SJ 3236-1989 Determination of trace oxygen in electronic grade gases Yellow phosphorus luminescence method SJ3236-1989 standard download decompression password: www.bzxz.net

Standard of the Ministry of Machinery and Electronics Industry of the People's Republic of China SJ3236-89
Determination of trace oxygen in electronic grade gases and
General provisions for gas chromatography analysis
Published on March 20, 1989
Implementation on March 25, 1989
Approved by the Ministry of Machinery and Electronics Industry of the People's Republic of China Standard of the Ministry of Machinery and Electronics Industry of the People's Republic of China Determination of trace oxygen in electronic grade gases - Yellow phosphorus luminescence method
1 Main contents and scope of application
1.1 Subject content
SJ3236-89
This standard specifies the principle, analytical instrument requirements and operating procedures of the yellow phosphorus luminescence method for the determination of trace oxygen in electronic grade gases.
1.2 Scope of application
This standard uses the method for determining trace oxygen in grade nitrogen and hydrogen, with a determination range of 0.1 to 10 ppm. 2 Principle of the method
Yellow phosphorus produces yellow phosphorus vapor at room temperature and pressure. When trace oxygen in the gas reacts with yellow phosphorus vapor, it produces trioxide and emits light energy. The light energy is converted into a current signal by a photomultiplier tube. The generated light energy is proportional to the oxygen in the measured gas and is also proportional to the current output by the photomultiplier tube. Therefore, the oxygen content can be directly obtained by measuring the current. The reaction equation is as follows:
P,+30z=2P,0,+light energy
3 Instruments and materials
3.1 Yellow phosphorus luminescent trace oxygen analyzer;
3.2 Sampling valve needle valve or pressure reducing valve;
3.3 Sampling tube with an outer diameter of 3mm stainless steel tube or purple tube: 3.4 Yellow phosphorus analytical grade or chemically pure;
3.5 The oxygen content in standard nitrogen or fluorine gas is 8ppm; the oxygen content in nitrogen or argon is 1.8ppm,
4 Determination process flow chart and test conditions
4.1 Process flow chart, see the figure below
Sample IV
Flow regulating valve
Service road regulating cabinetbzxz.net
Yellow phosphorus reaction case
Figure Flow chart for determination of trace oxygen in electronic grade gas Ministry of Machinery and Electronics Industry of the People's Republic of China 1989-03- 20 Approved photoelectric low-increase tube
Friendly gas
Regulating valve
Ammeter
1989-03-25Implementation
4.2 Test conditions
0.6~0.81/min;
4.2.1 Reaction flow
4.2.2 Bypass flow
0.5~1.21/min;||tt| |SJ3236--89
0.01~0.28kg/cm2
4.2.3 Sample gas pressure
4.2.4 Sample gas temperature is less than 35℃.
5 Operation steps
5.1. Preparation
5.1.1 Load the yellow phosphorus box Place the yellow phosphorus box in a water tank at about 45℃, then put an appropriate amount of solid yellow phosphorus into the box and wait for it to melt. After filling the box, add cold water to the water tank until the yellow phosphorus in the box solidifies. Then take out the yellow phosphorus box from the water and blow off the water droplets on the surface of the yellow phosphorus with high-purity nitrogen at about 21/min. When it is dried, quickly load the yellow phosphorus box into the instrument reaction chamber. At the same time, connect the high-purity nitrogen to the instrument inlet and continue to purge until the indication on the instrument indicator is stable, then close the reaction gas regulating valve and flow regulating valve. 5.1.2 Calibration: Use standard gas of about 1.51/min to purge the pipeline for 10 minutes, adjust the flow regulating valve and the reaction gas regulating valve so that the sample flow and bypass flow are 0.6~0.81/min and 0.5~1.21/min respectively, select the appropriate range, and adjust the coarse and fine adjustment potentiometers to adjust the pointer to the oxygen concentration value contained in the standard gas. 5.2 Connection
5.2.1 Use a stainless steel pipe with a diameter of 3mm to connect the sampling valve and the analytical instrument. 5.2.2 Strictly check the air tightness of the gas circuit.
5.2.3 Purge the pipeline: Open the sampling valve, use the bypass regulating valve and the sampling valve to adjust the gas flow to about 1.51/min, and purge the pipeline for 1~2h.
5.3 Measurement
Adjust the flow control valve and the reaction gas control valve so that the sample flow and bypass flow are 0.6~0.81/min and 0.5~1.21/min respectively, select the appropriate dial range, and start reading after the pointer stabilizes (ppm). 6 Analysis precision
Relative standard deviation ±10%.
7 Test report
The test report should include the following:
Time, place, unit, date;
Sampling method and number;
Sample name;
Type and model of instrument used;
Test conditions and results;
Any abnormal phenomenon observed during the measurement; f.
Analyst's signature.
8 Precautions
The sample gas must be below 35℃,
SJ3236-89
The oxygen concentration in the sample gas must be less than 10ppm, and the instrument must be calibrated with standard gas every month.
During the measurement, the standard gas and sample gas inlet temperature, pressure and flow rate must be kept consistent. 8.4
The air tightness of the sampling valve and pipeline must be checked frequently. Additional instructions:
This standard was proposed by the Electronic Standardization Institute of the Ministry of Machinery and Electronics Industry. This standard was drafted by Wuxi Microelectronics United Company, the Institute of Semiconductors of the Chinese Academy of Sciences, etc. The main drafters of this standard are Peng Yongqing, Zhu Guohua, Zhao Changchun and Yin Enhua. 3
Tip: This standard content only shows part of the intercepted content of the complete standard. If you need the complete standard, please go to the top to download the complete standard document for free.