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HJ 750-2015 English PDF

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HJ 750-2015: Solid Waste. Determination of total chromium. Furnace atomic absorption spectrometry
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HJ 750-2015English349 Add to Cart 3 days [Need to translate] Solid Waste. Determination of total chromium. Furnace atomic absorption spectrometry Valid HJ 750-2015

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Basic data

Standard ID HJ 750-2015 (HJ750-2015)
Description (Translated English) Solid Waste. Determination of total chromium. Furnace atomic absorption spectrometry
Sector / Industry Environmental Protection Industry Standard
Word Count Estimation 14,183
Date of Issue 2015-08-21
Date of Implementation 2015-10-01
Quoted Standard GB 5086.1; HJ/T 20; HJ/T 298; HJ/T 299; HJ/T 300; HJ 557
Regulation (derived from) Ministry of Environment Announcement 2015 No.54
Issuing agency(ies) Ministry of Ecology and Environment
Summary This standard specifies the determination by graphite furnace atomic solid waste and solid waste leaching solution total chromium absorption spectrophotometry. This standard applies to the determination of solid waste and solid waste leaching solution total chromium. The determination of solid waste, the amount of sample is 0.2g, set the volume to 50ml volume and injection volume of 20��l, this standard detection limit of 0.2mg/kg, detection limit of 0.8mg/kg. The determination of solid waste leachate, volume and volume of 50ml injection volume was 20��l, this standard detection limit of 0.7��g/L, detection limit was 2.8��g/L.

HJ 750-2015: Solid Waste. Determination of total chromium. Furnace atomic absorption spectrometry


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Solid Waste.Determination of total chromium.Furnace atomic absorption spectrometry National Environmental Protection Standard of the People 's Republic of China Determination of total chromium in solid waste Graphite Furnace Atomic Absorption Spectrophotometry Solid Waste-Determination of total chromium - Furnace atomic absorption spectrometry 2015-08-21 release 2015-10-01 implementation Ministry of Environmental Protection I directory Preface .ii

1 Scope of application

2 normative reference documents

3 Principle of the method

4 interference and elimination

5 reagents and materials 1 6 instruments and equipment 2 7 Sample 2

8 Analysis steps

The results are calculated and expressed 10 precision and accuracy 11 Quality assurance and quality control 12 Precautions 13 Waste treatment Appendix A (normative appendix) Standard addition method Appendix B (informative appendix) Applicability judgment of standard addition method 9 Appendix C (informative) Use of matrix modifiers.10

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 Environmental Pollution by Solid Wastes, Protect the environment, protect human health, regulate the determination of total chromium in solid waste, the development of this standard. This standard specifies the total chromium in solid waste by graphite furnace atomic absorption spectrophotometry. This standard is the first release. Appendix A to this standard is a normative appendix, Appendix B and Appendix C are informative appendices. This standard is organized by the Ministry of Environmental Protection Science and Technology Standards Division. The main drafting unit of this standard. Harbin Environmental Monitoring Center Station. The standard verification unit. Heilongjiang Province Environmental Monitoring Center Station, Dalian Environmental Monitoring Center, Changchun Environmental Monitoring Heart station, Qiqihar City Environmental Monitoring Center Station, Daqing City Environmental Monitoring Center Station and Anshan City Environmental Monitoring Center Station. The Environmental Protection Department of this standard approves on August 21,.2015. This standard is implemented on October 1,.2015. This standard is explained by the Ministry of Environmental Protection. Determination of total chromium - Solid waste - Graphite furnace atomic absorption spectrophotometric method WARNING. Disassembly shall be carried out in a fume hood and shall be protected against contact with skin and clothing as required.

1 Scope of application

This standard specifies the determination of total chromium in solid waste and solid waste leachate by graphite furnace atomic absorption spectrophotometry. This standard is applicable to the determination of total chromium in solid waste and solid waste leachate. Determination of solid waste, the sample volume of 0.2 g, constant volume of 50 ml and the injection volume of 20μl, the method detection limit 0.2 mg/kg, the determination of the lower limit of 0.8 mg/kg. Determination of solid waste leachate, volume volume of 50 ml and the amount of injection 20μl, the detection limit of this method is 0.7 μg/L, the determination of the lower limit of 2.8 μg/L.

2 normative reference documents

The contents of this standard refer to the following documents or their terms. Any annotated file that does not specify the date, its valid version Applicable to this standard. Solid waste leaching toxicity leaching method Technical specification for SJ sample preparation for industrial solid waste Technical Specification for Hazardous Waste Identification HJ/T 299 Solid waste leaching toxicity leaching method sulfuric acid nitric acid method HJ/T 300 solid waste leaching toxicity leaching method acetic acid buffer solution method HJ 557 Solid waste leaching toxicity leaching method Horizontal oscillation method

3 Principle of the method

The solid waste of the whole digestion or leaching solution into the graphite furnace atomizer, the chromium ions in the graphite tube through Atomization of the ground chromium atoms on the chromium hollow cathode lamp emission of 357.9 nm or 359.3nm characteristic line selective absorption, Its absorbance in a certain range with the mass concentration of chromium is proportional to.

4 interference and elimination

4.1 Low concentrations of calcium or phosphate may cause interference to the assay, and when the concentration of calcium or the concentration of phosphate is greater than.200 Mg/L, the effect of calcium remains constant and the effect of the phosphate is eliminated. Add calcium nitrate solution concentration greater than.2000 mg/L When the interference will be stable. Refer to Appendix C for the addition of the modifier. 4.2 The use of pyrolytic graphite tubes and coated graphite tubes can eliminate the effects of carbides.

5 reagents and materials

5.1 Experimental water. secondary distilled water or pure water equipment prepared by the water. Before use to be blank test, to confirm no target Or target concentration below the method detection limit. 5.2 Potassium Dichromate (K2Cr2O7). Reference reagent. 5.3 Calcium nitrate [Ca (NO3) 2 · 4H2O], excellent grade pure. 5.4 nitric acid (HNO3). ρ = 1.42 g/ml, excellent grade pure. 5.5 hydrochloric acid (HCl). ρ = 1.19 g/ml, excellent grade pure. 5.6 Hydrogen peroxide (H2O2). ρ = 1.11 g/ml, excellent grade pure. 25.7 hydrofluoric acid (HF). ρ = 1.18 g/ml, excellent grade pure. 5.8 Calcium nitrate solution. ρ (Ca) =.2000 mg/L 11.8 g of calcium nitrate [Ca (NO3) 2 · 4H2O] was weighed and dissolved in a nitric acid solution (5.9) and diluted to 1000 ml. 5.9 Nitric acid solution. 1 99 (V/V), prepared with nitric acid (5.4). 5.10 nitric acid solution. 1 1 (V/V), prepared with nitric acid (5.4). 5.11 hydrochloric acid solution. 1 2 (V/V), prepared with hydrochloric acid (5.5). 5.12 chromium standard stock solution. ρ (Cr) = 1000 mg/L Purchase a commercially available standard material/certified standard sample, or accurately weigh 0.2829 g of reference potassium dichromate (5.2) A small amount of water dissolved, transferred to 100 ml volumetric flask, the experimental water volume after shake, keep at room temperature for 6 months. 5.13 chromium standard intermediate solution. ρ (Cr) = 10 mg/L Accurate amount of chromium standard stock solution (5.12) 1.0 ml in 100 ml volumetric flask, the experimental water volume shake. 5.14 chromium standard use of liquid. ρ (Cr) = 0.5 mg/L Accurate amount of chromium standard intermediate solution (5.13) 5.0 ml in 100 ml volumetric flask, the experimental water volume shake. 5.15 argon. purity ≥99.99%.

6 instruments and equipment

6.1 Graphite Furnace Atomic Absorption Spectrophotometer with Chrome Hollow Cathode Lamp. 6.2 graphite tube, coated graphite tube. 6.3 Filtration device. 0.45 μm pore size acetate or polyethylene filter. 6.4 Electric plate. with temperature control function. 6.5 microwave digestion instrument. a temperature control and program temperature function, the temperature accuracy of up to ± 2 ℃. 6.6 balance. accuracy of 0.0001 g. 6.7 Balance. Accuracy 0.01 g. 6.8 Teflon crucible. 6.9 nylon screen. 100 mesh. 6.10 General laboratory equipment and equipment commonly used.

7 samples

7.1 Collection and storage of samples The collection and storage of solid waste samples are carried out in accordance with the relevant provisions of HJ/T 20 and HJ/T 298. 7.2 Preparation of the sample 7.2.1 Solid waste samples The preparation of solid waste samples was carried out in accordance with the relevant provisions of HJ/T 20. For solid waste or viscous sludge (M1, accurate to 0.01 g), naturally air-dried or freeze-dried, weighing again (m2, exact To 0.01 g), grinding, all over 100 mesh sieve. 7.2.2 Solid waste leachate samples A sample of solid waste leachate was prepared according to the method of HJ/T 299, HJ/T 300, HJ 557 and GB 5086.1. 7.3 Preparation of samples 7.3.1 Solid waste samples 37.3.1.1 Electric plate digestion method Weigh 0.2 g (m3, accurate to 0.0001 g) solid waste sample (7.2.1) in 50 ml polytetrafluoroethylene crucible, After wetting with water, add 10 ml of concentrated hydrochloric acid (5.5) and heat it at 50 ° C on a hot plate in a fume hood to initialize the sample. To be evaporated to about 3 ml or so, then add 5 ml of concentrated nitric acid (5.4), 5 ml of hydrofluoric acid (5.7), after capping Hot plate about 120 ~ 130 ℃ heating 0.5 ~ 1 h or so, open the lid by adding 2 ml of hydrogen peroxide (5.6), and then cover 150 ~ 160 ℃ heating 1 h or so, and then open the lid, drive white smoke and steamed into the contents of the liquid is not the state of the liquid beads (hot ). Visual digestion, and then add 3 ml concentrated nitric acid (5.4), 3 ml hydrofluoric acid (5.7), 1 ml hydrogen peroxide (5.6), The digestion process can be repeated until the solution is clear or the solution remains unchanged. Remove the crucible slightly cold, add 1 ml of nitric acid solution (5.10), dissolve the soluble residue in warm, all the test solution to 50 ml volumetric flask, the experimental water volume (V0), To be tested. Note 1. 30% of the total amount of hydrogen peroxide added shall not exceed 10 ml. 7.3.1.2 Microwave digestion method Weigh 0.2 g (m3, accurate to 0.0001 g) solid waste sample (7.2.1) in a microwave digestion tank with a small amount of water After wetting, add 3 ml of concentrated nitric acid (5.4), 1 ml of concentrated hydrochloric acid (5.5), refer to Table 1 for digestion, such as digestion has been clarified, You do not have to add hydrofluoric acid and hydrogen peroxide, acid directly after the constant volume. After cooling, the contents were all transferred to 50 ml of polytetrafluoroethylene crucible, capped, placed on the hot plate, micro boiling state Drive white smoke to white smoke is no longer produced, remove the slightly cold, add 2 ml of experimental water, 3 ml of hydrofluoric acid (5.7) and 2 ml Hydrogen peroxide (5.6), continue to heat, add 1 ml of hydrogen peroxide (5.6), to the reaction is stable, continuous heating to the inside The contents are viscous. Remove the slightly cold, add 3 ml hydrochloric acid solution (5.11), dissolve the soluble residue in warm, the whole volume moved to 50 ml volumetric flask, the experimental water volume (Vo), to be tested. Note 2. microwave digestion, such as digestion has been clarified, then do not have to add hydrofluoric acid and hydrogen peroxide, acid up after the constant volume. Table 1 microwave digestion instrument reference conditions Program temperature rise time (min) Decomposition temperature holding time (min) The first step 10 room temperature ~ 170 ℃ 5 The second step 10 170 ℃ ~ 175 ℃ 5 7.3.2 Solid waste leachate sample 7.3.2.1 Electric plate digestion method Measure the amount of 50.00 ml (V) leachate (7.2.2) in a 150 ml Erlenmeyer flask, add 2 ml of concentrated nitric acid (5.4) Shake well In the triangle bottle into the small funnel placed on the hot plate after heating, boil to the test solution volume of about 20 ml when removed, cold but. If the test solution is viscous, should add 2ml concentrated nitric acid (5.4), continue to heat, repeat the above operation, to test solution to clarify Or the color remains the same. Rinse the small funnel and the inner wall of the flask with a small amount of test water and move all the test solution to 50 ml Capacity of the bottle, the experimental water volume (V0), to be measured. Such as particles in the digestion solution, filtered and then determined. 7.3.2.2 Microwave digestion method Measure the amount of 5.00 ~ 10.00 ml leachate (7.2.2) in a microwave digestion tank, add 1 ml of concentrated nitric acid (5.4) According to Table 1 for digestion, cooling solution will be moved to 50 ml volumetric flask, with a small amount of experimental water rinse microwave digestion tank, The test solution all moved to 50 ml volumetric flask, the experimental water volume (V0), to be measured. 4 Note 3. Microwave digestion is not suitable for digestion of higher organic content of the sample, such as leaching solution contains high organic matter, it is recommended to use Hot plate method. 7.4 Preparation of blank sample 7.4.1 Solid waste blank sample A solid waste blank sample was prepared according to 7.3.1. 7.4.2 Solid waste leachate blank sample The solid waste leachate blank sample was prepared according to the procedure of 7.3.2.

8 Analysis steps

8.1 Instrument reference conditions Different models of atomic absorption spectrophotometer the best working conditions are different, should be in accordance with the instructions to operate the instrument, The recommended conditions for this instrument are as follows. Table 2 Instrument reference conditions Element Cr Measurement wavelength (nm) 357.9 (359.3) Passband width (nm) 0.7 Drying temperature (℃)/time (s) 100-130/30 Ashing temperature (℃)/time (s) 1200/30 Atomization temperature (℃)/time (s) 2600/3 Elimination temperature (° C) Time (s) 2700/30 Whether the atomic phase is stopped Argon flow rate (ml/min) 300 Injection volume (μl) 20 8.2 Calibration Respectively, the amount of 0,0.50,1.00,1.50,2.00,2.50 ml of chromium standard use of liquid (5.14) in the 50 ml volumetric flask , With nitric acid solution (5.9) constant volume to the mark, mix. The standard series concentrations are. 0,5.0,10.0,15.0, 20.0, 25.0 μg/L. The absorbance of the standard series was determined in turn from low to high concentrations according to the instrument reference conditions (8.1). To zero concentration Correct the absorbance as the ordinate, the chromium content (μg/L) as the abscissa, draw the calibration curve. 8.3 Sample determination The prepared sample was measured with the same instrumental analysis conditions as the calibration curve. When the sample concentration exceeds the calibration curve The maximum concentration of the line can increase the dilution factor or use flame atomic absorption spectrophotometer. 8.4 blank test The prepared blank sample 7.4 was measured according to the instrument reference conditions (8.1). Results and representations 9.1 Calculation of solid waste test results 9.1.1 Solid and viscous sludge solid waste The total chromium content in solid waste  (mg/kg) is calculated according to equation (1). ) () V  (1) Where.  - total chromium content in solid waste, mg/kg;  - the concentration of total chromium in the sample taken from the calibration curve, μg/L; 0 - the concentration of total chromium in the blank sample from the calibration curve, μg/L; V0 - volume after digestion, ml; M1 - the quality of solid samples, g; M2 - the quality of the solid sample after drying, g; M3 - the quality of the sample after grinding, g; 9.1.2 Liquid and semi-solid (except viscous sludge) Solid waste The total chromium content in solid waste  (mg/kg) is calculated according to formula (2). 00) ( V ω 310 -  (2) Where.  - total chromium content in solid waste, mg/kg;  - the concentration of total chromium in the sample taken from the calibration curve, μg/L; 0 - the concentration of total chromium in the blank sample from the calibration curve, μg/L; V0 - volume after digestion, ml; M3 - the quality of the sample, g; 9.2 Calculation of solid waste leachate test results The concentration of total chromium in the solid waste leachate is calculated (in mg/L) according to equation (3). 301 1050) (  (3) Where.  - concentration of total chromium in solid waste leachate, μg/L; 1 ü - the concentration of total chromium in the sample taken from the calibration curve, μg/L; 0 - the concentration of total chromium in the blank sample from the calibration curve, μg/L; V - the volume of leach solution when digested, ml; 9.3 The result is shown When the solid waste sample determination results less than 10 mg/kg, after the decimal point to retain 1; when the determination is greater than or equal to 10 mg/kg, retain 3 valid digits. When the solid waste leachate sample determination results less than 10 μg/L, the retention of the decimal point after 1; when the determination of large At 10 μg/L, 3 valid digits are reserved. 610 precision and accuracy 10.1 Precision For solid waste, six laboratories were treated with sewage at concentrations of 129.6 mg/kg and 118.7 mg/kg, respectively Treatment plant of domestic sludge and industrial sludge samples were measured, the relative standard deviation in the laboratory were 5.3 ~ 13.0% and 5.9 ~ 12.8%, the relative standard deviation between the laboratory were 12.4% and 5.8%, repeatability r were 76.0 mg/kg And 74.0 mg/kg, reproducibility R were 372 mg/kg and 342 mg/kg, respectively. For solid waste leachate, the total mass concentration of total chromium in the six laboratories was 2.5 μg/L, 12.0 μg/L and 22.0 Μg/L leaching solution samples were measured, the relative standard deviation of the laboratory were 0.4 ~ 5.7%, 0.6 ~ 11%, 0.20 ~ 6.5%; the relative standard deviations were 4.3%, 4.2% and 3.8%, respectively. The repeatability r was 0.3 μg/L, 2.0 μg/L And 2.4 μg/L, the reproducibility limit was 0.4 μg/L, 2.3 μg/L and 3.2 μg/L. 10.2 Accuracy For solid waste, six validation laboratories measured the zinc slag standard material with a relative error of 1.1 to 4.7% The final value is 2.8% ± 3.0%. For solid waste leachate, six laboratories added leachate samples from 7 to 19 μg/L leaching solution Standard determination, the standard concentration from 5 ~ 10 μg/L. The recoveries were. 92.2 ~ 114%, 93.4 ~ 119%, respectively The final yield was (103% ± 17.0%), (105% ± 19.7%). 11 quality assurance and quality control 11.1 Each sample analysis should draw a calibration curve with a correlation coefficient greater than or equal to 0.995. 11.2 Each 10 samples should be analyzed for a calibration curve for the intermediate point concentration of the standard solution, and its assay results with the calibration curve for the The relative deviation of the point concentration should be less than or equal to 10%. Otherwise, the calibration curve needs to be redrawn. 11.3 each batch of samples should be at least two blank test, the determination of the results should be lower than the lower limit of the method. 11.4 each batch of samples should be at least 10% of the parallel sample determination (less than 10 samples at least once), two parallel The relative deviation of the sample analysis results should be less than 20%. 11.5 each batch of samples should be at least 10% spike recovery sample test (the number of samples less than 10 at least once), plus standard The yield should be between 85.1 and 119%. 12 Precautions 12.1 graphite furnace has a high sensitivity, in the course of the experiment should avoid cross-contamination and sample contamination. Used in experiments Glass containers with 10% nitric acid solution soak for 24 h, and then tap water and experimental water followed by rinsing clean, The environment to dry. The entire cleaning process shall not use potassium dichromate lotion. 12.2 The solution shall not be evaporated during the digestion process and the boiling process shall prevent the sample from splashing. If steamed or splashed, should be heavy New sampling for digestion. 12.3 graphite tube in the use of high temperature before burning several times to clean the graphite tube. 12.4 When the sample matrix composition is complex or unknown, or spike recovery rate exceeds the scope of the requirements of this method should be adopted The standard addition method is used for the determination of the sample and the results are calculated. See Appendix A, the applicability of the standard addition method is given in Appendix B. 13 Waste treatment All samples of the waste produced in the experimental sample and in the course of the experiment shall be collected and stored in a centralized manner and sent to a qualified unit 7 processing.

8 Appendix A

(Normative appendix) Standard addition method A.1 Calibration of calibration curves Respectively, the amount of the same amount of test solution to be tested four copies of the preparation of the total volume of 50ml of the four solutions, the first Without standard solution, the first 2,3,4 copies were added in different proportions of different concentrations of standard solution, the solution concentration were. CX, CX C0, CX 2C0, CX 3C0; the concentration of C0 added to the standard solution should be approximately equal to 0.5 times the sample concentration that C0 ≈ 0.5CX, with nitric acid solution (5.9) volume. The blank solution was zeroed and the absorbance was measured in the same measurement conditions, With the standard solution concentration as the abscissa, the corresponding absorbance as the ordinate to draw the calibration curve, the curve of the reverse extension and concentration The intersection of the axis is the concentration of the element to be measured in the sample solution. This method is only applicable to areas where the concentration and absorbance are linear. (The error caused by the addition of the standard volume does not exceed 0.5%). The relationship between the measured element concentration and the corresponding absorbance, see attached Figure A.1. Figure A.1 Relationship between the concentration of the element to be measured and the corresponding absorbance A.2 Precautions The use of standard addition method can only eliminate the influence of matrix effect, can not eliminate the impact of background absorption. Concentration (mg/L) 3C02C0C00Cx

9 Appendix B

(Informative) Appraisal of Applicability of Standard Addition Determination of the actual sample absorbance of A, from the calibration curve on the detection of the concentration of x. And then add the standard to the actual sample The amount of s, and then tested, the absorbance of B, from the calibration curve on the detection of the concentration of y. Calculate in accordance with formula (B.1) The content of the sample c. Xy Sc ) ((B.1) When there is a matrix effect, Xy  between 0.5 and 1.5, the standard addition method can be used, when xy  beyond this range The standard addition method does not apply.

Appendix C

(Informative) Use of matrix modifier When the sample spiked recovery rate exceeds the required range, or know that the sample has basic interference, can be in the chromium standard solution Series at the same time by adding the same amount of calcium nitrate solution to eliminate matrix interference. Adding the matrix modifier chromium standard solution series preparation method. take the amount of 0,0.50,1.00,1.50,2.00, 2.50 ml of chromium standard use of liquid (5.14) in 50 ml volumetric flask, were added 5.00 ml of calcium nitrate solution (5.8), with Nitric acid solution (5.9) constant volume to the mark, mix. Sample of the addition of the basic modifier Preparation method. Solid waste sample. After completion of digestion as described in the text, Liquid all moved to 50 ml volumetric flask, add 5.00 ml of calcium nitrate solution (5.8), with the experimental water volume, to be measured; solid Body waste leachate sample. according to the text described after the completion of digestion, all the test solution all moved to 50 ml volumetric flask, with nitro Acid solution (5.9) constant volume, to be measured. Follow the calibration procedure (8) to calibrate the curve and sample.

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