SN/T 5250-2020 English PDF

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SN/T 5250-2020: (Determination of sulfur content in mineral products High-frequency combustion infrared absorption method)
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Basic data

Standard ID: SN/T 5250-2020 (SN/T5250-2020)
Description (Translated English): (Determination of sulfur content in mineral products High-frequency combustion infrared absorption method)
Sector / Industry: Commodity Inspection Standard (Recommended)
Classification of Chinese Standard: D04
Classification of International Standard: 73.060.01
Word Count Estimation: 10,179
Date of Issue: 2020-08-27
Date of Implementation: 2021-03-01
Regulation (derived from): General Administration of Customs Announcement No. 98 [2020]
Issuing agency(ies): General Administration of Customs

SN/T 5250-2020: (Determination of sulfur content in mineral products High-frequency combustion 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.
Determination of sulfur content in mineral products-High frequency combustion with infrared absorption method The People's Republic of China Entry-Exit Inspection and Quarantine Industry Standards Replace SN/T 2032-2007 2020-08-27 release 2021-03-01 implementation Issued by the General Administration of Customs of the People's Republic of China

Foreword

This standard was drafted in accordance with the rules given in GB/T 1.1-2009. This standard was proposed and managed by the General Administration of Customs of the People's Republic of China. Drafting organizations of this standard. Guiyang Customs of the People’s Republic of China, Dalian Customs of the People’s Republic of China, Nanjing of the People’s Republic of China Customs, Hohhot Customs of the People's Republic of China, Taiyuan Customs of the People's Republic of China. The main drafters of this standard. Zhou Fuqiang, Zhang Yanfu, Liu Tao, Wang Qiaoling, Liu Song, Zhao Ming, Li Chunping, Ran Fei, Luo Tianlin, Yang Puchen. Determination of sulfur content in mineral products High frequency combustion infrared absorption method

1 Scope

This standard specifies the high-frequency combustion-infrared absorption method for the determination of mineral products (iron ore, lead ore, tin ore, manganese ore, molybdenum ore, copper ore, tungsten Method for detecting sulfur in ore, chrome ore). This standard applies to high-frequency combustion of sulfur content in mineral products (iron ore, lead ore, tin ore, manganese ore, molybdenum ore, copper ore, tungsten ore, chrome ore) Measured by burning infrared absorption method, the measuring range is 0.005% to 55.0%. Note. This method can be used as a guideline test method with universal analytical procedures or techniques, which is convenient for laboratories to compile their internal detailed standards on this basis. Standardized operating procedures (SOP) or special applications, unless the parameters of the method are specified, the performance parameters in the method are for reference only and are not suitable for use as a laboratory The approved absolute quality control limit is used.

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 document. For documents, for undated reference documents, the latest version (including all amendments) is applicable to this document. GB/T.2007.2 General Rules for Sampling and Sample Preparation of Bulk Mineral Products Manual Sample Preparation Method GB/T 6379.2 Accuracy of measurement methods and results (accuracy and precision) Part 2.Determine the repeatability of standard measurement methods And the basic method of reproducibility (ISO 5725-2.1994, IDT) GB/T 6682 Analytical laboratory water specifications and test methods

3 Method summary

In the presence of flux, the mineral products are directly weighed or mixed and diluted by adding silica powder, and then enriched in a high-frequency infrared induction furnace. In the oxygen stream, it is heated and burned at high temperature, and the generated sulfur dioxide is carried by the oxygen to the measuring chamber of the infrared analyzer, and absorbs infrared energy of a specific wavelength. The absorption energy is proportional to its concentration, and the sulfur content is measured according to the change in the energy received by the detector.

4 Reagents and materials

Unless otherwise specified, the reagents are all analytically pure, and the experimental water is secondary water that meets the requirements of GB/T 6682. 4.1 Potassium sulfate. standard reagent, the content is greater than 99.95%, dried at 105 ℃ for 2 h, and then cooled in a desiccator for later use. 4.2 Silica powder. high purity, particle size less than 150 μm, sulfur content less than 0.0005%. 4.3 Pure iron flux. the sulfur content is less than 0.000 5%, and the particle size is 0.80 mm to 1.68 mm. 4.4 Tin particles. The sulfur content is less than 0.000 3%, and the particle size is 0.4 mm to 0.8 mm. 4.5 Tin capsule. 250 μL in capacity, 5 mm in diameter and 13 mm in length. 4.6 Tungsten particles. The sulfur content is less than 0.000 2%, and the particle size is 0.8 mm to 1.4 mm. 4.7 Magnesium perchlorate. granular. 4.8 Oxygen. purity ≥ 99.5%. 4.9 Power gas. nitrogen or compressed air. purity ≥ 99.5%. 4.10 Quartz wool. 5μm ~ 10μm in diameter.

5 Apparatus and equipment

5.1 High-frequency infrared carbon and sulfur analyzer (see Appendix A for instrument conditions). 5.2 Analytical balance. the sensitivity is 0.01 mg. 5.3 Analytical balance. Sensitivity 0.1 mg. 5.4 Mixing grinder. including grinding balls, with a volume of 25 mL to 50 mL, and a maximum oscillation frequency of 25 times/s. 5.5 High-temperature furnace. The maximum operating temperature is 1200°C. 5.6 Oven. The highest operating temperature is 300°C. 5.7 Porcelain crucible. burn it in a high temperature furnace at 110 0 ℃ for at least 4 h before use, cool it, and store it in a desiccator. 5.8 Micropipette (micropipette). 50 μL, 100 μL.

6 Sample preparation

6.1 Prepare the sample according to GB/T.2007.2, and the particle size of the sample should be less than 150 μm. 6.2 The sample is pre-baked at 100 ℃ for 2 hours, and then placed in a desiccator to cool to room temperature for later use. Note. The ore samples containing bound water should be roasted in a high-temperature furnace in advance.

7 Analysis steps

7.1 Preparation 7.1.1 Preparation of the instrument. turn on the instrument, warm up for 1 hour, check and debug the instrument, ensure that the instrument is in a normal and stable working state, and confirm The best working conditions. 7.1.2 Preparation before analysis. adjust and stabilize the instrument by burning several similar samples to be tested. 7.2 Preparation of low-content sulfur standard series Weigh the solid potassium sulfate (4.1) in a 50 mL volumetric flask according to Table 1, and dissolve it with water (see Appendix B for the saturated solubility of potassium sulfate), Mix to a constant volume and prepare each potassium sulfate standard solution. Use a micropipette (5.8) to take out the potassium sulfate standard solution and inject it into the solution. In a clean tin bag (4.5), bake in an oven at 80°C for 1 h, flatten and fold it, put it in a porcelain crucible (5.7), and cover with 0.5 g of pure iron (4.3) And 1.6 g tungsten particles (4.6), measured on the machine, as a standard working curve for the determination of low sulfur content. Note. At room temperature about 20°C, affected by the solubility of potassium sulfate, the preparation of the high point of the sulfur standard curve can be achieved by increasing the volume of the pipetting solution. 7.3 Preparation of high-content sulfur standard series Weigh the solid potassium sulfate (4.1) according to Table 2, put them into a porcelain crucible (5.7) pre-added with 0.2 g tin particles (4.4), and then cover 0.5 g pure iron (4.3) and 1.6 g tungsten particles (4.6), measured on the machine, as a standard working curve for the determination of high sulfur content. Note 1.The weighing amount of potassium sulfate does not need to be strictly in accordance with the requirements of Table 2, and it can reflect the gradient of the sulfur content accordingly. Note 2.According to the range of sulfur content in the sample to be tested, appropriate adjustments can be made when preparing the standard series. 7.4 Calibration According to the sulfur content of the sample to be tested, select two or more mineral samples with close and similar content to measure the accuracy of the results And precision, systematic linear adjustment, the fluctuation of the results of the certified reference material measured after calibration should be within its allowable error range, Used for subsequent sample analysis. 7.5 Sample analysis 7.5.1 Determination of the mass fraction of sulfur content in the range of 0.005% to 40.0% According to the range of the mass fraction of sulfur in the mineral sample, weigh the sample size (accurate to 0.0001 g) according to Table 3, and put it in the pre-added 0.2 g The porcelain crucible (5.7) of tin particles (4.4) is covered with 0.5 g pure iron (4.3) and 1.6 g tungsten particles (4.6), and the measurement is carried out on the machine. 7.5.2 Determination of the mass fraction of sulfur content in the range of 40.0% to 55.0% Weigh about 3.0 g (accurate to 0.0001 g) of high-purity silica powder (4.2) in a dry and clean 25 mL grinder (5.4) jar, Then add 0.5 g (accurate to 0.0001 g) sample, mix thoroughly in the jar for about 5 minutes, and transfer it to a 25 mL glass bottle. Call again Take 0.05 g (accurate to 0.0001 g) of the mixed sample and put it on the machine for measurement. 7.6 Blank test Except that no sample is added, in accordance with the added flux and working conditions of the sample test, determine the reagent blank results at least three times, whichever is equal Mean.

8 Calculation of analysis results

8.1 Specimens for direct testing Read the sulfur content directly from the instrument or from the standard curve, and the unit is percentage (%). 8.2 Samples diluted with silica powder Calculate the sulfur content according to formula (1), expressed in mass fraction.

9 Precision

The precision of this standard is to select multiple mineral samples with different sulfur content and conduct tests by more than 8 laboratories, according to GB/T 6379.2 Perform statistics, and the results are shown in Table 4.

Appendix A

(Informative appendix) Reference carbon and sulfur meter working conditions A.1 Oxygen pressure. 0.23 MPa ~ 0.30 MPa. A.2 Power air pressure. 0.25 MPa ~ 0.30 MPa. A.3 Analysis time. 40 S ~ 45 S. A.4 Catalyst temperature. 325 ℃ ~ 357 ℃. A.5 Incubator temperature. 46 ℃～50 ℃. A.6 Sulfur infrared detection cell voltage. 7.5 V ~ 8.1 V. A.7 Oscillation frequency. 18 MHz. A.8 System pressure. 740 mmHg ~ 790 mmHg. Note. The above-listed parameters are completed on the LECO CS 230C carbon and sulfur analyzer, which is only for reference and does not involve commercial purposes. Users are encouraged Try instruments of different manufacturers or models.

Appendix B

(Informative appendix) Saturated solubility of potassium sulfate ......

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