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GB/T 3653.7-2020: Ferroboron - Determination of sulfur content - Infrared absorption method
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Ferroboron - Determination of sulfur content - Infrared absorption method
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GB/T 3653.7-2020
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Basic data | Standard ID | GB/T 3653.7-2020 (GB/T3653.7-2020) | | Description (Translated English) | Ferroboron - Determination of sulfur content - Infrared absorption method | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | H11 | | Classification of International Standard | 77.100 | | Word Count Estimation | 10,118 | | Date of Issue | 2020-03-06 | | Date of Implementation | 2020-07-01 | | Issuing agency(ies) | State Administration for Market Regulation, China National Standardization Administration | GB/T 3653.7-2020: Ferroboron - Determination of sulfur content - Infrared absorption method---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Ferroboron - Determination of sulfur content - Infrared absorption method
ICS 77.100
H11
National Standards of People's Republic of China
Determination of boron, iron and sulfur content
Infrared absorption method
2020-03-06 released
2020-07-01 implementation
State Administration for Market Regulation
Issued by the National Standardization Management Committee
Foreword
GB/T 3653 is divided into 7 parts.
---GB/T 3653.1 Methods for chemical analysis of ferroboron and alkaline titration for the determination of boron content;
---GB/T 3653.2 Methods for chemical analysis of ferro-boron gas volumetric method for the determination of carbon content;
---GB/T 3653.3 Method for chemical analysis of ferro-boron with perchloric acid dehydration gravimetric method for the determination of silicon content;
---GB/T 3653.4 Determination of boron, iron and aluminum content by EDTA titration;
---GB/T 3653.5 Method for chemical analysis of boron-iron and chromatographic separation barium sulfate gravimetric method for the determination of sulfur content;
---GB/T 3653.6 Methods for chemical analysis of boron and iron. Antimony phosphomolybdenum blue photometric method for the determination of phosphorus content;
---GB/T 3653.7 Determination of boron, iron and sulfur content by infrared absorption method.
This part is Part 7 of GB/T 3653.
This section was drafted in accordance with the rules given in GB/T 1.1-2009.
This part was proposed by the China Iron and Steel Association.
This part is under the jurisdiction of the National Pig Iron and Ferroalloy Standardization Technical Committee (SAC/TC318).
Drafting organizations of this section. Maanshan Iron and Steel Co., Ltd., Qingdao Bozheng Inspection Technology Co., Ltd., Anhui Changjiang Iron and Steel Co., Ltd.
The company, Shanghai Lirun Mechanical and Electrical Equipment Co., Ltd., Anhui Jiangnan Iron and Steel Material Quality Supervision and Inspection Co., Ltd., Qingdao Siwenke testing technology has
Co., Ltd., China Metallurgical Construction Research Institute Co., Ltd., Metallurgical Industry Information Standards Research Institute.
The main drafters of this section. Song Zufeng, Zhijiangxia, Zhu Tao, Lu Jun, Chen Rong, Kan Bin, Fan Yu, Long Rucheng, Wang Chenweng, Guo Shiguang, Wang Zhongle,
Lu Chunsheng.
Determination of boron, iron and sulfur content
Infrared absorption method
Warning---The personnel using this section should have formal laboratory work experience. This section does not point out all possible security issues.
The user is responsible for taking appropriate safety and health measures and ensuring compliance with the conditions stipulated by relevant national laws and regulations.
1 Scope
This part of GB/T 3653 specifies the infrared absorption method to determine the sulfur content in ferroboron.
This section applies to the determination of sulfur content in ferroboron. Measuring range (mass fraction). 0.0020%~0.025%.
2 Normative references
The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this article
Pieces. For undated references, the latest version (including all amendments) applies to this document.
GB/T 4010 Collection and preparation of samples for chemical analysis of ferroalloys
GB/T 6379.1 Measurement methods and accuracy of results (accuracy and precision) Part 1.General principles and definitions
GB/T 6379.2 Accuracy of measurement methods and results (accuracy and precision) Part 2.Determine the repeatability of standard measurement methods
Basic methods of sex and reproducibility
GB/T 8170 Numerical rounding rules and the expression and determination of limit values
3 Principle
The sample is heated and burned in the oxygen stream of a high-frequency induction furnace, and the generated sulfur dioxide is carried by the oxygen to the measuring chamber of the infrared analyzer.
Sulfur absorbs infrared energy of a certain wavelength, and its absorption energy is proportional to the concentration of sulfur dioxide. According to the sulfur dioxide infrared detector to receive energy
The change in sulphur can be measured.
4 Reagents and materials
Unless otherwise specified, only reagents confirmed to be analytically pure are used in the analysis.
4.1 Acetone, analytically pure.
4.2 Magnesium perchlorate, anhydrous, granular.
4.3 Caustic soda asbestos, granular.
4.4 Glass wool.
4.5 Tungsten particles, the sulfur content is less than 0.0005%, and the particle size is 0.8mm~1.4mm.
4.6 Tin particles, sulfur content less than 0.0005%, particle size 0.4mm ~ 0.8mm, if necessary, use acetone (4.1) to clean the surface, and at room temperature
dry.
4.7 Pure iron, purity greater than 99.98%, sulfur content less than 0.0005%, particle size 0.8mm ~ 1.6mm.
4.8 Oxygen, the purity is greater than 99.95%, if other grades of oxygen can obtain a low and consistent blank, it can also be used.
4.9 The impurity (water and oil) content of power gas, nitrogen or compressed air is less than 0.5%.
4.10 Ceramic crucible, diameter × height. 23mm × 23mm or 25mm × 25mm, and in a high temperature heating furnace not lower than 1050 ℃
After burning for more than 2 hours and cooling to room temperature, immediately place it in a desiccator for sealed storage or burn it in an oxygen furnace not lower than 1500℃.
4.11 Crucible tongs.
5 Apparatus and equipment
5.1 Infrared absorption sulfur analyzer
Infrared absorption sulfur analyzer (sensitivity 1.0×10-6), its device is shown in Figure 1.
5.2 Air source
5.2.1 The carrier gas system includes an oxygen container, a two-stage pressure regulator and a timing control part to ensure the supply of appropriate pressure and rated flow.
5.2.2 Power gas source system includes power gas (4.9), two-stage pressure regulator and sequence control to ensure the supply of suitable pressure and rated flow
section.
5.3 High-frequency induction furnace
Should meet the requirements of the melting temperature of the sample.
5.4 Control system
Control functions include automatic loading and unloading of crucibles and furnace platform lifting, automatic cleaning, analysis condition selection and setting, analysis process monitoring and alarming
The collection, calculation, correction and processing of broken and analyzed data.
5.5 Measuring system
It is mainly composed of an electronic balance (with a sensitivity not greater than 1.0 mg) controlled by a microprocessor, an infrared analyzer and electronic measuring components.
6 Take samples
Take samples according to GB/T 4010, the samples should pass through 0.088mm mesh.
7 Analysis steps
7.1 Sample
Weigh 0.20g sample, accurate to 0.001g.
7.2 Number of determinations
The same sample should be tested independently at least twice.
7.3 Blank test
Weigh 0.2g tin pellets (4.6), 0.5g pure iron (4.7) and 1.5g tungsten pellets (4.5) into a ceramic crucible (4.10).
Road, measured according to 7.5.Repeat the measurement until the reading is relatively stable. Record the last 3 readings, calculate the average, and refer to the instrument
In the manual, input the average value into the infrared absorption sulfur analyzer, and the instrument will electronically compensate the blank value when measuring the sample.
7.4 Calibration test
7.4.1 According to the sulfur content of the sample to be tested, select the corresponding range or channel, and select at least two standard samples (standard sample sulfur content range
The range should cover the sulfur content of the sample to be tested), and the calibration should be carried out in sequence.The fluctuation of the measured result should be within the range of the reproducibility limit R to confirm the line of the system.
Otherwise, the linearity of the system should be adjusted according to the instrument manual.
7.4.2 When the analysis conditions change, if the instrument has not been preheated to 1h, and the blank value of the oxygen source, crucible or flux has changed, it should be renewed.
Determine the blank and correct.
7.5 Determination
7.5.1 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 and the comparison level
(Or setting number) setting, etc.
7.5.2 Place the sample (7.1) in a ceramic crucible (4.10) pre-filled with 0.2g tin particles (4.6), and evenly cover 0.5g pure iron (4.7) and
1.5g tungsten particles (4.5), operate according to the instrument manual, start the analysis and read the results.
7.6 Expression of analysis results
The range of the two independent analysis results of the same sample is not greater than the repeatability limit r, and the arithmetic mean value is taken as the analysis result. in case
The range of two independent analysis results is greater than the repeatability limit r, then the number of measurements is added in accordance with the provisions in Appendix A and the analysis results are determined.
The analysis result is rounded to two significant digits according to GB/T 8170.
8 Precision
The precision test of this part was conducted by 8 laboratories in.2018, and the sulfur content of 5 levels was measured; each laboratory measured each
The sulfur content of each level is measured 3 times under the repeatability conditions specified in GB/T 6379.1.
See Appendix B for the original data (measurement results) reported by each laboratory.
According to GB/T 6379.2, the measurement results obtained are statistically analyzed, and the precision is shown in Table 1.
Note. w---Sulfur content in the sample, %.
9 Test report
The test report should include the following.
a) Laboratory name and address;
b) Date of release of test report;
c) The standard number of this part;
d) Detailed instructions necessary for sample identification;
e) Analysis results;
f) The number of determinations of the result;
g) Any abnormal characteristics in the measurement process and the analysis results of the sample or certification standard that may not be specified in this section
Any operation that has an impact.
Appendix A
(Normative appendix)
Flowchart of the procedure for receiving the analysis value of the test sample
The flow chart of the procedure for receiving the analysis value of the test sample is shown in Figure A.1.
Figure A.1 Flow chart of the procedure for receiving the analysis value of the test sample
Appendix B
(Informative appendix)
Raw data of precision test
The raw data of the precision test is shown in Table B.1.
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