GB/T 14600-1993 Nitrous oxide gas for use in the electronics industry
Some standard content:
National Standard of the People's Republic of China
Nitrous oxide
Gases for electronic industry--Nitrous oxideSubject content and scope of application
GB/T 14600-93
This standard specifies the technical requirements, test methods, acceptance rules and packaging, marking, storage and transportation requirements of gas for electronic industry--nitrous oxide in bottles.
This standard applies to nitrous oxide produced by thermal decomposition of ammonium nitrate. This product is mainly used in chemical vapor deposition and plasma processes of silicon dioxide in the electronics industry.
Molecular formula: N, O
Relative molecular mass: 44.01 (according to the international relative atomic mass in 1989) 2 Reference standards
GB 190
GB3723
GB5099
Marking of dangerous goods packaging
General rules for sampling of industrial chemical products
Seamless steel gas cylinders
GB 5832. 1
GB6680
GB7144
GB7230
GB7445
GB8984
GB 10624
Determination of trace moisture in gas
Determination of trace moisture in gas
General rules for sampling of liquid chemical products
Color marking of gas cylinders
Gas detection tube device
Electrolysis method
Dew point method
Determination of carbon monoxide, carbon dioxide and methane content in gas High purity argon
GB/T14606 Determination of total hydrocarbons in gas Flame ionization detection method 3 Technical conditions
The quality of nitrous oxide products shall comply with the requirements of Table 1. Table 1
Purity of nitrous oxide, 10-2
Ammonia content, 10-6
Carbon dioxide content, 10-6
Carbon dioxide content, 10-6
State Administration of Technical Supervision, 1993-08-26, approved 558
Gas chromatography method
1994-07-01, implemented
Hydrocarbon C,~-C, (calculated as methane) content, 10--6Nitrogen content, 10°6
Oxygen content, 10-.
Nitric oxide content, 106
Nitrogen dioxide content, 10-6
Water content, 10-6
Note: Purity and impurity content are expressed in volume fraction. 4 Test methods
4.1 Sampling methods
GB/T 14600—93
Continued Table 1
When sampling, turn the sample cylinder upside down. Take liquid samples, and connect the liquid samples directly to the instrument with a conduit after gasification. Metal tubes are used for the determination of oxygen, nitrogen, water, carbon dioxide, carbon monoxide and hydrocarbons, and polytetrafluoroethylene tubes are used as sampling conduits for the determination of ammonia, nitrogen monoxide and nitrogen dioxide. 4.2 Purity
The purity of nitrous oxide product, expressed as volume fraction, is calculated according to formula (1): =100(++9++++9++9)×10-4
Wherein: —total
nitrous oxide purity, 10-2;
ammonia content, 10-°,
carbon dioxide content, 10-6;
carbon dioxide content, 10-6;
hydrocarbon C,～C, (calculated as methane) content, 10-6nitrogen content, 10-5,
oxygen content, 10-6;
nitrogen oxide content, 10-6,
-nitrogen dioxide content, 10-6;
—water content, 10~6.
4.3 Determination of Hydrogen Content
4.3.1 Summary of Method
Use a detector tube filled with bromophenol blue (or other equivalent) colorimetric reagent to determine ammonia in nitrous oxide. Detection limit: 0.5×10-6 (V/V).
4.3.2 Equipment and Materials
Stainless steel needle valve.
b. Polytetrafluoroethylene tube.
Ammonia detector tube: Measuring range (2~～30)×10-(V/V). d. Flowmeter: Measuring range 0～200mL/min, 4.3.3 Operating Steps
4.3.3.1 Install the stainless steel needle valve at the outlet of the sample cylinder. 4.3.3.2 Connect the flowmeter to the needle valve with a catheter. ++++-+++( 1)
Open the valve of the pre-inverted sample cylinder and fully replace the system with nitrous oxide gas. After the representative sample can be obtained, connect the detection tube to the outlet of the flowmeter.
GB/T 14600-93
4.3.3.4 When nitrous oxide gas passes through the detection tube, start metering. The control of injection volume and injection flow rate shall be carried out according to the operating instructions of the detection tube.
4.3.3.5 Read the ammonia content according to the length of the color change of the detection tube. 4.4 The determination of carbon dioxide and carbon dioxide content shall be carried out in accordance with the provisions of GB8984. However, this standard changes the following conditions: Carrier gas: hydrogen. Its purity should be greater than 99.999×10-2 and must comply with the provisions of GB7445. The flow rate is about 30mL/min. a.
b. Tail gas: argon. Change the combustion gas path to tail gas. The purity of argon should comply with the provisions of GB10624 c. Chromatographic column: a stainless steel tube with a length of about 0.70m and an inner diameter of 4mm, filled with TDX-01 carbon molecular sieve, with a particle size of 200-250um. d. Column temperature: about 80℃.
4.4.1 Standard mixed gas
4.4.1.1 The standard mixed gas should comply with relevant national regulations and have a number approved by the national standardization administrative department. 4.4.1.2 The concentration of carbon monoxide and carbon dioxide in the standard mixed gas should be similar to that of carbon monoxide and carbon dioxide in the sample to be tested, usually not more than 200% of the concentration of carbon monoxide and carbon dioxide in the sample to be tested, and not less than 50% of the concentration of carbon monoxide and carbon dioxide in the sample to be tested.
4.4.1.3 The base gas of the standard mixed gas is hydrogen. 4.5 Determination of hydrocarbon C,～Cs content
Determination shall be carried out in accordance with the provisions of GB/T14606.
4.6 Determination of nitrogen and oxygen content
4.6.1 Instrument
Use a gas chromatograph with a nitrogen ion detector or a photoionization detector to determine the nitrogen and oxygen content in nitrous oxide. Detection limit: not less than 0.5×10-(V/V). 4.6.2 Instrument parameters
4.6.2.1 The operating parameters of the instrument shall be selected in accordance with the instrument manual and the detection sensitivity requirements. 4.6.2.2 Chromatographic column: a stainless steel tube with a length of about 1.5m and an inner diameter of about 4mm, filled with 5A (or 13X) molecular sieve, with a particle size of 250～400μm.
4.6.2.3 Sample volume: 1~3mL.
4.6.2.4 Detector and chromatographic column temperature: room temperature. 4.6.3 Standard mixed gas
4.6.3.1 Standard mixed gas shall comply with relevant national regulations and have a number approved by the national standardization administrative department. 4.6.3.2 The concentration of nitrogen and oxygen in the standard mixed gas shall be similar to that of the sample to be tested, usually not more than 200% of the concentration of nitrogen and oxygen in the sample to be tested, and not less than 50% of the concentration of nitrogen and oxygen in the sample to be tested. 4.6.3.3 The base gas of the standard mixed gas is nitrogen. 4.6.4 Operation steps
4.6.4.1 Sampling
a Safety matters in sampling shall be in accordance with the provisions of GB3723. b. The sampling of liquid nitrous oxide samples shall comply with the provisions of Chapter 6 of GB6680. C. For the sampling of liquid nitrous oxide, a needle valve with a small dead volume must be used. After being fully replaced by the sample gas by at least three times of pressure increase and decrease, it is directly sent to the analysis instrument through a metal tube with an inner diameter of about 2 to 3 mm. 4.6.4.2 Calibration
Send the standard mixed gas that meets the requirements of 4.6.3 of this standard into the analytical instrument and fully replace the system with the standard mixed gas. After obtaining the representative sample, switch the sampling valve to allow the carrier gas to carry the standard mixed gas into the chromatographic column and detector. Repeat the injection at least twice, record and measure the retention time and chromatographic peak area (or peak height) of nitrogen and oxygen. When the relative average deviation of the chromatographic peak area (or peak height) measured twice does not exceed 5%, take the average value A, (or h) as the measured value of nitrogen and oxygen in the standard sample. 3
4.6.4.3 Determination
GB/T 14600--93
According to 4.6.4.1 The sample taken as specified shall be directly sent to the sampling system of the analytical instrument. After being fully replaced and a representative sample is obtained, the sampling valve shall be switched to allow the carrier gas to carry the sample into the chromatographic column and detector. The injection shall be repeated at least twice, and the retention time and chromatographic peak area (or peak height) of nitrogen and oxygen shall be recorded and measured. When the relative average deviation does not exceed 5%, the average value A, (or h,) shall be taken as the measured value of nitrogen and oxygen in the sample. 4.6.5 Result calculation
Where:
9——the content of component i in the sample gas 10-6 (V/V), g——the content of component i in the standard mixed gas, 10-6 (V/V), Ph)
A (or h,)---the peak area (or peak height) of component i in the sample gas, mm (or mm), A. (or h.)---the peak area (or peak height) of component i in the standard mixed gas, mm2 (or mm). 4.7 Determination of Nitric Oxide Content
4.7.1 Method and Instrument Requirements
The chemiluminescence method is used to determine the nitric oxide in nitrous oxide. The detector is equipped with a photomultiplier tube that can read the decay luminescence of nitrogen dioxide. The detector has an adjustable attenuator, zero point and span regulator, and is equipped with an ozone generator. Detection limit: 0.1×10-6 (V/V).
4.7.2 Instrument Parameterswww.bzxz.net
4.7.2.1 Flow Requirements: The flow rates of zero gas, standard mixed gas, and sample gas should all comply with the requirements of the instrument operating manual. 4.7.3 Standard Sample
4.7.3.1 Zero Gas: Argon (purity greater than 99.99×10-2) containing less than 0.1×10-6 (V/V) nitric oxide. 4.7.3.2 Standard mixed gas: Use argon as the base gas (purity greater than 99.99×10-2). The concentration of nitric oxide shall not be greater than five times the technical index.
4.7.3.3 The nitric oxide content of the oxygen fed into the ozone generator shall be less than 0.1×10-(V/V). 4.7.4 Operation steps
4.7.4.1 Pass zero gas and adjust the instrument to zero point with the zero adjustment knob. 4.7.4.2 Pass standard mixed gas and adjust with the span adjustment knob to make the output reading consistent with the concentration of the standard mixed gas. 4.7.4.3 Repeat steps 4.7.4.1 and 4.7.4.2 until the reproducibility of the reading is better than 1% of the full scale value. 4.7.4.4 Pass nitrous oxide sample and read the content of nitric oxide. The result shall meet the requirements. Note: This method does not determine the nitrogen dioxide impurity in nitrous oxide. 4.8 Determination of ammonia dioxide content
4.8.1 Summary of the method
Use a detection tube filled with o-(di)anisidine (or other equivalent) colorimetric reagent to determine nitrogen dioxide in nitrous oxide. Detection limit: 0.1×10-6 (V/V).
4.8.2 Equipment and materials
Needle regulating valve.
Polytetrafluoroethylene tube.
Nitrogen dioxide detection tube: Measuring range 0.2～6×10~6. Measuring range of flow meter 0~~200mL/min. 4.8.3 Operating steps
4.8.3.1 Install the needle regulating valve at the outlet of the cylinder. 4.8.3.2 Connect the flow meter and the needle valve with a polytetrafluoroethylene tube. 561
GB/T 14600---93
4.8.3.3 Open the valve of the pre-inverted sample cylinder, adjust the gas flow rate with the regulating valve and fully purge the displacement system. After the representative sample can be obtained, connect the detection tube to the outlet of the flowmeter. 4.8.3.4 Start measuring when the nitrous oxide gas passes through the detection tube. The control of the injection volume and injection flow rate shall be carried out according to the operating instructions of the detection tube. 4.8.3.5 Read the nitrogen dioxide content according to the length of the color change of the detection tube. 4.9 Determination of water content
Determine according to the provisions of GB5832.1 or GB5832.2. During the determination, the sample cylinder can be upright and samples can be taken from the gas phase. The two methods have equal validity.
5 Acceptance rules
5.1 Nitrous oxide products shall be inspected and accepted by the quality supervision department of the manufacturer, and the quality of all factory products shall be guaranteed to meet the requirements of this standard. 5.2 Nitrous oxide products should be inspected bottle by bottle.
5.3 When any indicator of the inspected sample does not meet the requirements of this standard, it shall be judged as a defective product. 5.4 Users have the right to accept in accordance with the provisions of this standard. 5.5 When the supply and demand parties have objections to the quality of the product, the supply and demand parties shall jointly accept or submit it to arbitration. 6 Packaging, marking, storage and transportation
6.1 Packaging, marking, storage and transportation shall comply with the "Regulations on Safety Supervision of Gas Cylinders", "Rules for the Transportation of Dangerous Goods" and relevant regulations of the transportation department.
6.2 Packaging and marking shall comply with the provisions of GB190. 6.3 The color marking of steel cylinders for packaging liquid nitrous oxide shall comply with the provisions of GB7144. 6.4 The maximum allowable amount of nitrous oxide filled in cylinders shall be calculated according to formula (3): m=VK
Wherein: m-mass of nitrous oxide in cylinder, kg; V-inner volume indicated on cylinder, L,
K——filling factor (see Table 2), kg/L. Table 2
Nominal pressure of gas cylinders
Filling factor K
kg/L shall not exceed
(3)
6.5 The actual amount of nitrous oxide filled in cylinders shall be measured by direct weighing. The weighing scale shall comply with the provisions of Article 56 of Chapter VII of the "Regulations on Safety Supervision of Gas Cylinders".
6.6 Nitrous oxide cylinders returned to the manufacturer for refilling shall have residual gas. Cylinders without residual gas, new cylinders and cylinders that have undergone water pressure testing shall be strictly heated and evacuated before filling, and fully replaced and cleaned with nitrous oxide. 6.7 Bottled nitrous oxide should be inspected for leaks at the bottle mouth, bottle valve stem, and the connection between the bottle valve and the thread before leaving the factory, and the bottle cap should be put on. 6.8 Nitrous oxide products should be accompanied by a product quality certificate when leaving the factory, and the content should include: a. Product name, manufacturer name; production date and production batch number; packaging container number; filling factor and mass number of nitrous oxide; analysis results; g. Code of this standard Safety requirements GB/T 14600-93 Chlorine dioxide (commonly known as laughing gas) is a colorless liquid gas with strong oxidizing properties. It has a slightly sweet smell and is a simple asphyxiating agent. When used, it needs to be discharged outdoors through a duct. Additional instructions: This standard was proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Southwest Research Institute of Chemical Industry, Ministry of Chemical Industry. This standard was drafted by the Southwest Research Institute of Chemical Industry, Ministry of Chemical Industry, with participation from Beijing Oxygen Plant, Guangzhou Gas Plant, and the 10th Design Institute of the Ministry of Mechanical and Electrical Engineering.
The main drafter of this standard is Duan Shufang4 Pass the nitrous oxide sample and read the content of nitric oxide. The result should meet the requirements. Note: This method does not determine the nitrogen dioxide impurity in nitrous oxide. 4.8 Determination of ammonia dioxide content
4.8.1 Method summary
Use a detection tube filled with o-(di)anisidine (or other equivalent) color developer to determine the nitrogen dioxide in nitrous oxide. Detection limit: 0.1×10-6 (V/V).
4.8.2 Equipment and materials
Needle regulating valve.
Polytetrafluoroethylene tube.
Nitrogen dioxide detection tube: Measuring range 0.2～6×10~6. Flowmeter measuring range 0~~200mL/min. 4.8.3 Operating steps
4.8.3.1 Install the needle regulating valve at the outlet of the cylinder. 4.8.3.2 Connect the flowmeter and needle valve with a polytetrafluoroethylene tube. 561
GB/T 14600---93
4.8.3.3 Open the valve of the pre-inverted sample cylinder, adjust the gas flow with a regulating valve and fully purge the displacement system. After the representative sample can be obtained, connect the detection tube to the outlet of the flowmeter. 4.8.3.4 Start measuring when nitrous oxide gas passes through the detection tube. The control of the injection volume and injection flow rate shall be carried out according to the operating instructions of the detection tube. 4.8.3.5 Read the nitrogen dioxide content according to the length of the color change of the detection tube. 4.9 Determination of water content
Determine in accordance with the provisions of GB5832.1 or GB5832.2. During the determination, the sample cylinder can be placed upright and samples can be taken from the gas phase. The two methods are equally effective.
5 Acceptance rules
5.1 Nitrous oxide products shall be inspected and accepted by the quality supervision department of the manufacturer, and the quality of all products leaving the factory shall be guaranteed to meet the requirements of this standard. 5.2 Nitrous oxide products shall be inspected bottle by bottle.
5.3 When any index of the inspected sample does not meet the requirements of this standard, it shall be judged as unqualified product. 5.4 Users have the right to accept in accordance with the provisions of this standard. 5.5 When the supply and demand parties have objections to the quality of the product, the supply and demand parties shall jointly accept or submit to arbitration. 6 Packaging, marking, storage and transportation
6.1 Packaging, marking, storage and transportation shall comply with the "Regulations on Safety Supervision of Gas Cylinders", "Regulations on the Transportation of Dangerous Goods" and relevant regulations of the transportation department.
6.2 Packaging and marking shall comply with the provisions of GB190. 6.3 The color marking of the cylinders for packaging liquid nitrous oxide shall comply with the provisions of GB7144. 6.4 The maximum allowable amount of nitrous oxide filled in cylinders shall be calculated according to formula (3): m=VK
Wherein: m-mass of nitrous oxide in cylinder, kg; V-inner volume indicated on cylinder, L,
K——filling factor (see Table 2), kg/L. Table 2
Nominal pressure of gas cylinders
Filling factor K
kg/L shall not exceed
(3)
6.5 The actual amount of nitrous oxide filled in cylinders shall be measured by direct weighing. The weighing scale shall comply with the provisions of Article 56 of Chapter VII of the "Regulations on Safety Supervision of Gas Cylinders".
6.6 Nitrous oxide cylinders returned to the manufacturer for refilling shall have residual gas. Cylinders without residual gas, new cylinders and cylinders that have undergone water pressure testing shall be strictly heated and evacuated before filling, and fully replaced and cleaned with nitrous oxide. 6.7 Bottled nitrous oxide should be inspected for leaks at the bottle mouth, bottle valve stem, and the connection between the bottle valve and the thread before leaving the factory, and the bottle cap should be put on. 6.8 Nitrous oxide products should be accompanied by a product quality certificate when leaving the factory, and the content should include: a. Product name, manufacturer name; production date and production batch number; packaging container number; filling factor and mass number of nitrous oxide; analysis results; g. Code of this standard Safety requirements GB/T 14600-93 Chlorine dioxide (commonly known as laughing gas) is a colorless liquid gas with strong oxidizing properties. It has a slightly sweet smell and is a simple asphyxiating agent. When used, it needs to be discharged outdoors through a duct. Additional instructions: This standard was proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Southwest Research Institute of Chemical Industry, Ministry of Chemical Industry. This standard was drafted by the Southwest Research Institute of Chemical Industry, Ministry of Chemical Industry, with participation from Beijing Oxygen Plant, Guangzhou Gas Plant, and the 10th Design Institute of the Ministry of Mechanical and Electrical Engineering.
The main drafter of this standard is Duan Shufang4 Pass the nitrous oxide sample and read the content of nitric oxide. The result should meet the requirements. Note: This method does not determine the nitrogen dioxide impurity in nitrous oxide. 4.8 Determination of ammonia dioxide content
4.8.1 Method summary
Use a detection tube filled with o-(di)anisidine (or other equivalent) color developer to determine the nitrogen dioxide in nitrous oxide. Detection limit: 0.1×10-6 (V/V).
4.8.2 Equipment and materials
Needle regulating valve.
Polytetrafluoroethylene tube.
Nitrogen dioxide detection tube: Measuring range 0.2～6×10~6. Flowmeter measuring range 0~~200mL/min. 4.8.3 Operating steps
4.8.3.1 Install the needle regulating valve at the outlet of the cylinder. 4.8.3.2 Connect the flowmeter and needle valve with a polytetrafluoroethylene tube. 561
GB/T 14600---93
4.8.3.3 Open the valve of the pre-inverted sample cylinder, adjust the gas flow with a regulating valve and fully purge the displacement system. After the representative sample can be obtained, connect the detection tube to the outlet of the flowmeter. 4.8.3.4 Start measuring when nitrous oxide gas passes through the detection tube. The control of the injection volume and injection flow rate shall be carried out according to the operating instructions of the detection tube. 4.8.3.5 Read the nitrogen dioxide content according to the length of the color change of the detection tube. 4.9 Determination of water content
Determine in accordance with the provisions of GB5832.1 or GB5832.2. During the determination, the sample cylinder can be placed upright and samples can be taken from the gas phase. The two methods are equally effective.
5 Acceptance rules
5.1 Nitrous oxide products shall be inspected and accepted by the quality supervision department of the manufacturer, and the quality of all products leaving the factory shall be guaranteed to meet the requirements of this standard. 5.2 Nitrous oxide products shall be inspected bottle by bottle.
5.3 When any index of the inspected sample does not meet the requirements of this standard, it shall be judged as unqualified product. 5.4 Users have the right to accept in accordance with the provisions of this standard. 5.5 When the supply and demand parties have objections to the quality of the product, the supply and demand parties shall jointly accept or submit to arbitration. 6 Packaging, marking, storage and transportation
6.1 Packaging, marking, storage and transportation shall comply with the "Regulations on Safety Supervision of Gas Cylinders", "Regulations on the Transportation of Dangerous Goods" and relevant regulations of the transportation department.
6.2 Packaging and marking shall comply with the provisions of GB190. 6.3 The color marking of the cylinders for packaging liquid nitrous oxide shall comply with the provisions of GB7144. 6.4 The maximum allowable amount of nitrous oxide filled in cylinders shall be calculated according to formula (3): m=VK
Wherein: m-mass of nitrous oxide in cylinder, kg; V-inner volume indicated on cylinder, L,
K——filling factor (see Table 2), kg/L. Table 2
Nominal pressure of gas cylinders
Filling factor K
kg/L shall not exceed
(3)
6.5 The actual amount of nitrous oxide filled in cylinders shall be measured by direct weighing. The weighing scale shall comply with the provisions of Article 56 of Chapter VII of the "Regulations on Safety Supervision of Gas Cylinders".
6.6 Nitrous oxide cylinders returned to the manufacturer for refilling shall have residual gas. Cylinders without residual gas, new cylinders and cylinders that have undergone water pressure testing shall be strictly heated and evacuated before filling, and fully replaced and cleaned with nitrous oxide. 6.7 Bottled nitrous oxide should be inspected for leaks at the bottle mouth, bottle valve stem, and the connection between the bottle valve and the thread before leaving the factory, and the bottle cap should be put on. 6.8 Nitrous oxide products should be accompanied by a product quality certificate when leaving the factory, and the content should include: a. Product name, manufacturer name; production date and production batch number; packaging container number; filling factor and mass number of nitrous oxide; analysis results; g. Code of this standard Safety requirements GB/T 14600-93 Chlorine dioxide (commonly known as laughing gas) is a colorless liquid gas with strong oxidizing properties. It has a slightly sweet smell and is a simple asphyxiating agent. When used, it needs to be discharged outdoors through a duct. Additional instructions: This standard was proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Southwest Research Institute of Chemical Industry, Ministry of Chemical Industry. This standard was drafted by the Southwest Research Institute of Chemical Industry, Ministry of Chemical Industry, with participation from Beijing Oxygen Plant, Guangzhou Gas Plant, and the 10th Design Institute of the Ministry of Mechanical and Electrical Engineering.
The main drafter of this standard is Duan Shufang
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