GB/T 4333.10-1990 Chemical analysis methods for ferrosilicon - Determination of carbon content by infrared absorption method

This standard specifies the infrared absorption method for the determination of carbon content. This standard is applicable to the determination of carbon content in ferrosilicon. Determination range: 0.025%~0.250%. GB/T 4333.10-1990 Chemical analysis method for ferrosilicon Determination of carbon content by infrared absorption method GB/T4333.10-1990 Standard download decompression password: www.bzxz.net

National Standard of the People's Republic of ChinabZxz.net
Chemical analysis method of ferrosilican-Thc
Determination of carbon content by infrared absorption method
Methods for chemical enalysis of ferrosilican-Thc Infrared ahsorption method for thedetermination of carbon cantent1 Subject content and scope of application
This standard specifies the determination of carbon content by infrared absorption method. This standard is applicable to the determination of carbon content in ferrosilicon. Determination range: 0.025%~0.250%. 2 Method summary
GB4333.10
The sample is heated and burned in the oxygen flow of a high-grained induction furnace. The generated carbon dioxide is carried by oxygen to the measurement chamber of the infrared analyzer. Carbon dioxide absorbs infrared energy of a specific wavelength. Its absorption energy is proportional to the concentration of carbon. The carbon scene can be measured according to the change in energy received by the detector. 3 Reagents and materials
3.1 Indole, the magnetic content of the residue after evaporation is less than 0.005%. 3.2 Magnesium perchlorate (anhydrous); granular.
3.3 Caustic soda asbestos: granular.
3.4 ​​Glass wool.
3.5 Tungsten granules; carbon content less than 0.02%, particle size 0.8~1,4 mm. 3.6 Tin granules: carbon content less than 0.002%, particle size 0.4~0.8mm. If necessary, clean the surface with acetone (3.1) and dry at room temperature. 3.7 Pure iron, carbon content less than 0.002%, crumbs. 3.8 Oxygen: purity greater than 99.95%, other grades of oxygen can also be used if a low and consistent blank can be obtained. 3.9 Power gas source nitrogen, argon or compressed air, the impurity content (water and oil) of which is less than 0.5%. 3.10 Quality (×h, mm; 23×23 or 25×25), burn in a high temperature heating furnace above 1200℃ for 4h or burn in oxygen until the white value is the lowest.
3. 11 Crucible tongs.
Apparatus and equipment
4.1 Infrared absorption carbon determination instrument (sensitivity is 1.0ppm) The device is shown in the figure. Approved by the State Administration of Technical Supervision on May 4, 1990 and implemented on January 1, 1991
GB 4333.10 - 90
Infrared absorption carbon analyzer device diagram
1—oxygen cylinder + 2·two-stage pressure regulator; 3—gas washing bottle: 4, 9—lower drying tube, 5-pressure regulator: 6—high induction furnace, 7 combustion tube, 8—deoxidizer, 10—flow controller: 11—converter for converting carbon monoxide to sulfur dioxide; 12—desulfurizer; 13—carbon monoxide red. External detector 4.7.7 Gas washing bottle (3) contains caustic soda asbestos (3.3) 4.1.2 Drying tube (4, 9), containing magnesium perchlorate (3.2). 4.2 Gas source
4.2.1 The carrier gas system includes an oxygen container, a two-stage pressure regulator and a timing control part to ensure the provision of appropriate pressure and rated flow. 4.2.2 The power gas source system includes power gas (nitrogen, argon or compressed air), two-stage pressure regulator and timing control part to ensure the provision of appropriate pressure and rated flow.
4.3 The high-frequency induction furnace
should meet the requirements of the melting temperature of the sample.
4.4 Control system
4.4.1 The microprocessor system includes central processing unit, memory, keyboard input device, information center display screen, analysis result display screen and analysis result printer, etc.
4.4.2 The control functions include automatic loading and unloading and furnace lifting, automatic cleaning, analysis condition selection and setting, analysis process monitoring and alarm interruption, analysis data collection, calculation, correction and processing, etc. 4.5 Measurement system
It is mainly composed of an electronic balance controlled by a microprocessor (the maximum sensitivity is not more than 1.0mg), an infrared analyzer and electronic measuring elements. 5 Samples
All samples should pass through a 0.125mm sieve.
6 Analysis steps
6.1 Test material
GB 4333. 10 --90
Weigh 0.200~0.250g of sample. Accurate to 0.001g. 6.2 Blank test
In (3.10) pre-filled with 0.400±0.005g of tin particles (3.6), cover 0.600±0.005g of pure iron (3.7) and 1.500±0.005g of tungsten particles (3.5), and measure according to 6.5 in the same range or channel. Repeat enough times until a low and relatively consistent reading is obtained. Record the minimum three readings, calculate the average value, and refer to the instrument manual to enter the average value into the analyzer. The instrument will then perform electronic compensation for the blank value when measuring the sample. 6-3 Analysis Preparation
6.3.1 Check and debug the instrument according to the instrument manual to ensure that the instrument is in a normal and stable state. 6.3.2 Select and set the best analysis conditions.
6.3.3 Use standard push samples and flux to conduct two test tests according to 6.5.1 and 6.5.2 to determine whether the instrument is normal. 6.3. 4 Weigh several portions of 0.250g of standard samples with a carbon content of about 0.050%, and measure them according to 6.5. The result fluctuation should be within 0.003%, otherwise the sensitivity of the instrument should be adjusted according to the instrument requirements. 6.4 Calibration test
6. 4. 1 According to the carbon content of the sample to be tested, select the corresponding range or channel, and select three standard samples of the same type (the carbon content of the sample to be tested should fall within the range of the carbon content of the selected three standard samples) for calibration in turn. The passiveness of the measured results should be within the allowable error range to confirm the linearity of the system, otherwise the linearity of the system should be adjusted according to the instrument manual. 6.4.2 The blank values ​​of different ranges or channels should be measured and calibrated respectively. 6.4.3 When the analytical conditions change, such as when the instrument has not been preheated for 1h, the oxygen source, or the blank value of the flux has changed, it is required to re-measure the blank and calibrate.
6.5 Determination
6.5.1 According to the carbon content range of the sample to be tested: Select the best analytical conditions of the instrument, such as the combustion integration time of the instrument, the setting of the comparison level (or set number), etc.:
6.5.2 Evenly place the weighed sample (6.1) in a crucible (3.10) pre-filled with 0.400 g of tungsten pellets (3.6), and cover it with 0.600 g of pure iron (3.7) and 1.500 g of tungsten pellets (3.5). Use tongs to take the crucible and place it on the crucible stand on the furnace table. Operate according to the instrument manual, start analysis and read the results. 7 Allowable Difference
The difference in analysis results between laboratories should not be greater than the allowable difference listed in the following table. %
0. 025 ~ 0. 070
20. 070 ~ 0. 120
>0,120~～0,250
Additional Notes:
This standard was proposed by the Ministry of Metallurgical Industry of the People's Republic of China and drafted by Xinyu Iron and Steel Plant.
The main drafters of this standard are Zhou Juhan, Wu Taibai, Liu Jinhua and Zhao Chengzhong. The level of this standard is marked as GB4333.10--90I.
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