This standard specifies the technical requirements, inspection methods, inspection rules, and packaging, marking, transportation, storage and safety requirements for hydrogen chloride. This standard applies to hydrogen chloride synthesized from hydrogen and chlorine as raw materials and bottled liquid hydrogen chloride purified from industrial hydrogen chloride as raw materials. Hydrogen chloride is mainly used in the electronics industry and is used in etching, passivation, epitaxy and other processes in the production of integrated circuits. It can also be used in metal smelting, optical communications and scientific research. GB/T 14602-1993 Gaseous hydrogen chloride for electronics industry GB/T14602-1993 Standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Gases for electronic industry-Hydrogen chloride
Gases for electronic industry-Hydrogen chloride1Subject content and scope of application
GB/T14602--93
This standard specifies the technical requirements, inspection methods, inspection rules, and packaging, marking, transportation, storage and safety requirements of hydrogen chloride. This standard applies to hydrogen chloride synthesized from hydrogen and chlorine as raw materials and bottled liquid hydrogen chloride purified from industrial hydrogen chloride as raw material. Hydrogen chloride is mainly used in the electronics industry and in etching, passivation, epitaxy and other processes in the production of integrated circuits. It can also be used in metal smelting, optical communication and scientific research.
Molecular formula: HCl
Relative molecular mass: 36.461 (according to the international relative atomic mass in 1989) 2 Reference standards
Dangerous goods packaging mark
GB4845
GB7144
GB7445
GB8984
3 Technical requirements
Ammonia test method
Gas cylinder color marking
Determination of carbon monoxide, carbon dioxide and methane in gas, gas chromatography The quality of hydrogen chloride shall meet the technical requirements in the following table. Item
Hydrogen chloride purity, 10-2
Carbon dioxide content, 10-6
Nitrogen content, 10-6
Oxygen + argon content, 10*6
Hydrocarbon content, 10~6
Water content, 10~6
Hydrogen content, 106
Note: ①This index is the gas quality index of bottled products, with a guarantee period of 6 months. ②The purity and content in the table are volume fractions. 4 Test method
4.1 Purity of hydrogen chloride
Approved by the State Bureau of Technical Supervision on August 26, 1993
Implementation on July 1, 1994
The purity of hydrogen chloride (V/V) shall be calculated according to formula (1): GB/T 14602-93
=100+++++)×10-4
Wu Zhong:
Purity of hydrogen chloride, 10-2;
9——Oxygen (containing fluorine) content, 106;
Nitrogen content, 106,
-Carbon dioxide content, 10;
Hydrocarbon content, 106;
9-Water content, 10°6;
9-Hydrogen content, 10 6.
4.2 Determination of oxygen (including ammonia) and nitrogen content
4.2.1 Principle of the method
(1)
Use gas chromatography and thermal conductivity detector for detection. First, pass the sample gas through a pre-separation column to separate hydrogen chloride from the component to be measured, and cut and back-blown the hydrogen chloride, and then pass through a chromatographic column to separate the oxygen and nitrogen in the component to be measured, and enter the detector for detection in turn. The oxygen and nitrogen content are proportional to the change in bridge resistance caused by the thermal conductivity detector. Oxygen and nitrogen are quantified in this way. 4.2.2 Instrument
Use a thermal conductivity chromatograph equipped with a cut and back-blown gas path. The instrument's minimum detection concentration for oxygen and nitrogen should meet the requirements of this standard. The schematic flow chart of the determination is shown in Figure A1 of Appendix A (reference). 4.2.3 Reference conditions for determination
Detector: thermal conductivity cell with cold resistance value of 120Ω; bridge current: 200mA;
Carrier gas purity: not less than 99.9999×10-2 hydrogen; carrier gas flow rate: 40mL/min;
Backflush gas purity: not less than 99.9999×10~2 hydrogen; backflush gas flow rate: 70mL/min;
Pre-separation column: stainless steel tube with a length of 800mm and an inner diameter of 4mm, filled with 0.2~0.3mm porapakQ, and the column temperature is room temperature; chromatographic column: stainless steel tube with a length of 900mm and an inner diameter of .4mm, filled with 0.4~0.5mm 13X molecular sieve, and the column temperature is 50℃; injection volume: 5mL.
4.2.4 Determination steps
4.2.4.1 Start: Start the instrument according to the instruction manual of the gas chromatograph. First turn on the carrier gas, adjust all parts of the instrument to meet the measurement conditions, then turn on the power of the thermal conductivity cell and wait for the instrument to work stably. 4.2.4.2 Blank: Follow the normal measurement method, and use blank injection to check the sealing of the gas system. 4.2.4.3 Replacement: Connect the sample gas to the chromatograph through the gas path, adjust valve 3 and valve 5, and use more than 20 times the pipeline volume of sample gas to fully replace the connecting basket channel and the injection tube to make the sample taken representative. 4.2.4.4 Injection: Turn valve 6 to allow the sample gas in the injection tube to enter the pre-separation column with the carrier gas, separate and cut off the hydrogen chloride in it, and then enter the chromatographic column with the carrier gas to separate the oxygen and nitrogen components to be measured, and then enter the detector for measurement in turn. 4.2.4.5 Cutting: After the injection, when oxygen and nitrogen completely flow out of the pre-separation column, synchronously rotate valve 9 and valve 8 to keep the hydrogen chloride in the pre-separation column. At the same time, back-blowing hydrogen through valve 9, pre-separation column and valve 8 to blow out the hydrogen chloride in the column. 4.2.4.6 Measurement: Record the chromatographic elution curves of oxygen and nitrogen, and measure the peak area A of each component respectively. 4.2.5 Calibration
a. Calibrate with standard gas prepared by heavy base method or exponential dilution method. The calibration method of exponential dilution method is shown in GB4845. b. Standard gas: Ultrapure hydrogen in accordance with GB7445 is used as the base gas. The oxygen and nitrogen content in it is not less than 0.5 times and the upper limit is not more than 2 times compared with the oxygen and nitrogen content in the sample to be tested. GB/T14602-93
c. Directly inject the standard gas and measure the peak area A of oxygen and nitrogen. 4.2.6 Calculation of results
4.2.6.1 The arithmetic mean of two parallel determinations is taken as the determination result, and the relative deviation of parallel determinations shall not exceed 20×10-. 4.2.6.2 The content of the measured component in hydrogen chloride is calculated according to formula (2): 9=·
Wherein: 9——the content of the measured component in the sample gas, 10-6 (V/V); g-—the content of the measured component in the standard gas, 10-6 (V/V); 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 Determination of carbon dioxide and hydrocarbon content
4.3.1 Principle of the method
Gas chromatography is used, and detection is carried out with a hydrogen flame ionization detector. First, the sample gas is passed through the chromatographic column to separate hydrogen chloride from the measured component, and the hydrogen chloride is cut and backblown out, and then the measured component is converted into methane, and then enters the detector for detection. 4.3.2 Instrument
A gas chromatograph equipped with a hydrogen flame ionization detector and a nickel catalyst conversion column shall be used, and the backflush gas path shall be installed and cut. The instrument's minimum detection concentration of methane shall comply with the requirements of this standard. The schematic flow chart of the measuring device is shown in Figure A2 of Appendix A (reference). 4.3.3 Reference conditions for measurement
Carrier gas (combustion gas): high-purity hydrogen, flow rate 40mL/min; b.
Combustion-supporting gas: air, flow rate 350mL/min; c.
Tail gas: high-purity nitrogen, flow rate 50ml./min, injection volume: 0.6mL;
Chromatographic column: a stainless steel tube with a length of 3m and an inner diameter of 4mm, filled with 0.2~0.3mm porapakQ, and the column temperature is room temperature; f.
Conversion column: a stainless steel tube with a length of 300mm and an inner diameter of 3mm, filled with 0.25~0.4mm nickel catalyst. Under the conditions of use, the conversion rate should not be less than 95×10-2, and the column temperature is 370±10℃. g.
Detector: hydrogen flame ionization detector. 4.3.4 Determination steps
4.3.4.1 Startup: Start the instrument according to the chromatograph instruction manual. First, turn on the carrier gas, tail gas and combustion-supporting gas, adjust the various parts of the instrument to meet the measurement conditions, then turn on the power of the instrument and wait for the recorder baseline to stabilize. 4.3.4.2 Replacement: Connect the sample gas to the instrument through the gas line, then adjust valve 4, and use more than 20 times the pipeline volume of sample gas to fully replace the connecting pipe and injection tube of the six-way valve to make the sample representative. 4.3.4.3 Injection: Turn valve 5 to allow the sample gas to enter the chromatographic column with the carrier gas, separate and cut off the hydrogen chloride, and then enter the conversion column to convert the measured component into methane, and then enter the detector for detection in turn. 4.3.4.4 Cutting: After injection, when the measured component has finished emitting peaks from the chromatographic column, turn valves 8 and 7 synchronously to keep the hydrogen chloride in the chromatographic column. At the same time, backflush hydrogen through valve 8, the chromatographic column, and valve 7 to blow away the hydrogen chloride and vent it. ：4.3.4.5 Measurement: Record the chromatographic elution curve of each component to be measured, and measure the peak area A respectively;. 4.3.5 Calibration
a. Calibrate with standard gas prepared by weight method or exponential dilution method. The calibration method of exponential dilution method is shown in GB4845. b. The standard gas is based on ultrapure hydrogen that meets the requirements of GB7445, and the carbon dioxide and methane content is not less than 0.5 times, the upper limit is not higher than 2 times. c. Directly inject the standard gas and determine the peak area As of carbon dioxide and methane. 4.3.6 Calculation of results
The results are calculated according to 4.2.6.
GB/T14602-93
The contents of carbon dioxide and hydrocarbons in hydrogen chloride are calculated according to formula (2). 4.4 Determination of water content
4.4.1 Principle of method
The Karl Fischer method is used. A certain volume of sample gas is passed through a freezer to freeze the water therein and separate it from the hydrogen chloride. Then, dry nitrogen is used to heat and thaw the frozen water through the freezer to vaporize it, and the frozen water is detected by the nitrogen in the Karl Fischer instrument. The ratio of the measured water volume to the sample gas volume is the water content.
4.4.2 Instrument
Use a CA-02 or other model of Karl Fischer tester, equipped with a glass freezer and freezing, heating and blowing gas path. The instrument has a detection sensitivity of 1 μg for water. For the schematic flow chart of the measuring device and the schematic diagram of the freezer structure, see Figure A3 and Figure A4 in Appendix A (reference).
4.4.3 Reference conditions for determination
Flow rate of hydrogen chloride: 400 mL/min;
Injection volume: 10 L;
Blowing gas: high-purity nitrogen, in which the water content is less than 1×10-s (V/V), flow rate 400 mL/min; c
Heating bath temperature: 25°C;
Cold bath temperature: -78°C;
f. Freezer: Made of a glass tube with a length of 500 mm and an inner diameter of 6×1 mm. 4.4.4 Determination steps
4.4.4.1 Background: First, adjust the flow rate of high-purity nitrogen to the specified value according to route 1-5---4-3, and then let it enter the Karl Fischer instrument for detection according to the replacement route. If the same volume of high-purity nitrogen is taken twice continuously, and the cumulative water content read by the instrument is equal, then the water content measured at this time is the high-purity nitrogen background value.
4.4.4.2 Replacement: Open valve 1, turn valves 5, 4, and 8, control the high-purity nitrogen to 400mL/min, and flow through the freezer to vent according to route 1-5-4-6-5-8-10-11 until the water content in the system drops to the background value. 4.4.4.3 Freezing: First, put a cold bath on the freezer, then open valve 2, and then turn valve 4 and valve 8 synchronously, control the hydrogen chloride flow rate to 400ml/min, and remove the tail gas according to route 2--4-6-5-8-9. Record the time and flow until the specified injection volume V, and multiply it with the background value to calculate the sample tail gas water volume m2.
4.4.4.4 Blowing off: Turn valve 4 to allow high-purity nitrogen to enter the freezer according to route 1-5-4--6--5-8-9, blow out the hydrogen chloride with more than 20 times the pipeline volume, and blow out the gas through valve 8 for tail gas treatment. 4.4.4.5 Injection: Turn valve 8 to control the high-purity nitrogen to enter the measuring instrument at a flow rate of 400mL/min along route 8-10-11, remove the cold bath, put on the hot bath, blow out until the water content of the blown gas remains unchanged, measure the blown water volume m2 in the blown gas, and record the blown gas volume at the same time, and multiply it with the background value to calculate the background water volume m1 of the blown gas.
4.4.5 Calculation of results
4.4.5.1 The arithmetic mean of two parallel determinations is taken as the determination result, and the relative deviation of parallel determinations shall not exceed 20×10-2. 4.4.5.2 The water content in hydrogen chloride is calculated according to formula (3): 9 = m= +mx 24
Wherein: 9g——water content in sample gas, 10-6 (V/V); m——blow-out water volume, μg;
ml—background water volume of blow-out gas, ug;
m2-water volume of sample tail gas·g;
V—sample gas injection volume, L.
4.5 Determination of hydrogen content
Carry out according to the provisions of 4.2. The carrier gas and calibration base gas are changed to 99.999×10-2 argon gas, and the bridge current is 100mA. (3)
5 Acceptance rules
GB/T 14602—93
5.1 The manufacturer shall inspect hydrogen chloride according to this standard, and the user shall have the right to inspect and accept according to this standard. When the two parties have any disagreement on the quality of the product, they shall negotiate and resolve it or submit it to arbitration.
5.2 Hydrogen chloride products shall be inspected bottle by bottle.
5.3 When all the sample inspection results meet the requirements of this standard, the bottle of product is a qualified product and can be accepted. 5.4 When any indicator of the sample inspection result does not meet the requirements of this standard, the bottle of product is an unqualified product and cannot be accepted. 5.5 The quantity of hydrogen chloride in the bottle is measured by weight. 6 Packaging, marking, transportation and storage
6.1 The paint color and marking of hydrogen chloride cylinders shall comply with the provisions of GB7144 and GB190. 6.2 The use, transportation and storage of hydrogen chloride cylinders shall comply with the "Regulations on Safety Supervision of Gas Cylinders" and the "Regulations on the Transportation of Dangerous Goods". 6.3 Hydrogen chloride products are packaged in stainless steel bottles or carbon steel bottles with treated inner walls. The volume of the gas cylinder can be determined according to the needs. The liquid volume of the filled product is filled according to the filling coefficient of 0.57kg/L, and the nominal working pressure of the gas cylinder shall not be less than 12.5MPa. 6.4 The gas cylinder shall be heated, evacuated and replaced before filling the product. 6.5 Hydrogen chloride gas cylinders shall be placed in a ventilated place, and the gas cylinders shall be placed vertically. It is strictly forbidden to place them horizontally. The bottle valve shall be closed tightly, and the bottle valve outlet shall be covered with a cap, and the bottle cap shall be screwed on.
6.6 Each bottle of hydrogen chloride leaving the factory shall be accompanied by a quality analysis report and a product certificate. The content of the certificate shall include: a. Product name;
Manufacturer name;
Production date;
d. Gas cylinder weight,
Product weight;
Standard number.
7 Safety requirements
7.1 Hydrogen chloride is a colorless, irritating gas. Its permissible limit of contact in the air is 5×10-°. If this limit is exceeded, it can cause coughing, pulmonary edema, and even life-threatening. Therefore, strict attention should be paid when producing and using hydrogen chloride, and corresponding protective measures should be taken. 7.2 When hydrogen chloride comes into contact with metal, it can react to generate chloride and hydrogen. Due to the generation of hydrogen, there is a potential risk of explosion and fire. Therefore, open flames and the storage of flammable and explosive items are strictly prohibited at the use and storage points. 7.3 When using bottled hydrogen chloride, a pressure reducer should be equipped to prevent the system from overpressure and explosion during use. After using the hydrogen chloride cylinder, the bottle valve should be closed in time and removed from the system to prevent accidents. 7.4 Before inspecting and handling hydrogen fluoride pipelines, equipment, and gas cylinders, the hydrogen chloride must be completely replaced and work can only start when it complies with safety regulations.
7.5 The pressure reducer, pipeline, valve and pipe fittings of the measuring device shall be made of stainless steel resistant to hydrogen chloride corrosion. 573
High-purity fluorine
Hydrogen purity, etc.
GB/T14602-93
Appendix A
Schematic diagram of gas flow and freezer structure
(reference)
Figure A1 Schematic diagram of thermal conductivity chromatography cutting gas flow chart Venting
1 Needle stop valve; 2 Rotor flowmeter; 3. Three-way valve; 4—-dilution bottle; 5, 6, 8, 9.-switching four-way valve; 7-fixed volume injection tube; 10·pre-separation column; 11--chromatographic column; 12 thermal conductivity detector ammonia gas
sample gas
Figure A2 Schematic flow chart of conversion hydrogen flame chromatography cutting gas path 1·needle valve; 2—-dilution bottle; 3-three-way valve; 4, 5, 7, 8—switching four-way valve; 6—fixed volume injection tube; 9 chromatographic column; 10—conversion column; 11 hydrogen flame detector Additional instructions ：
Sample tail gas treatment
GB/T1460293
Figure A3 Schematic diagram of Karl Fischer test device Pure gas-free
1, 2 Needle valve; 4, 5—Four-way valve; 6--Freezer; 7 Cold bath or hot bath; 8—Three-way valve; 3, 9 Rotor flowmeter; 10 Karl Fischer tester; 11 Wet flowmeter Figure A4 Schematic diagram of freezer structure
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 Southwest Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Guangming Chemical Research Institute of the Ministry of Chemical Industry. The drafter of this standard is Wang Xiguang.2 InstrumentsbZxz.net
A CA-02 or other type of Karl Fischer tester shall be used, equipped with a glass freezer and freezing, heating and blowing gas paths. The instrument shall have a water detection sensitivity of 1μg. See Figures A3 and A4 in Appendix A (reference) for the schematic flow chart of the test device and the schematic diagram of the freezer structure.
4.4.3 Reference conditions for determination
Flow rate of hydrogen chloride: 400mL/min;
Injection volume: 10L;
Blowing gas: high-purity nitrogen, in which the water content is less than 1×10-s (V/V), flow rate 400mL/min; c
Heating bath temperature: 25℃;
Cold bath temperature: -78℃;
f. Freezer: Made of a glass tube with a length of 500mm and an inner diameter of 6×1mm. 4.4.4 Determination steps
4.4.4.1 Background: First, adjust the flow rate of high-purity nitrogen to the specified value according to route 1-5---4-3, and then let it enter the Karl Fischer instrument for detection according to the replacement route. If the same volume of high-purity nitrogen is taken twice continuously, and the cumulative water content read by the instrument is equal, then the water content measured at this time is the high-purity nitrogen background value.
4.4.4.2 Replacement: Open valve 1, turn valves 5, 4, and 8, control the high-purity nitrogen to 400mL/min, and flow through the freezer to vent according to route 1-5-4-6-5-8-10-11 until the water content in the system drops to the background value. 4.4.4.3 Freezing: First, put a cold bath on the freezer, then open valve 2, and then turn valve 4 and valve 8 synchronously, control the hydrogen chloride flow rate to 400ml/min, and remove the tail gas according to route 2--4-6-5-8-9. Record the time and flow until the specified injection volume V, and multiply it with the background value to calculate the sample tail gas water volume m2.
4.4.4.4 Blowing off: Turn valve 4 to allow high-purity nitrogen to enter the freezer according to route 1-5-4--6--5-8-9, blow out the hydrogen chloride with more than 20 times the pipeline volume, and blow out the gas through valve 8 for tail gas treatment. 4.4.4.5 Injection: Turn valve 8 to control the high-purity nitrogen to enter the measuring instrument at a flow rate of 400mL/min along route 8-10-11, remove the cold bath, put on the hot bath, blow out until the water content of the blown gas remains unchanged, measure the blown water volume m2 in the blown gas, and record the blown gas volume at the same time, and multiply it with the background value to calculate the background water volume m1 of the blown gas.
4.4.5 Calculation of results
4.4.5.1 The arithmetic mean of two parallel determinations is taken as the determination result, and the relative deviation of parallel determinations shall not exceed 20×10-2. 4.4.5.2 The water content in hydrogen chloride is calculated according to formula (3): 9 = m= +mx 24
Wherein: 9g——water content in sample gas, 10-6 (V/V); m——blow-out water volume, μg;
ml—background water volume of blow-out gas, ug;
m2-water volume of sample tail gas·g;
V—sample gas injection volume, L.
4.5 Determination of hydrogen content
Carry out according to the provisions of 4.2. The carrier gas and calibration base gas are changed to 99.999×10-2 argon gas, and the bridge current is 100mA. (3)
5 Acceptance rules
GB/T 14602—93
5.1 The manufacturer shall inspect hydrogen chloride according to this standard, and the user shall have the right to inspect and accept according to this standard. When the two parties have any disagreement on the quality of the product, they shall negotiate and resolve it or submit it to arbitration.
5.2 Hydrogen chloride products shall be inspected bottle by bottle.
5.3 When all the sample inspection results meet the requirements of this standard, the bottle of product is a qualified product and can be accepted. 5.4 When any indicator of the sample inspection result does not meet the requirements of this standard, the bottle of product is an unqualified product and cannot be accepted. 5.5 The quantity of hydrogen chloride in the bottle is measured by weight. 6 Packaging, marking, transportation and storage
6.1 The paint color and marking of hydrogen chloride cylinders shall comply with the provisions of GB7144 and GB190. 6.2 The use, transportation and storage of hydrogen chloride cylinders shall comply with the "Regulations on Safety Supervision of Gas Cylinders" and the "Regulations on the Transportation of Dangerous Goods". 6.3 Hydrogen chloride products are packaged in stainless steel bottles or carbon steel bottles with treated inner walls. The volume of the gas cylinder can be determined according to the needs. The liquid volume of the filled product is filled according to the filling coefficient of 0.57kg/L, and the nominal working pressure of the gas cylinder shall not be less than 12.5MPa. 6.4 The gas cylinder shall be heated, evacuated and replaced before filling the product. 6.5 Hydrogen chloride gas cylinders shall be placed in a ventilated place, and the gas cylinders shall be placed vertically. It is strictly forbidden to place them horizontally. The bottle valve shall be closed tightly, and the bottle valve outlet shall be covered with a cap, and the bottle cap shall be screwed on.
6.6 Each bottle of hydrogen chloride leaving the factory shall be accompanied by a quality analysis report and a product certificate. The content of the certificate shall include: a. Product name;
Manufacturer name;
Production date;
d. Gas cylinder weight,
Product weight;
Standard number.
7 Safety requirements
7.1 Hydrogen chloride is a colorless, irritating gas. Its permissible limit of contact in the air is 5×10-°. If this limit is exceeded, it can cause coughing, pulmonary edema, and even life-threatening. Therefore, strict attention should be paid when producing and using hydrogen chloride, and corresponding protective measures should be taken. 7.2 When hydrogen chloride comes into contact with metal, it can react to generate chloride and hydrogen. Due to the generation of hydrogen, there is a potential risk of explosion and fire. Therefore, open flames and the storage of flammable and explosive items are strictly prohibited at the use and storage points. 7.3 When using bottled hydrogen chloride, a pressure reducer should be equipped to prevent the system from overpressure and explosion during use. After using the hydrogen chloride cylinder, the bottle valve should be closed in time and removed from the system to prevent accidents. 7.4 Before inspecting and handling hydrogen fluoride pipelines, equipment, and gas cylinders, the hydrogen chloride must be completely replaced and work can only start when it complies with safety regulations.
7.5 The pressure reducer, pipeline, valve and pipe fittings of the measuring device shall be made of stainless steel resistant to hydrogen chloride corrosion. 573
High-purity fluorine
Hydrogen purity, etc.
GB/T14602-93
Appendix A
Schematic diagram of gas flow and freezer structure
(reference)
Figure A1 Schematic diagram of thermal conductivity chromatography cutting gas flow chart Venting
1 Needle stop valve; 2 Rotor flowmeter; 3. Three-way valve; 4—-dilution bottle; 5, 6, 8, 9.-switching four-way valve; 7-fixed volume injection tube; 10·pre-separation column; 11--chromatographic column; 12 thermal conductivity detector ammonia gas
sample gas
Figure A2 Schematic flow chart of conversion hydrogen flame chromatography cutting gas path 1·needle valve; 2—-dilution bottle; 3-three-way valve; 4, 5, 7, 8—switching four-way valve; 6—fixed volume injection tube; 9 chromatographic column; 10—conversion column; 11 hydrogen flame detector Additional instructions ：
Sample tail gas treatment
GB/T1460293
Figure A3 Schematic diagram of Karl Fischer test device Pure gas-free
1, 2 Needle valve; 4, 5—Four-way valve; 6--Freezer; 7 Cold bath or hot bath; 8—Three-way valve; 3, 9 Rotor flowmeter; 10 Karl Fischer tester; 11 Wet flowmeter Figure A4 Schematic diagram of freezer structure
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 Southwest Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Guangming Chemical Research Institute of the Ministry of Chemical Industry. The drafter of this standard is Wang Xiguang.2 Instruments
A CA-02 or other type of Karl Fischer tester shall be used, equipped with a glass freezer and freezing, heating and blowing gas paths. The instrument shall have a water detection sensitivity of 1μg. See Figures A3 and A4 in Appendix A (reference) for the schematic flow chart of the test device and the schematic diagram of the freezer structure.
4.4.3 Reference conditions for determination
Flow rate of hydrogen chloride: 400mL/min;
Injection volume: 10L;
Blowing gas: high-purity nitrogen, in which the water content is less than 1×10-s (V/V), flow rate 400mL/min; c
Heating bath temperature: 25℃;
Cold bath temperature: -78℃;
f. Freezer: Made of a glass tube with a length of 500mm and an inner diameter of 6×1mm. 4.4.4 Determination steps
4.4.4.1 Background: First, adjust the flow rate of high-purity nitrogen to the specified value according to route 1-5---4-3, and then let it enter the Karl Fischer instrument for detection according to the replacement route. If the same volume of high-purity nitrogen is taken twice continuously, and the cumulative water content read by the instrument is equal, then the water content measured at this time is the high-purity nitrogen background value.
4.4.4.2 Replacement: Open valve 1, turn valves 5, 4, and 8, control the high-purity nitrogen to 400mL/min, and flow through the freezer to vent according to route 1-5-4-6-5-8-10-11 until the water content in the system drops to the background value. 4.4.4.3 Freezing: First, put a cold bath on the freezer, then open valve 2, and then turn valve 4 and valve 8 synchronously, control the hydrogen chloride flow rate to 400ml/min, and remove the tail gas according to route 2--4-6-5-8-9. Record the time and flow until the specified injection volume V, and multiply it with the background value to calculate the sample tail gas water volume m2.
4.4.4.4 Blowing off: Turn valve 4 to allow high-purity nitrogen to enter the freezer according to route 1-5-4--6--5-8-9, blow out the hydrogen chloride with more than 20 times the pipeline volume, and blow out the gas through valve 8 for tail gas treatment. 4.4.4.5 Injection: Turn valve 8 to control the high-purity nitrogen to enter the measuring instrument at a flow rate of 400mL/min along route 8-10-11, remove the cold bath, put on the hot bath, blow out until the water content of the blown gas remains unchanged, measure the blown water volume m2 in the blown gas, and record the blown gas volume at the same time, and multiply it with the background value to calculate the background water volume m1 of the blown gas.
4.4.5 Calculation of results
4.4.5.1 The arithmetic mean of two parallel determinations is taken as the determination result, and the relative deviation of parallel determinations shall not exceed 20×10-2. 4.4.5.2 The water content in hydrogen chloride is calculated according to formula (3): 9 = m= +mx 24
Wherein: 9g——water content in sample gas, 10-6 (V/V); m——blow-out water volume, μg;
ml—background water volume of blow-out gas, ug;
m2-water volume of sample tail gas·g;
V—sample gas injection volume, L.
4.5 Determination of hydrogen content
Carry out according to the provisions of 4.2. The carrier gas and calibration base gas are changed to 99.999×10-2 argon gas, and the bridge current is 100mA. (3)
5 Acceptance rules
GB/T 14602—93
5.1 The manufacturer shall inspect hydrogen chloride according to this standard, and the user shall have the right to inspect and accept according to this standard. When the two parties have any disagreement on the quality of the product, they shall negotiate and resolve it or submit it to arbitration.
5.2 Hydrogen chloride products shall be inspected bottle by bottle.
5.3 When all the sample inspection results meet the requirements of this standard, the bottle of product is a qualified product and can be accepted. 5.4 When any indicator of the sample inspection result does not meet the requirements of this standard, the bottle of product is an unqualified product and cannot be accepted. 5.5 The quantity of hydrogen chloride in the bottle is measured by weight. 6 Packaging, marking, transportation and storage
6.1 The paint color and marking of hydrogen chloride cylinders shall comply with the provisions of GB7144 and GB190. 6.2 The use, transportation and storage of hydrogen chloride cylinders shall comply with the "Regulations on Safety Supervision of Gas Cylinders" and the "Regulations on the Transportation of Dangerous Goods". 6.3 Hydrogen chloride products are packaged in stainless steel bottles or carbon steel bottles with treated inner walls. The volume of the gas cylinder can be determined according to the needs. The liquid volume of the filled product is filled according to the filling coefficient of 0.57kg/L, and the nominal working pressure of the gas cylinder shall not be less than 12.5MPa. 6.4 The gas cylinder shall be heated, evacuated and replaced before filling the product. 6.5 Hydrogen chloride gas cylinders shall be placed in a ventilated place, and the gas cylinders shall be placed vertically. It is strictly forbidden to place them horizontally. The bottle valve shall be closed tightly, and the bottle valve outlet shall be covered with a cap, and the bottle cap shall be screwed on.
6.6 Each bottle of hydrogen chloride leaving the factory shall be accompanied by a quality analysis report and a product certificate. The content of the certificate shall include: a. Product name;
Manufacturer name;
Production date;
d. Gas cylinder weight,
Product weight;
Standard number.
7 Safety requirements
7.1 Hydrogen chloride is a colorless, irritating gas. Its permissible limit of contact in the air is 5×10-°. If this limit is exceeded, it can cause coughing, pulmonary edema, and even life-threatening. Therefore, strict attention should be paid when producing and using hydrogen chloride, and corresponding protective measures should be taken. 7.2 When hydrogen chloride comes into contact with metal, it can react to generate chloride and hydrogen. Due to the generation of hydrogen, there is a potential risk of explosion and fire. Therefore, open flames and the storage of flammable and explosive items are strictly prohibited at the use and storage points. 7.3 When using bottled hydrogen chloride, a pressure reducer should be equipped to prevent the system from overpressure and explosion during use. After using the hydrogen chloride cylinder, the bottle valve should be closed in time and removed from the system to prevent accidents. 7.4 Before inspecting and handling hydrogen fluoride pipelines, equipment, and gas cylinders, the hydrogen chloride must be completely replaced and work can only start when it complies with safety regulations.
7.5 The pressure reducer, pipeline, valve and pipe fittings of the measuring device shall be made of stainless steel resistant to hydrogen chloride corrosion. 573
High-purity fluorine
Hydrogen purity, etc.
GB/T14602-93
Appendix A
Schematic diagram of gas flow and freezer structure
(reference)
Figure A1 Schematic diagram of thermal conductivity chromatography cutting gas flow chart Venting
1 Needle stop valve; 2 Rotor flowmeter; 3. Three-way valve; 4—-dilution bottle; 5, 6, 8, 9.-switching four-way valve; 7-fixed volume injection tube; 10·pre-separation column; 11--chromatographic column; 12 thermal conductivity detector ammonia gas
sample gas
Figure A2 Schematic flow chart of conversion hydrogen flame chromatography cutting gas path 1·needle valve; 2—-dilution bottle; 3-three-way valve; 4, 5, 7, 8—switching four-way valve; 6—fixed volume injection tube; 9 chromatographic column; 10—conversion column; 11 hydrogen flame detector Additional instructions ：
Sample tail gas treatment
GB/T1460293
Figure A3 Schematic diagram of Karl Fischer test device Pure gas-free
1, 2 Needle valve; 4, 5—Four-way valve; 6--Freezer; 7 Cold bath or hot bath; 8—Three-way valve; 3, 9 Rotor flowmeter; 10 Karl Fischer tester; 11 Wet flowmeter Figure A4 Schematic diagram of freezer structure
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 Southwest Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Guangming Chemical Research Institute of the Ministry of Chemical Industry. The drafter of this standard is Wang Xiguang.3 Freezing: First, put a cold bath on the freezer, then open valve 2, and then turn valve 4 and valve 8 synchronously, control the hydrogen chloride flow rate to 400ml/min, and remove the tail gas according to route 2--4-6-5-8-9. Record the time and flow until the specified injection volume V, and multiply it with the background value to calculate the sample tail gas water volume m2.
4.4.4.4 Blowing off: Turn valve 4 to allow high-purity nitrogen to enter the freezer according to route 1-5-4--6--5-8-9, blow out the hydrogen chloride with more than 20 times the pipeline volume, and blow out the gas through valve 8 to remove the tail gas. 4.4.4.5 Injection: Turn valve 8 to control the high-purity nitrogen to enter the measuring instrument at a flow rate of 400mL/min along route 8-10-11, remove the cold bath, put on the hot bath, blow out until the water content of the blown gas remains unchanged, measure the blown water volume m2 in the blown gas, and record the blown gas volume at the same time, and multiply it with the background value to calculate the background water volume m1 of the blown gas.
4.4.5 Calculation of results
4.4.5.1 The arithmetic mean of two parallel determinations is taken as the determination result, and the relative deviation of parallel determinations shall not exceed 20×10-2. 4.4.5.2 The water content in hydrogen chloride is calculated according to formula (3): 9 = m= +mx 24
Wherein: 9g——water content in sample gas, 10-6 (V/V); m——blow-out water volume, μg;
ml—background water volume of blow-out gas, ug;
m2-water volume of sample tail gas·g;
V—sample gas injection volume, L.
4.5 Determination of hydrogen content
Carry out according to the provisions of 4.2. The carrier gas and calibration base gas are changed to 99.999×10-2 argon gas, and the bridge current is 100mA. (3)
5 Acceptance rules
GB/T 14602—93
5.1 The manufacturer shall inspect hydrogen chloride according to this standard, and the user shall have the right to inspect and accept according to this standard. When the two parties have any disagreement on the quality of the product, they shall negotiate and resolve it or submit it to arbitration.
5.2 Hydrogen chloride products shall be inspected bottle by bottle.
5.3 When all the sample inspection results meet the requirements of this standard, the bottle of product is a qualified product and can be accepted. 5.4 When any indicator of the sample inspection result does not meet the requirements of this standard, the bottle of product is an unqualified product and cannot be accepted. 5.5 The quantity of hydrogen chloride in the bottle is measured by weight. 6 Packaging, marking, transportation and storage
6.1 The paint color and marking of hydrogen chloride cylinders shall comply with the provisions of GB7144 and GB190. 6.2 The use, transportation and storage of hydrogen chloride cylinders shall comply with the "Regulations on Safety Supervision of Gas Cylinders" and the "Regulations on the Transportation of Dangerous Goods". 6.3 Hydrogen chloride products are packaged in stainless steel bottles or carbon steel bottles with treated inner walls. The volume of the gas cylinder can be determined according to the needs. The liquid volume of the filled product is filled according to the filling coefficient of 0.57kg/L, and the nominal working pressure of the gas cylinder shall not be less than 12.5MPa. 6.4 The gas cylinder shall be heated, evacuated and replaced before filling the product. 6.5 Hydrogen chloride gas cylinders shall be placed in a ventilated place, and the gas cylinders shall be placed vertically. It is strictly forbidden to place them horizontally. The bottle valve shall be closed tightly, and the bottle valve outlet shall be covered with a cap, and the bottle cap shall be screwed on.
6.6 Each bottle of hydrogen chloride leaving the factory shall be accompanied by a quality analysis report and a product certificate. The content of the certificate shall include: a. Product name;
Manufacturer name;
Production date;
d. Gas cylinder weight,
Product weight;
Standard number.
7 Safety requirements
7.1 Hydrogen chloride is a colorless, irritating gas. Its permissible limit of contact in the air is 5×10-°. If this limit is exceeded, it can cause coughing, pulmonary edema, and even life-threatening. Therefore, strict attention should be paid when producing and using hydrogen chloride, and corresponding protective measures should be taken. 7.2 When hydrogen chloride comes into contact with metal, it can react to generate chloride and hydrogen. Due to the generation of hydrogen, there is a potential risk of explosion and fire. Therefore, open flames and the storage of flammable and explosive items are strictly prohibited at the use and storage points. 7.3 When using bottled hydrogen chloride, a pressure reducer should be equipped to prevent the system from overpressure and explosion during use. After using the hydrogen chloride cylinder, the bottle valve should be closed in time and removed from the system to prevent accidents. 7.4 Before inspecting and handling hydrogen fluoride pipelines, equipment, and gas cylinders, the hydrogen chloride must be completely replaced and work can only start when it complies with safety regulations.
7.5 The pressure reducer, pipeline, valve and pipe fittings of the measuring device shall be made of stainless steel resistant to hydrogen chloride corrosion. 573
High-purity fluorine
Hydrogen purity, etc.
GB/T14602-93
Appendix A
Schematic diagram of gas flow and freezer structure
(reference)
Figure A1 Schematic diagram of thermal conductivity chromatography cutting gas flow chart Venting
1 Needle stop valve; 2 Rotor flowmeter; 3. Three-way valve; 4—-dilution bottle; 5, 6, 8, 9.-switching four-way valve; 7-fixed volume injection tube; 10·pre-separation column; 11--chromatographic column; 12 thermal conductivity detector ammonia gas
sample gas
Figure A2 Schematic flow chart of conversion hydrogen flame chromatography cutting gas path 1·needle valve; 2—-dilution bottle; 3-three-way valve; 4, 5, 7, 8—switching four-way valve; 6—fixed volume injection tube; 9 chromatographic column; 10—conversion column; 11 hydrogen flame detector Additional instructions ：
Sample tail gas treatment
GB/T1460293
Figure A3 Schematic diagram of Karl Fischer test device Pure gas-free
1, 2 Needle valve; 4, 5—Four-way valve; 6--Freezer; 7 Cold bath or hot bath; 8—Three-way valve; 3, 9 Rotor flowmeter; 10 Karl Fischer tester; 11 Wet flowmeter Figure A4 Schematic diagram of freezer structure
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 Southwest Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Guangming Chemical Research Institute of the Ministry of Chemical Industry. The drafter of this standard is Wang Xiguang.3 Freezing: First, put a cold bath on the freezer, then open valve 2, and then turn valve 4 and valve 8 synchronously, control the hydrogen chloride flow rate to 400ml/min, and remove the tail gas according to route 2--4-6-5-8-9. Record the time and flow until the specified injection volume V, and multiply it with the background value to calculate the sample tail gas water volume m2.
4.4.4.4 Blowing off: Turn valve 4 to allow high-purity nitrogen to enter the freezer according to route 1-5-4--6--5-8-9, blow out the hydrogen chloride with more than 20 times the pipeline volume, and blow out the gas through valve 8 to remove the tail gas. 4.4.4.5 Injection: Turn valve 8 to control the high-purity nitrogen to enter the measuring instrument at a flow rate of 400mL/min along route 8-10-11, remove the cold bath, put on the hot bath, blow out until the water content of the blown gas remains unchanged, measure the blown water volume m2 in the blown gas, and record the blown gas volume at the same time, and multiply it with the background value to calculate the background water volume m1 of the blown gas.
4.4.5 Calculation of results
4.4.5.1 The arithmetic mean of two parallel determinations is taken as the determination result, and the relative deviation of parallel determinations shall not exceed 20×10-2. 4.4.5.2 The water content in hydrogen chloride is calculated according to formula (3): 9 = m= +mx 24
Wherein: 9g——water content in sample gas, 10-6 (V/V); m——blow-out water volume, μg;
ml—background water volume of blow-out gas, ug;
m2-water volume of sample tail gas·g;
V—sample gas injection volume, L.
4.5 Determination of hydrogen content
Carry out according to the provisions of 4.2. The carrier gas and calibration base gas are changed to 99.999×10-2 argon gas, and the bridge current is 100mA. (3)
5 Acceptance rules
GB/T 14602—93
5.1 The manufacturer shall inspect hydrogen chloride according to this standard, and the user shall have the right to inspect and accept according to this standard. When the two parties have any disagreement on the quality of the product, they shall negotiate and resolve it or submit it to arbitration.
5.2 Hydrogen chloride products shall be inspected bottle by bottle.
5.3 When all the sample inspection results meet the requirements of this standard, the bottle of product is a qualified product and can be accepted. 5.4 When any indicator of the sample inspection result does not meet the requirements of this standard, the bottle of product is an unqualified product and cannot be accepted. 5.5 The quantity of hydrogen chloride in the bottle is measured by weight. 6 Packaging, marking, transportation and storage
6.1 The paint color and marking of hydrogen chloride cylinders shall comply with the provisions of GB7144 and GB190. 6.2 The use, transportation and storage of hydrogen chloride cylinders shall comply with the "Regulations on Safety Supervision of Gas Cylinders" and the "Regulations on the Transportation of Dangerous Goods". 6.3 Hydrogen chloride products are packaged in stainless steel bottles or carbon steel bottles with treated inner walls. The volume of the gas cylinder can be determined according to the needs. The liquid volume of the filled product is filled according to the filling coefficient of 0.57kg/L, and the nominal working pressure of the gas cylinder shall not be less than 12.5MPa. 6.4 The gas cylinder shall be heated, evacuated and replaced before filling the product. 6.5 Hydrogen chloride gas cylinders shall be placed in a ventilated place, and the gas cylinders shall be placed vertically. It is strictly forbidden to place them horizontally. The bottle valve shall be closed tightly, and the bottle valve outlet shall be covered with a cap, and the bottle cap shall be screwed on.
6.6 Each bottle of hydrogen chloride leaving the factory shall be accompanied by a quality analysis report and a product certificate. The content of the certificate shall include: a. Product name;
Manufacturer name;
Production date;
d. Gas cylinder weight,
Product weight;
Standard number.
7 Safety requirements
7.1 Hydrogen chloride is a colorless, irritating gas. Its permissible limit of contact in the air is 5×10-°. If this limit is exceeded, it can cause coughing, pulmonary edema, and even life-threatening. Therefore, strict attention should be paid when producing and using hydrogen chloride, and corresponding protective measures should be taken. 7.2 When hydrogen chloride comes into contact with metal, it can react to generate chloride and hydrogen. Due to the generation of hydrogen, there is a potential risk of explosion and fire. Therefore, open flames and the storage of flammable and explosive items are strictly prohibited at the use and storage points. 7.3 When using bottled hydrogen chloride, a pressure reducer should be equipped to prevent the system from overpressure and explosion during use. After using the hydrogen chloride cylinder, the bottle valve should be closed in time and removed from the system to prevent accidents. 7.4 Before inspecting and handling hydrogen fluoride pipelines, equipment, and gas cylinders, the hydrogen chloride must be completely replaced and work can only start when it complies with safety regulations.
7.5 The pressure reducer, pipeline, valve and pipe fittings of the measuring device shall be made of stainless steel resistant to hydrogen chloride corrosion. 573
High-purity fluorine
Hydrogen purity, etc.
GB/T14602-93
Appendix A
Schematic diagram of gas flow and freezer structure
(reference)
Figure A1 Schematic diagram of thermal conductivity chromatography cutting gas flow chart Venting
1 Needle stop valve; 2 Rotor flowmeter; 3. Three-way valve; 4—-dilution bottle; 5, 6, 8, 9.-switching four-way valve; 7-fixed volume injection tube; 10·pre-separation column; 11--chromatographic column; 12 thermal conductivity detector ammonia gas
sample gas
Figure A2 Schematic flow chart of conversion hydrogen flame chromatography cutting gas path 1·needle valve; 2—-dilution bottle; 3-three-way valve; 4, 5, 7, 8—switching four-way valve; 6—fixed volume injection tube; 9 chromatographic column; 10—conversion column; 11 hydrogen flame detector Additional instructions ：
Sample tail gas treatment
GB/T1460293
Figure A3 Schematic diagram of Karl Fischer test device Pure gas-free
1, 2 Needle valve; 4, 5—Four-way valve; 6--Freezer; 7 Cold bath or hot bath; 8—Three-way valve; 3, 9 Rotor flowmeter; 10 Karl Fischer tester; 11 Wet flowmeter Figure A4 Schematic diagram of freezer structure
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 Southwest Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Guangming Chemical Research Institute of the Ministry of Chemical Industry. The drafter of this standard is Wang Xiguang.6 Each bottle of hydrogen chloride leaving the factory should be accompanied by a quality analysis report and a product certificate. The contents of the certificate should include: a. Product name;
Manufacturer name;
Production date;
d. Cylinder weight,
Product weight;
Standard number.
7 Safety requirements
7.1 Hydrogen chloride is a colorless, irritating gas. Its permissible limit of contact with air is 5×10-°. If this limit is exceeded, it can cause coughing, pulmonary edema, and even life-threatening. Therefore, strict attention should be paid when producing and using hydrogen chloride, and corresponding protective measures should be taken. 7.2 When hydrogen chloride comes into contact with metal, it can react to generate chloride and hydrogen. Due to the generation of hydrogen, there is a potential risk of explosion and fire. Therefore, it is strictly prohibited to have open flames and store flammable and explosive items at the use and storage points. 7.3 When using bottled hydrogen chloride, a pressure reducer should be equipped to prevent the system from overpressure and explosion during use. After using the hydrogen chloride cylinder, the bottle valve should be closed in time and removed from the system to prevent accidents. 7.4 Before inspecting and handling hydrogen fluoride pipelines, equipment, and cylinders, the hydrogen chloride must be completely replaced and work can only begin in accordance with safety regulations.
7.5 The pressure reducer, pipeline, valve and pipe fittings of the measuring device should be made of stainless steel resistant to hydrogen chloride corrosion. 573
High-purity fluorine
Hydrogen purity, etc.
GB/T14602—93
Appendix A
Schematic diagram of gas flow and freezer structure
(reference)
Figure A1 Schematic diagram of thermal conductivity chromatography cutting gas flow chart Venting
1 Needle stop valve; 2 Rotor flowmeter; 3. Three-way valve; 4—-dilution bottle; 5, 6, 8, 9.-switching four-way valve; 7-fixed volume injection tube; 10·pre-separation column; 11--chromatographic column; 12 thermal conductivity detector ammonia gas
sample gas
Figure A2 Schematic flow chart of conversion hydrogen flame chromatography cutting gas path 1·needle valve; 2—-dilution bottle; 3-three-way valve; 4, 5, 7, 8—switching four-way valve; 6—fixed volume injection tube; 9 chromatographic column; 10—conversion column; 11 hydrogen flame detector Additional instructions ：
Sample tail gas treatment
GB/T1460293
Figure A3 Schematic diagram of Karl Fischer test device Pure gas-free
1, 2 Needle valve; 4, 5—Four-way valve; 6--Freezer; 7 Cold bath or hot bath; 8—Three-way valve; 3, 9 Rotor flowmeter; 10 Karl Fischer tester; 11 Wet flowmeter Figure A4 Schematic diagram of freezer structure
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 Southwest Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Guangming Chemical Research Institute of the Ministry of Chemical Industry. The drafter of this standard is Wang Xiguang.6 Each bottle of hydrogen chloride leaving the factory should be accompanied by a quality analysis report and a product certificate. The contents of the certificate should include: a. Product name;
Manufacturer name;
Production date;
d. Cylinder weight,
Product weight;
Standard number.
7 Safety requirements
7.1 Hydrogen chloride is a colorless, irritating gas. Its permissible limit of contact with air is 5×10-°. If this limit is exceeded, it can cause coughing, pulmonary edema, and even life-threatening. Therefore, strict attention should be paid when producing and using hydrogen chloride, and corresponding protective measures should be taken. 7.2 When hydrogen chloride comes into contact with metal, it can react to generate chloride and hydrogen. Due to the generation of hydrogen, there is a potential risk of explosion and fire. Therefore, it is strictly prohibited to have open flames and store flammable and explosive items at the use and storage points. 7.3 When using bottled hydrogen chloride, a pressure reducer should be equipped to prevent the system from overpressure and explosion during use. After using the hydrogen chloride cylinder, the bottle valve should be closed in time and removed from the system to prevent accidents. 7.4 Before inspecting and handling hydrogen fluoride pipelines, equipment, and cylinders, the hydrogen chloride must be completely replaced and work can only begin in accordance with safety regulations.
7.5 The pressure reducer, pipeline, valve and pipe fittings of the measuring device should be made of stainless steel resistant to hydrogen chloride corrosion. 573
High-purity fluorine
Hydrogen purity, etc.
GB/T14602—93
Appendix A
Schematic diagram of gas flow and freezer structure
(reference)
Figure A1 Schematic diagram of thermal conductivity chromatography cutting gas flow chart Venting
1 Needle stop valve; 2 Rotor flowmeter; 3. Three-way valve; 4—-dilution bottle; 5, 6, 8, 9.-switching four-way valve; 7-fixed volume injection tube; 10·pre-separation column; 11--chromatographic column; 12 thermal conductivity detector ammonia gas
sample gas
Figure A2 Schematic flow chart of conversion hydrogen flame chromatography cutting gas path 1·needle valve; 2—-dilution bottle; 3-three-way valve; 4, 5, 7, 8—switching four-way valve; 6—fixed volume injection tube; 9 chromatographic column; 10—conversion column; 11 hydrogen flame detector Additional instructions ：
Sample tail gas treatment
GB/T1460293
Figure A3 Schematic diagram of Karl Fischer test device Pure gas-free
1, 2 Needle valve; 4, 5—Four-way valve; 6--Freezer; 7 Cold bath or hot bath; 8—Three-way valve; 3, 9 Rotor flowmeter; 10 Karl Fischer tester; 11 Wet flowmeter Figure A4 Schematic diagram of freezer structure
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 Southwest Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Guangming Chemical Research Institute of the Ministry of Chemical Industry. The drafter of this standard is Wang Xiguang.
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