1 Method and principle
The bromine fluorescent yellow color development method is used.
When the chlorine in hydrogen passes through the cotton plug impregnated with bromine fluorescent yellow indicator, a chemical reaction occurs to generate tetrabromofluorescein, forming a red coloring layer, thereby determining the chlorine.
4.5.2 Reagents and materials
Potassium hydroxide (GB/T1919): 100g/L solution; Potassium bromide (GB/T649);
Potassium carbonate (GB/T1397),
Bromofluorescent yellow indicator: weigh 30g potassium bromide and 1g potassium carbonate and dissolve them in 100mL distilled water; dissolve 0.1g fluorescein sodium d.
salt in 1mL100g/L potassium hydroxide solution and mix the two solutions. e. Absorbent cotton;
f. Distilled water.
4.5.3 Determination steps
The determination device is shown in Figure 2.
Insert 0.15-0.20g of absorbent cotton in a glass sampling tube with tweezers, soak it with 20-25 drops of bromine fluorescent yellow indicator, and then immediately connect it to the measuring device (the catheter opening in the rubber stopper should be 2-5mm away from the cotton stopper). Open the sample gas valve, pass the gas through the sampling tube at a rate of 100mL/min, measure with a wet flow meter, and sample 1L. If the cotton stopper does not turn red, the alkali content in the hydrogen meets the test. 5 Inspection Rules
5.1 Industrial hydrogen shall be inspected by the technical supervision department of the manufacturer, and the industrial hydrogen leaving the factory shall be guaranteed to meet the requirements of this standard. 5.2 Bottled industrial hydrogen is sampled and inspected randomly according to the number of bottles specified in Table 2, and accepted in batches. When the inspection results show that one bottle does not meet the technical requirements of this standard, it shall be double sampled and inspected again. If there is still one bottle that does not meet the technical requirements of this standard, the batch of products shall be unqualified. Table 2 Number of samples of bottled industrial hydrogen
Number of bottled industrial hydrogen in each batch, bottle
Below 100
101~500
501～1000
Number of samples, bottle
GB/T3634—1995
5.3 Industrial hydrogen transported by pipeline shall be sampled and inspected once every 8 hours. When any of the indicators in the inspection results do not meet the requirements of this standard, the product shall be unqualified within the 8 hours.
5.4 Users shall also accept in accordance with the provisions of this standard. 5.5 When the supply and demand parties have different opinions on the quality of the product, both parties shall conduct joint inspection or submit it to arbitration. 6 Packaging, marking, storage and transportation
6.1 The packaging, marking, storage and transportation of hydrogen shall comply with the provisions of the "Regulations on Safety Supervision of Gas Cylinders". 6.2 Gas cylinders filled with hydrogen shall comply with the provisions of GB5099, and the color markings of gas cylinders shall comply with the provisions of GB7144. 6.3 The filling pressure of bottled hydrogen is 13.5±0.5MPa at 20℃. The pressure gauge used for measurement has an accuracy of Class 2.5 and a range of 0~25.0MPa.
6.4 The residual pressure of returned hydrogen cylinders shall not be less than 0.05MPa. Gas cylinders without residual pressure, gas cylinders after water pressure test, new gas cylinders, etc. must be heated, evacuated and replaced according to the specified requirements before filling. 6.5 Hydrogen should be accompanied by a quality certificate when leaving the factory, the contents of which include: product name;
manufacturer name;
production date or batch number;
product volume;
this standard code and grade.
6.6 The volume of hydrogen is calculated according to formula (3):
V = KV.
Where: V is the volume of bottled hydrogen at 0.1013MPa and 20°C, m; V is the water volume of the hydrogen bottle, L,
K is the coefficient for converting to the volume of hydrogen at 20°C and 0.1013MPa, which can be calculated or found in Appendix A (Supplement). 7 Safety requirements
7.1 The use of hydrogen should comply with the provisions of GB4962. 7.2 Hydrogen is a colorless, odorless, filmless, flammable and explosive gas. Its mixture with chlorine, oxygen, carbon monoxide and air is explosive. The explosion limit of hydrogen and air mixture is 4×10-2~75×10-2 (hydrogen), the explosion limit of hydrogen and oxygen mixture is 4×10-2~95×10-2 (hydrogen); the explosion limit of hydrogen and carbon monoxide mixture is 13.5×10-2~49×10-2 (hydrogen); when the mixing ratio of hydrogen and chlorine is 1:1, it can explode under light. Since the presence of hydrogen is not easy to be detected by the senses, the ignition energy of hydrogen is very small, and the explosion energy is very high, so strict attention should be paid during use and storage and transportation.
7.3 Hydrogen gathers indoors, and when its content reaches the explosion limit, there is a risk of explosion. In a hydrogen atmosphere, people are in danger of suffocation, so ventilation devices should be installed in places where the hydrogen content may increase. If necessary, a hydrogen alarm should be installed to monitor the hydrogen content. 7.4 Before inspecting or handling hydrogen pipelines, equipment, and gas cylinders, the hydrogen must be replaced with nitrogen to meet the fire regulations before work can begin. 7.5 There is a risk of fire when hydrogen leaks from the nozzle of the gas cylinder or is discharged quickly. Therefore, when bottled hydrogen leaves the factory, the bottle nozzle and bottle valve should be guaranteed to be leak-free, and the bottle cap should be tightened. Therefore, when using bottled hydrogen, the bottle valve should be opened slowly. 7.6 Bottled hydrogen should be stored in a place without open flames, away from heat sources, with good ventilation, away from oxidant gas cylinders and combustible materials. The construction, electrical, fire resistance, and explosion-proof requirements of hydrogen cylinder warehouses should comply with the provisions of relevant specifications. 7.7 During long-distance transportation, the hydrogen cylinder should be affixed with the specified mark in GB190. 129
GB/T3634-1995
Appendix A
Conversion factor K Calculation of the value
(Supplement)
At 20C, 0.1013MPa, the volume conversion coefficient K of hydrogen is calculated as follows: 10-3
3+1×:
Where: p——
Gas pressure in the cylinder, MPa;
Gas temperature in the cylinder, ℃;
When the temperature is t and the pressure is P, the compression coefficient of hydrogen. The K value of hydrogen at different temperatures and pressures is as follows: Temperature, (
Additional notes:
Force, MPa
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China and is under the jurisdiction of the Southwest Research Institute of Chemical Industry of the Ministry of Chemical Industry. This standard is drafted by the Guangming Chemical Research Institute of the Ministry of Chemical Industry and the Southwest Research Institute of Chemical Industry of the Ministry of Chemical Industry. The main drafters of this standard are Wang Xiguang and Duan Shufang. The superior products of this standard are equivalent to industrial hydrogen (Class 4) in JISK0512-74 "Hydrogen". 1307 For long-distance transportation, the hydrogen cylinder should be affixed with the designated mark in GB190. 129
GB/T3634-1995
Appendix A
Conversion factor K Calculation of the value
(Supplement)
At 20C, 0.1013MPa, the volume conversion coefficient K of hydrogen is calculated as follows: 10-3
3+1×:
Where: p——
Gas pressure in the cylinder, MPa;
Gas temperature in the cylinder, ℃;
When the temperature is t and the pressure is P, the compression coefficient of hydrogen. The K value of hydrogen at different temperatures and pressures is as follows: Temperature, (
Additional notes:
Force, MPa
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China and is under the jurisdiction of the Southwest Research Institute of Chemical Industry of the Ministry of Chemical Industry. This standard is drafted by the Guangming Chemical Research Institute of the Ministry of Chemical Industry and the Southwest Research Institute of Chemical Industry of the Ministry of Chemical Industry. The main drafters of this standard are Wang Xiguang and Duan Shufang. The superior products of this standard are equivalent to industrial hydrogen (Class 4) in JISK0512-74 "Hydrogen". 1307 For long-distance transportation, the hydrogen cylinder should be affixed with the designated mark in GB190. 129bzxZ.net
GB/T3634-1995
Appendix A
Conversion factor K Calculation of the value
(Supplement)
At 20C, 0.1013MPa, the volume conversion coefficient K of hydrogen is calculated as follows: 10-3
3+1×:
Where: p——
Gas pressure in the cylinder, MPa;
Gas temperature in the cylinder, ℃;
When the temperature is t and the pressure is P, the compression coefficient of hydrogen. The K value of hydrogen at different temperatures and pressures is as follows: Temperature, (
Additional notes:
Force, MPa
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China and is under the jurisdiction of the Southwest Research Institute of Chemical Industry of the Ministry of Chemical Industry. This standard is drafted by the Guangming Chemical Research Institute of the Ministry of Chemical Industry and the Southwest Research Institute of Chemical Industry of the Ministry of Chemical Industry. The main drafters of this standard are Wang Xiguang and Duan Shufang. The superior products of this standard are equivalent to industrial hydrogen (Class 4) in JISK0512-74 "Hydrogen". 130
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