Some standard content:
National Standard of the People's Republic of China
Gases for electronic industry--OxygenSubject Content and Scope of Application
GB/T 14604-93
This standard specifies the technical requirements, inspection methods, inspection rules and product packaging, marking, transportation, storage and safety requirements of gaseous oxygen and bulk liquid oxygen for the electronic industry.
Oxygen for electronic industry is mainly used for chemical vapor deposition of silicon dioxide, as an oxidation source and a reactant for producing high-purity water, and for plasma etching and separation. It can also be used for optical fibers. Molecular formula: 02
Relative molecular weight: 31.999 (1989 International Relative Atomic Mass Table) 2 Reference standards
(B 3863
GB4844
GB5099
Dangerous goods packaging mark
Industrial gaseous oxygen
Steel seamless gas cylinders
GB 5832. 2
GB 6680
GB 6681
GB 7144
GB7445
GB 8984
GB 8991
Determination of trace water in gas-Dew point method
General rules for sampling of liquid chemical products
General rules for sampling of gas chemical products
Color marking of gas cylinders
Determination of carbon monoxide, carbon dioxide and methane in gas-Gas chromatography
Determination of trace hydrogen in gas-Gas chromatography GB/T 14605
Determination of trace argon, nitrogen and nitrogen content in oxygen Gas chromatography GB/T14606 Determination of total hydrocarbons in gas Flame ionization detection method 3 Technical requirements
The quality of oxygen used in the electronics industry should meet the requirements of the following table
Oxygen purity, 102
Mouse content. 106
Mouse content, 10.
Approved by the State Administration of Technical Supervision on August 26, 199382
Ultra-large scale integrated circuit level
Semiconductor and integrated circuit level| |tt||Electronic grade and bulk liquid oxygen
1994-07-01 implementation
Nitrogen content, 106
Carbon monoxide content, 106
Carbon dioxide content, 10-6
Carbon monoxide and carbon dioxide content, 10-6Total hydrocarbon content (as methane), 10°5
Nitrous oxide content, 106
Nitrogen content, 10-6
Water content, 106
Total impurity content (including rare gases), 10-6GB/T 14604--93
VLSI level
Semiconductor and integrated circuit level
Note: () This standard does not include technical requirements for particles, which shall be agreed upon by the supply and demand parties. ②Purity and content are both expressed in volume fraction. 4 Inspection method
4.1 Sampling
Electronic grade and bulk liquid oxygen
4.1.1 The sampling of bottled gaseous oxygen shall comply with the provisions of GB6681. Sampling shall be carried out directly from the sample bottle using a needle valve and a metal tube, and transfer is not allowed.
4.1.2 For gaseous oxygen transported by pipeline, use a short metal tube as much as possible to send the sample gas directly into the analyzer. 4.1.3 The sampling of liquid oxygen shall comply with the provisions of GB6680. Liquid oxygen must be sampled from the liquid phase and ensure that the liquid oxygen is completely gasified. After the sample is restored to room temperature, it can be sampled.
4.2 Determination of oxygen purity
4.2.1 Determination of oxygen purity at VLSI level The oxygen purity (V/V) is calculated by the difference method after deducting the impurity content according to formula (1): =100-++++++++) × 10-4
Wherein:
Oxygen purity, 10-2,
Hydrogen content, 10-6,
Argon content, 10-6;
Nitrogen content, 10-6,
Carbon monoxide content, 10-6,
Carbon dioxide content, 10-6;
Total hydrocarbon content, 10-°,
Nitrous oxide content, 10-6;
Krypton content, 10-
Water content, 10-6.
4.2.2 The determination of semiconductor and integrated circuit grade, electronic grade and bulk liquid grade oxygen purity shall be determined according to the method specified in 3.1 of GB3863. 4.3 Determination of hydrogen content
Determination shall be carried out according to the provisions of GB8991.
(1)
4.4 Determination of fluorine, nitrogen and nitrogen content
Determination shall be carried out according to the provisions of GB/T14605. 4.5 Determination of carbon dioxide and carbon dioxide
Determination shall be carried out according to the provisions of GB8984.
GB/T 14604-93
4.5.1 When determining carbon dioxide, the adsorbent shall be 13X molecular sieve with a diameter of 0.25 to 0.20 mm, activated by fluorine gas at 350°C for 4 hours; the column temperature shall be 50°C; the injection volume shall be 3 mL; the minimum detection amount shall be 0.5×10-6 (V/V). 4.5.2 When determining carbon dioxide, a stainless steel column with a length of 40 cm and an inner diameter of 2 mm is used, filled with 0.20-0.15 mm TDX, activated by chlorine gas at 130°C for 4 hours, and the column temperature is 40°C; the injection volume is 3 mL. 4.5.3 The pre-cutting deoxygenation method is allowed to determine the content of carbon monoxide and carbon dioxide. 4.6 Determination of total hydrocarbon content
Determine in accordance with the provisions of GB/T14606.
4.7 Determination of water content
Determine in accordance with the provisions of GB5832.2.
4.8 Determination of nitrous oxide content
4.8.1 Method and principle
Nitrogen ionization gas chromatography is used.
This method is based on the Penning effect principle. When the carrier gas nitrogen enters the detector, some nitrogen atoms are excited to the metastable state under the action of the β particles radiated by the chlorine source. After the sample gas is separated by the chromatographic column, it enters the detector together with the carrier gas. When the sample contains a component with an ionization energy lower than the excitation energy of the metastable nitrogen atom, the component collides with the metastable ammonia atom and is ionized. Under the action of the external electric field, an ion flow is formed. Within a certain range, the output ion flow is proportional to the concentration of the component. 4.8.2 Instrument
Gas chromatograph with nitrogen ionization detector. The instrument is required to have a minimum detection amount of nitrous oxide of 0.5×10-6. 4.8.3 Operating reference conditions
4.8.3.1 Carrier gas: nitrogen, high-purity nitrogen in GB4844, flow rate of 30~40mL/min. 4.8.3.2 Operating gas: nitrogen, pure nitrogen first-grade in GB4844, mainframe pressure indication value of 0.3MPa. 4.8.3.3 Impurity gas: hydrogen, high-purity hydrogen in GB7445, mainframe pressure indication value of 0.05MPa. 4.8.3.4 Chromatographic column: a stainless steel tube with a length of 4m and an inner diameter of 3mm, filled with 0.20~0.15mm porapakR, activated by passing argon or ammonia at 180℃ for 4h.
4.8.3.5 Chromatographic column temperature: 30℃.
4.8.3.6 Polarization voltage: 500~600V.
4.8.3.7 Recorder: 1~2.5mV.
4.8.3.8 Injection volume: 1.5mL.
4.8.4 Provisions for standard mixed gas
The standard mixed gas uses oxygen as the base gas, and the component content should be close to the component content to be measured. The standard mixed gas should have a number approved by the national standardization administrative department.
4.8.5 Operating steps
4.8.5.1 Turn on the instrument according to the instrument manual and operating conditions until it is stable. 4.8.5.2 Connect the sample gas to the instrument through the needle valve and metal pipe, open the sample gas cylinder valve, adjust the flow rate with the needle valve, fully replace the sampling system and switch the six-way valve to inject the sample, and measure the peak area A (or peak height h). 4.8.5.3 Connect the standard mixed gas that meets the requirements of 4.8.4 to the instrument through the needle valve and Jinteng pipe, operate according to 4.8.5.2, and measure the peak area Az (or peak height hz).
4.8.6 Calculation of results
4.8.6.1 Nitrous oxide content (V/V) is calculated according to formula (2): 58.1
GB/T 14604-93
will be × or 9
where: 9-nitrous oxide content in the sample gas, 10-nitrous oxide content in the standard mixed gas, 10-°; hi
A, (or h,)-the peak area (or peak height) of nitrous oxide in the sample gas, mm2 (or mm); Az (or h2)-the peak area (or peak height) of nitrous oxide in the standard mixed gas, mm2 (or mm). (2)
4.8.6.2 Take the arithmetic mean of the results of two parallel determinations as the determination result, and the relative deviation of the parallel determination results shall not exceed 10%. 5 Inspection rules
5.1 The quality supervision department of the manufacturer shall conduct acceptance inspection for gas oxygen for the electronic industry in accordance with the provisions of this standard. The manufacturer shall ensure that all products leaving the factory meet the requirements of this standard. 5.2 Ultra-large-scale integrated circuit grade oxygen shall be inspected bottle by bottle. If one of the indicators does not meet the requirements of this standard, the bottle of product shall be unqualified.
5.3 Semiconductor and integrated circuit grade oxygen, electronic grade and bulk liquid grade oxygen shall be inspected in batches, and the number of bottles in each batch shall not exceed the products of one production shift. Randomly select 5% of the samples from each batch for inspection. If one of the indicators does not meet the requirements of this standard, the random double sampling inspection shall be carried out again. If there is still one indicator that does not meet the requirements of this standard, the batch of products shall be unqualified. 5.4 When liquid oxygen is shipped by tank or tank truck, each tank or tank truck is a batch, and samples should be taken from each tank or tank truck for inspection.
5.5 When gas oxygen is transported by pipeline, sampling inspection should be carried out at least once within 8 hours. 5.6 Users have the right to accept in accordance with the provisions of this standard. 5.7 When the supply and demand parties have objections to the quality of the product, they can jointly accept or apply for arbitration. 6 Marking, packaging, storage and transportation
6.1 The use, storage and transportation of gas cylinders shall comply with the relevant provisions of the "Regulations on Safety Supervision of Gas Cylinders" and the "Regulations on the Transportation of Dangerous Goods". 6.2 The packaging, storage and transportation of liquefied gas storage tanks or tank trucks for liquid oxygen shall comply with the relevant provisions of the "Regulations on Safety Supervision of Pressure Vessels" and the "Regulations on the Transportation of Dangerous Goods".
6.3 The color and packaging markings of gas cylinders shall comply with the provisions of GB7144 and GB190. The outer surface of the packaging container should be marked with words such as "Gas oxygen for electronic industry".
6.4 The gas cylinder and the maximum working pressure should comply with the provisions of GB5099. 6.5 The pressure of bottled oxygen shall not be less than 15.0 ± 0.5MPa at 20℃. When measuring the pressure in the bottle, it should be confirmed that the gas temperature is equal to the ambient temperature, and the accuracy of the pressure gauge used for measurement shall not be less than Class 2.5. 6.6 There shall be no leakage at the threaded connection between the bottle valve and the bottleneck of the gas cylinder, the outlet of the bottle valve and the gap between the bottle valve stem. 6.7 Safety helmets must be worn for cylinders filled with oxygen. 6.8 When the user returns the empty bottle to the manufacturer, the residual pressure in the bottle must not be less than 0.4MPa. 6.9 The filling volume of oxygen shall be calculated according to Appendix A. 6.10
The weight of liquid oxygen is converted to the volume of gaseous oxygen at 20℃ and 101.3kPa, which shall be calculated according to Appendix B. 6. 11
When oxygen leaves the factory, it shall be accompanied by a quality certificate, which shall include: product name and grade;
name of manufacturer;
production date or batch number;
gas cylinder number;
GB/T 14604-93
e: quantity of oxygen (m\), or weight (kg), or pressure (MPa); f. implementation standard code.
7 Safety requirements
7.1 Oxygen is a colorless, tasteless, odorless, non-toxic and non-flammable gas. It is a strong oxidant that can support combustion. It is explosive when mixed with flammable gases. Compressed oxygen is prohibited from contacting with grease. 7.2 Oxygen accumulation in the room may cause fire, so ventilation devices should be installed in places where the oxygen concentration may increase, and oxygen alarms should be installed when necessary to monitor the oxygen concentration. The volume concentration of oxygen in the workplace shall not exceed 23%. 7.3 Before repairing or handling oxygen containers, oxygen must be blown out first, and work can only be carried out when the oxygen concentration drops below 23%. 7.4 When working in an oxygen-rich environment, smoking and open flames are not allowed. Containers filled with oxygen are prohibited from being filled with other gases. 7.5
When loading, unloading, storing and transporting gas cylinders, special care should be taken to prevent accidents caused by gas cylinders falling. 7.6
The volume of oxygen in the gas cylinder is calculated according to formula (A1): In the formula, V—the volume of oxygen in the gas cylinder, m*, V. —the water volume of the gas cylinder, L;
GB/T14604-93
Appendix A
Calculation of the volume of oxygen in the gas cylinder
(reference)
V=K·V.
.........( A1 )
K is converted to the volume conversion coefficient of oxygen at 20℃ and 101.3kPa. The K value is calculated according to formula (A2): K=
Where: p~ is the pressure of the gas in the cylinder, MPa, +1x
is the temperature of the gas in the cylinder when the pressure is measured, ℃; the compression coefficient of oxygen at temperature t. The conversion coefficient K value at different temperatures and pressures can be found in Table A1. Table A1 Conversion coefficient K
Gas temperature in bottle, C
Pressure, MPa
....(A2)
GB/T 14604—93
Appendix B
Calculation of the weight of bottled liquid oxygen converted to the volume of gaseous oxygen (reference)
The weight of bottled liquid oxygen converted to the volume of gaseous oxygen at 20℃ and 101.3kPa is calculated according to formula (B1): V
Where: V-Www.bzxZ.net
Volume of gaseous oxygen, m~;
Weight of liquid oxygen, kg;
Density of oxygen, kg/m.
Additional remarks:
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 Research Institute of Chemical Industry of the Ministry of Chemical Industry. m
This standard is drafted by the Southwest Research Institute of Chemical Industry of the Ministry of Chemical Industry. The main drafter of this standard is Dai Peishu.
·(B1)
This standard refers to the American Semiconductor Association standards SEMIC3STD.16-86 "Bottled Electronic Grade Oxygen", C3STD.17-86 "Bottled MOS Grade Oxygen", C3.23-90 "Bottled VLSI Grade Oxygen". S8N11
When oxygen leaves the factory, it shall be accompanied by a quality certificate, the contents of which include: product name and grade;
name of manufacturer;
production date or batch number;
gas cylinder number;
GB/T 14604-93
e: quantity of oxygen (m\), or weight (kg), or pressure (MPa); f. implementation standard code.
7 Safety requirements
7.1 Oxygen is a colorless, tasteless, odorless, non-toxic and non-flammable gas. It is a strong oxidant that can support combustion. It is explosive when mixed with flammable gases. Compressed oxygen is prohibited from contacting with grease. 7.2 Oxygen accumulation in the room is dangerous for fire, so ventilation equipment should be installed in places where the oxygen concentration may increase, and oxygen alarm should be installed when necessary to monitor the oxygen concentration. The volume concentration of oxygen in the workplace shall not exceed 23%. 7.3 Before repairing or handling oxygen containers, oxygen must be blown out first, and work can only be carried out when the oxygen concentration drops below 23%. 7.4 When working in an oxygen-rich environment, smoking and open flames are not allowed. Containers filled with oxygen are prohibited from being filled with other gases. 7.5
When loading, unloading, storing and transporting gas cylinders, special care should be taken to prevent accidents caused by gas cylinders falling. 7.6
The volume of oxygen in the gas cylinder is calculated according to formula (A1): In the formula, V—the volume of oxygen in the gas cylinder, m*, V. —the water volume of the gas cylinder, L;
GB/T14604-93
Appendix A
Calculation of the volume of oxygen in the gas cylinder
(reference)
V=K·V.
.........( A1 )
K is converted to the volume conversion coefficient of oxygen at 20℃ and 101.3kPa. The K value is calculated according to formula (A2): K=
Where: p~ is the pressure of the gas in the cylinder, MPa, +1x
is the temperature of the gas in the cylinder when the pressure is measured, ℃; the compression coefficient of oxygen at temperature t. The conversion coefficient K value at different temperatures and pressures can be found in Table A1. Table A1 Conversion coefficient K
Gas temperature in bottle, C
Pressure, MPa
....(A2)
GB/T 14604—93
Appendix B
Calculation of the weight of bottled liquid oxygen converted to the volume of gaseous oxygen (reference)
The weight of bottled liquid oxygen converted to the volume of gaseous oxygen at 20℃ and 101.3kPa is calculated according to formula (B1): V
Where: V-
Volume of gaseous oxygen, m~;
Weight of liquid oxygen, kg;
Density of oxygen, kg/m.
Additional remarks:
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 Research Institute of Chemical Industry of the Ministry of Chemical Industry. m
This standard is drafted by the Southwest Research Institute of Chemical Industry of the Ministry of Chemical Industry. The main drafter of this standard is Dai Peishu.
·(B1)
This standard refers to the American Semiconductor Association standards SEMIC3STD.16-86 "Bottled Electronic Grade Oxygen", C3STD.17-86 "Bottled MOS Grade Oxygen", C3.23-90 "Bottled VLSI Grade Oxygen". S8N11
When oxygen leaves the factory, it shall be accompanied by a quality certificate, the contents of which include: product name and grade;
name of manufacturer;
production date or batch number;
gas cylinder number;
GB/T 14604-93
e: quantity of oxygen (m\), or weight (kg), or pressure (MPa); f. implementation standard code.
7 Safety requirements
7.1 Oxygen is a colorless, tasteless, odorless, non-toxic and non-flammable gas. It is a strong oxidant that can support combustion. It is explosive when mixed with flammable gases. Compressed oxygen is prohibited from contacting with grease. 7.2 Oxygen accumulation in the room is dangerous for fire, so ventilation equipment should be installed in places where the oxygen concentration may increase, and oxygen alarm should be installed when necessary to monitor the oxygen concentration. The volume concentration of oxygen in the workplace shall not exceed 23%. 7.3 Before repairing or handling oxygen containers, oxygen must be blown out first, and work can only be carried out when the oxygen concentration drops below 23%. 7.4 When working in an oxygen-rich environment, smoking and open flames are not allowed. Containers filled with oxygen are prohibited from being filled with other gases. 7.5
When loading, unloading, storing and transporting gas cylinders, special care should be taken to prevent accidents caused by gas cylinders falling. 7.6
The volume of oxygen in the gas cylinder is calculated according to formula (A1): In the formula, V—the volume of oxygen in the gas cylinder, m*, V. —the water volume of the gas cylinder, L;
GB/T14604-93
Appendix A
Calculation of the volume of oxygen in the gas cylinder
(reference)
V=K·V.
.........( A1 )
K is converted to the volume conversion coefficient of oxygen at 20℃ and 101.3kPa. The K value is calculated according to formula (A2): K=
Where: p~ is the pressure of the gas in the cylinder, MPa, +1x
is the temperature of the gas in the cylinder when the pressure is measured, ℃; the compression coefficient of oxygen at temperature t. The conversion coefficient K value at different temperatures and pressures can be found in Table A1. Table A1 Conversion coefficient K
Gas temperature in bottle, C
Pressure, MPa
....(A2)
GB/T 14604—93
Appendix B
Calculation of the weight of bottled liquid oxygen converted to the volume of gaseous oxygen (reference)
The weight of bottled liquid oxygen converted to the volume of gaseous oxygen at 20℃ and 101.3kPa is calculated according to formula (B1): V
Where: V-
Volume of gaseous oxygen, m~;
Weight of liquid oxygen, kg;
Density of oxygen, kg/m.
Additional remarks:
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 Research Institute of Chemical Industry of the Ministry of Chemical Industry. m
This standard is drafted by the Southwest Research Institute of Chemical Industry of the Ministry of Chemical Industry. The main drafter of this standard is Dai Peishu.
·(B1)
This standard refers to the American Semiconductor Association standards SEMIC3STD.16-86 "Bottled Electronic Grade Oxygen", C3STD.17-86 "Bottled MOS Grade Oxygen", C3.23-90 "Bottled VLSI Grade Oxygen". S8N
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