SJ 3240-1989 Determination of trace hydrogen and methane in electronic grade argon Argon ionization gas chromatography SJ3240-1989 standard download decompression password: www.bzxz.net

Standard of the Ministry of Machinery and Electronics Industry of the People's Republic of China Method for the determination of trace hydrogen and methane in electronic grade argon Argon ionization gas chromatography
1 Subject and scope of application
1.1 Subject content
SJ3240-—89
This standard specifies the hydrogen ionization gas chromatography analysis method for trace hydrogen and methane in electronic grade argon. 1.2 Scope of application
This standard is applicable to the determination of trace hydrogen and methane in electronic grade argon. When the injection volume is 3ml, the determination range is 0.5~25ppm for hydrogen and 0.3~20ppm for methane. 2 Principle of the method
2.1 This method is an ionization detector gas chromatography method using high-purity fluorine as carrier gas. 2.2 The hydrogen and methane in the analyzed gas are separated from other impurities by the molecular sieve chromatographic column and then enter the argon ionization detector. 2.3 The argon ionization detector uses a fluorine source as energy. The beta particles radiated by the fluorine source excite the argon molecules to generate metastable argon. The metastable hydrogen atoms with a constant energy disk ionize the organic vapor molecules with lower excitation energy than hydrogen to produce base flow. When the impurity molecules enter the ionization chamber, a quenching effect occurs, causing the base flow to decrease. Under certain conditions, the base flow decrease value is proportional to the impurity concentration, so the impurity concentration can be measured. 3 Instruments and materials
. Hydrogen ionization gas chromatograph;
b. Index diluter;
c. Argon purifier with 10~15 mesh aluminum 16 getter; d. Injection valve:
e. Chromatographic column stainless steel tube, inner diameter 2mm, length 1~2m, filled with 4060 mesh 5A or 13X molecular sieve;
f. Recorder 0~1mv, or microprocessor;
g. Pure fluorine meets GB4842; wwW.bzxz.Net
h. Organic gas source stainless steel tube, inner diameter 2mm, length 15cm, filled with pure trichlorobenzene, 4 Determination flow chart and test Conditions
4.1 Flow chart is shown in Figure 1
Approved by the Ministry of Machinery and Electronics Industry of the People's Republic of China on March 20, 1989 and implemented on March 25, 1989
Pure rat in one purifier
4.2 Test conditions
SJ3240--89
Inlet sample reading
Exponential selector
Rice release standard gas
Factory sample gas
One color mushroom cake
High voltage electrical appliance
Figure 1 Flow chart of oxygen ionization gas chromatography
8. Column chamber temperature (15~35C)
b. Detector temperature room temperature (15~35℃);
c. Purification furnace temperature
First-level purification 700℃; Second-level purification 400℃; d. Detector high voltage
250~500V;
c. Collect extremely high resistance 10n;
f. Carrier gas flow rate 40ml/min;
g. Dilution gas flow rate
Standard gas injection volume
60ml/min;
i. Sample gas injection volume
5 Operation steps
5.1 Before starting the instrument, strictly check the sealing of the gas circuit. Organic gas source
Detector
Micro power amplifier upgrade
Recorder
5.2 Turn on the purification furnace heating switch, connect the host, micro current amplifier and high voltage power supply; after the purification furnace temperature reaches the set value, turn the organic gas valve to allow the carrier gas to flow through trichlorobenzene and then enter the detector, and adjust the carrier gas flow rate. Turn on the recorder and start the test after the baseline is stable. 5.3 Standard Adjust the dilution gas flow rate to the set value and turn on the diluter switch. Inject 0.61 ml of standard gas through the six-way valve, and then inject 1 ml of diluted standard gas through the injection valve every 3 minutes. 5.4 Sample gas test is injected through the six-way valve, record the peak height and retention time, and repeat three times. 6 Result calculation
6.1 Standard calculation
a The initial concentration C of the diluted standard gas. Calculate according to formula (1): Ca=0.61.C
SJ3240-89
Where: Co is the initial concentration of the diluted standard gas, ppm; C- is the standard gas concentration;
V- is the volume of the dilution bottle, ml;
0.61 is the volume of the standard gas entering the diluter, m1. b. The average dilution factor is calculated according to formula (2):
wherein: n is the number of times the dilution standard gas is injected;
h is the standard peak height at the i-th injection, mm. h
c, the concentration of hydrogen or methane in each injection of standard gas C, is calculated according to formula (3): Ci
wherein: C is the concentration of hydrogen or methane in the standard gas, ppm; d. The response coefficient F is ppm/mm,
........(2)
The standard curve is drawn with h as the vertical axis and C as the horizontal axis. The inverse of its slope is c
F, see Figure 2.
Figure 2 Standard curve
The concentration of hydrogen and methane in the sample gas C is calculated according to formula (4): 8
SJ3240--89
wherein: C is the concentration of hydrogen and methane in the same gas! ' concentration, ppm; h#- is the peak height of the component in the sample gas, mm; Vb- is the injection volume of the standard gas, ml; V#- is the injection volume of the sample gas, ml. Note: The calculation formula is derived from Appendix A of SJ3237-89 Determination of trace oxygen in electronic grade hydrogen by hydrogen ionization gas chromatography. 7 Analysis accuracy The relative average deviation of the three analysis results is less than 15%. 8 Test report The test report should include the following: Time, place, unit, date Sampling method and number Sample name Instrument type and model Test conditions and results Any abnormal phenomenon observed during the measurement Analyst signature.
Precautions
The detector atmosphere source must always have argon gas passing through it. The gas system must be hard-wired. Before use, the air tightness of each part must be strictly checked. 9.3
The carrier gas flow rate must be stable and consistent during a test. 9.4The dilution gas flow rate must be constant at the set value. The standard gas line and sample gas line must be fully purged before injection until there is no injection blank. 9.5
After the analysis is completed, turn off the organic gas.
The typical chromatogram is shown in Figure 3.
+（4）
Additional instructions:
SJ3240-89
Figure 3 Typical chromatogram of impurity analysis in electronic grade argon This standard was proposed by the Electronic Standardization Institute of the Ministry of Machinery and Electronics Industry. This standard was drafted by the Beijing Nonferrous Metals Research Institute. The main drafters of this standard are Cui Xizhong, Zhou Shaolian, Zhao Changchun and Yin Enhua. 5
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.