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HJ 769-2015 English PDF

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HJ 769-2015: Determination of total sulfur in coal. Eschka-Ion chromatography method
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Basic data

Standard ID HJ 769-2015 (HJ769-2015)
Description (Translated English) Determination of total sulfur in coal. Eschka-Ion chromatography method
Sector / Industry Environmental Protection Industry Standard
Word Count Estimation 8,856
Date of Issue 2015-11-20
Date of Implementation 2015-12-15
Quoted Standard GB/T 212.3; GB/T 474; GB/T 475; GB/T 1997
Regulation (derived from) Ministry of Environment Announcement 2015 No.73
Issuing agency(ies) Ministry of Ecology and Environment
Summary This Standard specifies the determination of total sulfur in coal Ai Shika - Ion Chromatography. This Standard applies to the determination of anthracite, bituminous coal, lignite and coke in total sulfur. When the sample volume is 1.0 g, burning the volume to 250 ml, injection volume 25 ��l, this standard detection limit of 0.02%, detection limit is 0.08%.

HJ 769-2015: Determination of total sulfur in coal. Eschka-Ion chromatography method

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Determination of total sulfur in coal.Eschka-Ion chromatography method National Environmental Protection Standard of the People 's Republic of China Determination of total sulfur in coal Escherichia - ion chromatography Determination of total sulfur in coal -Eschka-Ion chromatography method 2015-11-20 release 2015-12-15 implementation release Ministry of Environmental Protection Directory Preface .ii

1 Scope of application

2 normative reference documents

3 Principle of the method

4 reagents and materials 1 5 instruments and equipment 2 6 Sample 2

7 Analysis steps

8 results are calculated and expressed

9 precision and accuracy

Quality assurance and quality control

Foreword

In order to implement the Environmental Protection Law of the People's Republic of China and the Law of the People's Republic of China on the Prevention and Control of Atmospheric Pollution, Protection of human health, standardize the determination of total sulfur content in coal, the development of this standard. This standard specifies the determination of total sulfur content in coal by escroine-ion chromatography. This standard is the first release. This standard is organized by the Ministry of Environmental Protection Science and Technology Standards Division. The main drafting of this standard. Liaoning Province Environmental Monitoring Experimental Center, Environmental Protection Department of Environmental Standards Institute. The standard verification unit. Dalian Environmental Monitoring Center, Anshan City Environmental Monitoring Center Station, Fushun City Environmental Monitoring Center Station, Yingkou City Environmental Monitoring Center Station, Tieling City Environmental Protection Monitoring Station, Huludao City Environmental Protection Monitoring Center Station. The Environmental Protection Department of this standard approves on November 20,.2015. This standard is implemented as of December 15,.2015. This standard is explained by the Ministry of Environmental Protection. Determination of Total Sulfur in Coal - Ash Chromatography - Ion Chromatography

1 Scope of application

This standard specifies the determination of total sulfur content in coal by escroine-ion chromatography. This standard applies to the determination of total sulfur in anthracite, bituminous coal, lignite and coke. When the sampling volume is 1.0 g, the calcination volume is 250 ml and the injection volume is 25 μl, the detection limit of this method is 0.02% The lower limit is 0.08%.

2 normative reference documents

The contents of this standard refer to the following documents or their terms. Those who do not specify the date of the reference file, the effective version of the appropriate For this standard. Methods for industrial analysis of coal - Determination of moisture content GB/T Method for preparing GB/T 474 coal samples GB/T 475 Method for artificial extraction of commercial coal samples GB/T.1997 Coke Specimen Preparation and Preparation

3 Principle of the method

The coal sample and Aishi card reagent mixed burning, coal sulfur sulfate, sulfate with alkaline eluent into the anion The column was separated in the form of sulfate (SO42-) and detected by conductivity detector. According to the quality of sulfate Total sulfur content in coal.

4 reagents and materials

Unless otherwise stated, analytical pure chemical reagents conforming to national standards are used in the analysis, and the test water is freshly prepared. Ion water. 4.1 Light Magnesium Oxide (MgO). Analytical purity. 4.2 anhydrous sodium carbonate (Na2CO3). analytical grade. 4.3 Aceka Reagent. Mix 2 parts by weight of light magnesium oxide (4.1) with 1 part by mass of anhydrous sodium carbonate (4.2) Grinding to a particle size of less than 0.2 mm, the room temperature stored in a closed dryer. 4.4 Sulfuric acid standard stock solution. ρ (SO42 -) = 1 000 μg/ml. Weigh 1.814 0 g potassium sulfate (105 ± 5 ℃ drying 2 h) dissolved in water, into the 1 000 ml volumetric flask, water volume, Shake well Stored in polyethylene bottles, 0 ~ 4 ℃ frozen storage for 6 months. You can also purchase commercially available standard solutions. 4.5 Sulfuric acid standard liquid. ρ (SO42 -) = 100 μg/ml. Remove 10.00 ml of sulfate standard stock solution (4.4), in 100 ml volumetric flask, with water volume, shake. Stored in Polyethylene bottles, temporary with the current allocation. 4.6 filter paper. the speed of qualitative filter paper. 4.7 Filter. A pore size of 0.45 μm acetate fiber microporous membrane (can be used with the syringe). 4.8 syringes. 10 ml. 4.9 Eluent stock solution. C (KOH) = 0.20 mol/L. Weigh 5.611 g potassium hydroxide (105 ± 5 ℃ drying 2 h) dissolved in water, into the 500 ml volumetric flask, water volume, shake uniform. Stored in polyethylene plastic bottles. 4.10 Rinse the use of liquid. C (KOH) = 0.02 mol/L. Remove the eluent stock solution (4.9) 100.00 ml in a 1 000 ml volumetric flask, shake with water, shake. Note 1. Prepare the eluent according to the instrument type and column conditions. If the instrument model supports automatic generation of eluent, it can be automatically generated.

5 instruments and equipment

Unless otherwise stated, all Class A glass gauges conforming to national standards are used for analysis. 5.1 ion chromatograph. with conductivity detector. 5.2 Columns. Anion Separation Columns and Anion Protection Columns. 5.3 muffle furnace. with temperature test instrument temperature, can be heated to 900 ℃, adjustable temperature and ventilation. 5.4 porcelain crucible. capacity 30 ml. 5.5 Analytical Balance. Accuracy of 0.000 1 g. 5.6 Common laboratory equipment and equipment.

6 samples

6.1 Collection and storage of samples In accordance with the relevant provisions of GB/T 475 for coal sample collection, in accordance with the relevant provisions of GB/T.1997 for coke collection. Samples should be stored in a non-absorbent, airtight sealed container and placed in a cool place. 6.2 Preparation of samples In accordance with the relevant provisions of GB/T 474 for the preparation of coal samples, in accordance with the relevant provisions of GB/T.1997 coke preparation. 6.3 Preparation of the sample 6.3.1 Weigh coal sample 1 g (nominal to 0.000 2 g), Escherichia reagent (4.3) 2 g (nominal to 0.01 g), placed in 30 ml Porcelain crucible (5.4) after mixing, and then 1 g (called quasi to 0.01 g) Eskka reagent (4.3) covered. 6.3.2 The porcelain crucible into a well-ventilated muffle furnace (5.3), in 1 h ~ 2 h gradually heated to 800 ℃ ~ 850 ℃, And after 1 h ~ 2 h to remove the crucible, cooled to room temperature. 6.3.3 with a glass rod in the porcelain crucible in the burning material stir loose, mashed (if not burned coal particles, should be 800 ℃ ~ 850 ℃ Continue to burn 0.5 h), and then transferred to the 250 ml beaker burned, with hot water rinse porcelain crucible inner wall, lotion into the burning Cup, then add 100 ml just boiled distilled water, stir well. So there are still black coal particles floating, this determination is invalid. 6.3.4 Wash the lotion with medium speed qualitative filter paper (4.6) by pouring method and rinse it with hot water 3 times. The residue into the filter paper, And then wash the filter paper with hot water at least 10 times, full rinse after the total volume of not more than.200 ml. Wash the liquid to cool to room temperature 250 ml volumetric flask. The washings were analyzed by means of a filter (4.7). Note 2. Escherichia reagents must be mixed with coal samples evenly. Note 3. mixing the coal sample with the escatch reagent After burning the residue with hot water, be sure to carefully rinse the filter paper so that the sulfate Attached to the filter paper, resulting in low measurement results. Note 4. For unknown concentration samples, dilute 25 to 50 times before analysis, and then select the appropriate dilution factor based on the results Injection analysis. Note 5. hot water temperature above 60 ℃. 6.4 Preparation of blank samples The preparation of a blank sample was carried out in the same manner as in the preparation of the sample (6.3) except that no coal sample was added. 6.5 Determination of water content of samples The moisture content of coal samples was determined according to the relevant provisions of GB/T 212.3.

7 Analysis steps

7.1 Instrument reference conditions According to the instrument manual operation of the instrument, the instrument work reference conditions are as follows. Name and concentration of eluent. KOH 0.02 mol/L. Eluent flow rate. 1.00 ml/min. Suppressor current. 50 mA. Injection volume. 25 μl. 7.2 Drawing of calibration curves A standard series of sulphates at concentrations of 1.00, 1.00, 5.00, 0.00, 15.00, 25.00, 50.00 μg/ml The standard series of samples from the low concentration to high concentration followed by injection, injection volume of 25 μl, get different concentrations of sulfate chromatograms. With the sulfate concentration (μg/ml) as the abscissa, the peak area (or peak height) as the ordinate, draw the calibration curve. Sulfate ion The chromatogram is shown in Fig. Figure 1 Sulfate ion chromatogram 7.3 Determination of samples The peak area (or peak height) of the sample was recorded by plotting the same chromatographic conditions and procedures as the calibration curve. 7.4 blank test The determination of the blank sample was carried out according to the procedure of 7.3. Calculation and representation of results 8.1 Results calculation The total sulfur content (ω) in the air-dry coal samples is calculated according to the formulas (1), (2) and (3). 8.2 The result is shown When the result is less than 1.00%, the result is retained to 2 decimal places; if the value is greater than or equal to 1.00%, the result is retained 3 Bit effective number.

9 precision and accuracy

9.1 precision Six laboratories carried out six replicates of uniform samples with sulfur content of 0.06% in coal. the relative standard deviations in the laboratory The relative standard deviation between the two groups was 0.67%. The repeatability limit was 0.01% and the reproducibility limit was 0.02%. Six laboratories carried out six replicates of uniform samples with a sulfur content of 0.43% in coal. the relative standard deviations in the laboratory . 1.0% ~ 3.4%; the relative standard deviation between the laboratory. 1.0%; repeatability limit. 0.03%; reproducibility limit. 0.18%. Six laboratories carried out six replicates of uniform samples with a sulfur content of 1.42% in coal. the relative standard deviations in the laboratory The relative standard deviation was. 1.1%; the repeatability limit was 0.07%; the reproducibility limit was 0.16%. 9.2 Accuracy (0.96 ± 0.03)%, (1.14 ± 0.03)% of the certified sulfur in coal in six laboratories The relative error was. -1.8% ~ 0%, - 3.1% ~ 0%, - 0.88% ~ 2.6%, the relative error was The final values were. -0.60% ± 1.9%, -1.4% ± 2.6%, 1.2% ± 2.4%. 10 quality assurance and quality control 10.1 blank test Each batch of samples at least two laboratory blanks, the blank value should not exceed 0.15%. Otherwise, the cause should be identified and reanalyzed Until the qualified sample can be measured. 10.2 Calibration validity check The calibration curve shall be plotted for each batch of samples, and the correlation coefficient of the calibration curve is greater than or equal to 0.999. Each test of 10 samples need to use a calibration curve of the intermediate concentration of the solution for calibration verification, the relative determination of the results Poor ≤ 5%, otherwise you need to redraw the calibration curve. 10.3 Precision control Each batch of samples should be measured at least 10% of the parallel sample, the number of samples less than 10, at least a parallel sample. When coal When the sulfur content is less than 0.45%, the relative deviation of the test result should be ≤10%. When the sulfur content in the coal is ≥0.45%, the phase of the test results The deviation should be ≤ 5%. 10.4 Accuracy control Each batch of samples need to use the national standard coal samples for calibration, the measured value should be within the guaranteed value range, at least 10 per sample Product calibration once.