GB/T 4701.10-1988 Chemical analysis methods for ferrotitanium - Determination of sulfur content by infrared absorption method

This standard is applicable to the determination of sulfur content in ferrotitanium. Determination range: 0.005% to 0.045%. This standard complies with GB 1467-78 "General Principles and General Provisions for Chemical Analysis Methods of Metallurgical Products". GB/T 4701.10-1988 Chemical analysis method for ferrotitanium - Determination of sulfur content by infrared absorption method GB/T4701.10-1988 Standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Methods for chemical analysis of ferotltanium
Determinadon of sultur content by infrared absorption method
Methods for chemical analysis of ferotltaniumThe infrared absorption method for thedeterminadon of sultur contentThis standard is applicable to the determination of sulfur content in chain iron. Determination range: 0.005%~0.045%. UDC669.15°295
GE 4701.10—88
This standard complies with GB146778 "General Principles and General Provisions of Standards for Chemical Analysis Methods of Metallurgical Products". 1 Summary of the method
The sample is heated and burned in the oxygen flow of a high-frequency induction furnace. The generated sulfur dioxide is carried by oxygen to the measuring chamber of the infrared analyzer. Sulfur dioxide absorbs infrared energy of a specific wavelength. Its absorption energy is proportional to the concentration of sulfur dioxide. Sulfur can be measured based on the changes in the detector's energy receiving disk.
2 Reagents and materials
2.1 Magnesium peracid: anhydrous, granular,
2.2 Caustic soda asbestos: granular.
2.3 Glass wool.
2.4 Tungsten particles: sulfur content less than 0.0002%, particle size 0.8~1.4mm. 2.5 Tin particles: sulfur content less than 0.0003%, particle size 0.4~0.8m. 2.6 Pure deficiency, purity greater than 99.80%, sulfur content less than 0.002%, particle size 0.8~1.68 mm. 2.7 Oxygen: purity greater than 99.95%, other grades of oxygen can also be used if low and consistent blank values ​​can be obtained. 2.8 Power gas source, nitrogen or compressed air, its impurities (water and oil) are less than 0.6%. 2.9 Quality: X*, mm, 23×2325×25, and burn in a furnace at a temperature higher than 1200℃ for 4h: or burn in oxygen until the blank value is the lowest.
2.10 Crucible.
3 Instruments and equipment
3.1 Infrared absorption sulfur analyzer (sensitivity is 1.0ppm) The device is shown in the figure below.
Approved by the Ministry of Metallurgical Industry of the People's Republic of China on February 2, 1988, and implemented on March 1, 1989
GE 4701. 10 -- 88
1—Oxygen cylinder 12—Two-stage pressure regulator + 3—Gas washing bottle 14, 9—Dry gas pipe + 5—Pressure regulator; 6—High temperature combustion furnace 7—Combustion pipe; 8—Dust removal group, 10—Vegetable quantity controller; 11—Sulfur difluoride infrared detector 3.1.1 Gas washing bottle (3): Contains caustic soda asbestos (2.2). 3.1.2 Dry gas pipe (4.9): Contains perchloric acid (2.1). 3.2 Gas source
3.2.1 The carrier gas system includes an oxygen container, a two-stage pressure regulator, and a timing control part that ensures the provision of appropriate pressure and rated flow. 3.2.2 The power gas source system includes power gas (nitrogen or compressed air), a two-stage pressure regulator and a timing control part to ensure the provision of appropriate pressure and rated flow.
3.3 The high-frequency induction furnace
should meet the requirements of the melting temperature of the sample.
3.4 ​​Control system
3.4.1 The microprocessor system includes a central processing unit, a memory, a keyboard input device, an information center display screen, an analysis result display screen and an analysis result printer.
3.4.2 The control functions include automatic loading and unloading of the crucible and the lifting of the furnace, automatic cleaning and analysis condition selection and setting, monitoring of the analysis results and alarm interruption, analysis data collection, calculation, correction and processing, etc. 3.5 The measurement system
is mainly composed of an electronic balance (sensitivity is not large +1.0mg) controlled by a microprocessor, an infrared analyzer and electronic measuring elements. 4 The test samples
should all pass through a 0.125 mm sieve. 5 Analysis steps
5.1 Sample quantity
Weigh 0.500g of sample.
5.2 Blank test
Weigh 0.500g of pure iron standard sample with sulfur content less than 20ppm, place it in (2.9) pre-filled with 0300±0.005B pellets (2.5), cover it with 1.500±0.005g of tungsten pellets (2.4), and measure according to 5.5 on the same range or channel, repeat enough times until a low and relatively consistent reading is obtained (the blank value should be equal to the difference between the measured sulfur content and the known sulfur content of the standard sample). Record at least three readings, calculate the average blank value, and enter the blank value into the analyzer with reference to the instrument manual. The instrument will then perform electronic compensation for the blank value when measuring the sample.
5.3 Analysis preparation
GB 4701. 1088.
5.3.1 Check the instrument according to the instrument manual to ensure that the instrument is in a normal and stable state. 5.3.2 Select and set the best analysis conditions. 5.3.3 Perform two test tests with standard samples and flux according to 5.5 to determine whether the instrument is normal. 5.3.4 Weigh 0.500 of the standard sample (or pure iron standard sample) with a sulfur content of about 0.0025%. If the sample is below, measure it according to 5.5. The result fluctuation should be within the range of ±0.0003%. Otherwise, adjust the instrument sensitivity according to the instrument requirements. 5.4 Calibration test
5.4.1 According to the sulfur content of the sample to be tested, select the corresponding range or channel, and select three standard samples of the same type (the sulfur content of the sample to be tested should fall within the sulfur content range of the three selected standard samples), and calibrate in sequence. The fluctuation of the 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. 5.4.2 Different ranges or channels should be measured and calibrated separately. 5.4.3 When the analysis conditions change, such as the instrument has not been preheated for 1 hour, the blank value of the oxygen source, crucible or flux has changed, it is required to re-measure the blank and calibrate
5.5.1 According to the sulfur content range of the sample to be tested, select the best analysis conditions of the instrument, such as the combustion integration time of the instrument, the setting of the comparison level (or set number), etc. wwW.bzxz.Net
5.5.2 Place the sample (5.1) in a crucible (2.9) pre-filled with 0.30g of pick axe (2.5), cover it with 1.50g of tungsten axe (2.4), take the crucible with tongs and place it on the furnace stand, operate according to the instrument manual, start analysis and obtain the results. 6 Allowable Difference
The difference in analysis results between laboratories should not be greater than the allowable difference listed in the following table. %
Additional Notes:
0. 005 ~~0. 015
>0. 015 ~ 0. 025
>0. 025 ~0. 045
This standard was drafted by Qinglin Ferroalloys.
The main drafter of this standard is Chang Yanfu.
From the date of implementation of this standard, the former Ministry of Metallurgical Industry standard YB581 This standard level mark GB 4701.10--88I is added
65 Titanium-iron chemical analysis method\work degree.
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