GB/T 8647.9-1988 Chemical analysis method for nickel - Determination of sulfur content by high frequency induction furnace combustion infrared absorption method GB/T8647.9-1988 standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Chemical analysis method of nickel
Determination of sulfur content by infrared absorption method after high frequency induction furnace combustionNickel--- Deternaination of sulphur content- Infra-redabsorption method after high frequency induction furnace combustionThis standard applies to the determination of sulfur content in nickel. Determination range: 0.0010%~0.050%. UDC 669. 24
GB 8647.9--88
This standard complies with GB146778 "General Principles and General Provisions for Chemical Analysis Methods of Metallurgical Products". This standard refers to the international standard ISO7526--1985 "Determination of sulfur content of nickel metal, ferronickel and nickel alloy by infrared absorption method after induction furnace combustion".
1 Method Summary
In the presence of flux, oxygen flow is introduced into the high-temperature induction furnace to make the sample burn at high temperature. Sulfur generates sulfur dioxide gas and enters the infrared absorption cell. The instrument automatically measures its absorption of infrared energy, calculates and displays the results. 2 Reagents and Materials
2.1 Purifier and Catalyst
2.1.1 Anhydrous magnesium perchlorate.
2.1.2 Caustic soda asbestos.
2.1.3 Glass wool.
2.1.4 Absorbent cotton.
2.1.5 Platinum-coated silica gel.
2.2 Flux
Low sulfur tungsten, tin: W+Sn(1g+0.2~0.25g). 2.3 Crucible
Ceramic crucible (±24mm×24mm), should be burned in oxygen flow >1100℃ for 1~1.5h before use, take out and cool in a desiccator for use (valid for two days).
2.4 Standard steel sample
2.4.1 Standard steel sample: sulfur content 0.067%~0.13%. 2.4.2 Standard steel sample or pure iron standard sample: sulfur content is about 0.002%. Note: It is best to use nickel standard sample for standard steel sample
3 Instrument
High frequency infrared gas analyzer (with electronic AC voltage regulator) Instrument working conditions refer to Appendix A.
High frequency furnace power: 1.0~2.5kW.
Frequency: >6.0 MHz.
Approved by China National Nonferrous Metals Industry Corporation on January 11, 1988 436
Implemented on January 1, 1989
Detector sensitivity: 1ppm
4 Analysis steps
4.1 Instrument preparation
GB 8647.9-88
Determine the measurement conditions according to Appendix A and prepare the instrument for use according to the instrument manual. 4.2 Instrument stability
4.2.1 Adjust and stabilize the instrument by burning several samples similar to the sample to be tested. 4.2.2 Cycle the instrument through oxygen several times and then adjust the blank to zero. 4.3 Calibrate the instrument
4.3.1 Weigh 0.500g of standard steel sample (2.4.1) and place it in (2.3), add flux (2.2). 4.3.2 Place the crucible on the support of the furnace, raise it to the burning position, and follow the "automatic" calibration steps in the instrument manual. Repeat 2 to 3 standard steel samples and pass the "automatic" calibration steps until the sulfur result is stable within the error range. Note: When selecting a standard steel sample, the sulfur content should be greater than the sulfur content of the sample being tested. 4.4 Calibrate the blank
4.4.1 Weigh 0.500g of standard steel sample (2.4.2) and place it in (2.3), add flux (2.2). 4.4.2 Place the crucible on the support of the furnace, raise it to the burning position, and follow the "automatic" calibration steps in the instrument manual. Repeat 3 to 5 steel samples to obtain an average result with good reproducibility. Deduct the percentage of sulfur in the standard steel sample by "automatic" calibration blank, and store the blank value in the computer (blank value should be 0.0005%). 4.4.3 Repeat the determination of the standard steel sample according to 4.3. The determination result should be stable within the error range. Then select a standard sample with the same sulfur content as the sample to be tested for re-testing.
4.5 Determination
4.5.1 Weigh 0.5008 sample and place it in (2.3), add flux (2.2). 4.5.2 Place the crucible on the support of the furnace, raise it to the burning position, and operate according to the "automatic" analysis steps in the instrument manual. After the instrument automatically deducts the blank value, it displays and prints out the percentage of sulfur. 5 Allowable Difference
The difference in analysis results between laboratories should not be greater than the allowable difference listed in the following table. %
0. 001 0-~0. 002
>0. 002~0. 005
>0. 005~0. 010 0
>0.010～0. 030
≥0. 030~- 0. 050
Allowance difference
GB8647.9--88
Appendix A
Instrument working conditions
(reference part)
The reference working conditions for determining sulfur using LECOCS-344 high-frequency infrared analyzer are as follows: Input oxygen pressure
MPa(psi,kgf/ cm' )
System gas pressure
MPa(psi,kgf/ cm )
99.5%(35~37,2.5~2.6)
Additional Notes:
(12,0.85)
This standard is under the technical jurisdiction of Beijing Mining Research Institute. Shortest Analysis TimebZxz.net
Pneumatic Air Flow
This standard was drafted by Beijing Mining Research Institute and Jinchuan Nonferrous Metals Company. This standard was drafted by Beijing Mining Research Institute. The main drafters of this standard are Xu Cuiduan and Huang Yuehua. Oxygen Flow
From the date of implementation of this standard, the former Ministry of Metallurgical Industry Standard YB128-76 "Nickel Chemical Analysis Method" will be invalid. 438
Comparison Level
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