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HJ 766-2015 English PDF

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HJ 766-2015: Solid Waste. Determination of metals. Inductively coupled plasma mass spectrometry (ICP-MS)
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HJ 766-2015English329 Add to Cart 3 days [Need to translate] Solid Waste. Determination of metals. Inductively coupled plasma mass spectrometry (ICP-MS) Valid HJ 766-2015

Standard similar to HJ 766-2015

HJ 511   HJ 945.3   HJ 943   

Basic data

Standard ID HJ 766-2015 (HJ766-2015)
Description (Translated English) Solid Waste. Determination of metals. Inductively coupled plasma mass spectrometry (ICP-MS)
Sector / Industry Environmental Protection Industry Standard
Word Count Estimation 14,158
Date of Issue 2015-11-20
Date of Implementation 2015-12-15
Quoted Standard HJ/T 20; HJ/T 298; HJ/T 299; HJ/T 300; HJ 557
Regulation (derived from) Ministry of Environment Announcement 2015 No.73
Issuing agency(ies) Ministry of Ecology and Environment
Summary This Standard specifies the determination by inductively coupled plasma mass spectrometry and solid waste leachate of solid wastes in metallic elements. This Standard applies to solid waste and solid waste leaching solution of silver (Ag), arsenic (As), barium (Ba), beryllium (Be), cadmium (Cd), cobalt (Co), chromium (Cr), copper (Cu), Determination of manganese (Mn), molybdenum (Mo), Nickel (Ni), lead (Pb), antimony (Sb), selenium (Se), thallium (Tl), vanadium (V), zinc (Zn) 17 metal elements. If verified, this standard is also applicable to the determination of other metallic elements.

HJ 766-2015: Solid Waste. Determination of metals. Inductively coupled plasma mass spectrometry (ICP-MS)


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Solid Waste.Determination of metals.Inductively coupled plasma mass spectrometry (ICP-MS) National Environmental Protection Standard of the People 's Republic of China Determination of metallic elements in solid wastes Inductively coupled plasma mass spectrometry Solid Waste-Determination of metals-Inductively coupled plasma mass Spectrometry (ICP-MS) 2015-11-20 release 2015-12-15 implementation Ministry of Environmental Protection Directory Preface .ii

1 Scope of application

2 normative reference documents

3 Principle of the method

4 interference and elimination

5 reagents and materials

6 instruments and equipment

7 Sample 3

8 Analysis steps

The results are calculated and expressed 10 precision and accuracy Quality assurance and quality control 12 Waste treatment 13 Precautions Appendix A (Normative Appendix) Method Detection limit and lower limit of measurement 8 Appendix B (informative) Common multipath ion interference and interference correction commonly used mathematical equations. Appendix C (informative) method of precision and accuracy

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 solid metal waste metal monitoring methods, the development of this standard. This standard specifies the inductively coupled plasma mass spectrometry for the determination of metal elements in solid waste and solid waste leachate. This standard is the first release. Appendix A to this standard is a normative appendix, Appendix B, Appendix C is an informative appendix. This standard is organized by the Ministry of Environmental Protection Science and Technology Standards Division. The main drafting unit of this standard. Qingdao Environmental Monitoring Center Station The standard verification unit. Heilongjiang Province Environmental Monitoring Center Station, Jinan City Environmental Monitoring Center Station, Harbin Environmental Monitoring Measuring center station, Yantai City Environmental Monitoring Center Station, Zaozhuang City Environmental Monitoring Station, Qingdao Economic and Technological Development Zone Water Supply and Drainage Monitoring 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. Solid waste - Determination of metallic elements - Inductively coupled plasma mass spectrometry Warning. Preparation of thallium, beryllium and other highly toxic substances in the standard solution, should avoid direct contact with the skin. Nitric acid used in the experiment, Hydrochloric acid, hydrofluoric acid is volatile and corrosive, the operation should be required to wear protective equipment, the entire experimental process must Operate in a fume hood.

1 Scope of application

This standard specifies the inductively coupled plasma mass spectrometry for the determination of metal elements in solid waste and solid waste leachate. This standard applies to the solid waste and solid waste leaching solution of silver (Ag), arsenic (As), barium (Ba), beryllium (Be), cadmium (Cd), cobalt (Co), chromium (Cr), copper (Cu), manganese (Mn), molybdenum (Mo), nickel (Ni), lead (Pb) Determination of 17 kinds of metal elements such as selenium (Se), thallium (Tl), vanadium (V) and zinc (Zn). This standard is also applicable if verified Determination of other metal elements. When the sampling volume of solid waste leaching solution is 25 ml, the detection limit of 17 kinds of metal elements is 0.7 μg/L to 6.4 μg/L, The lower limit of determination was 2.8 μg/L ~ 25.6 μg/L. The limit of detection for each element is given in Appendix A. When the amount of solid waste sample is 0.1 g , The detection limit of 17 kinds of metal elements was 0.4 mg/kg ~ 3.2 mg/kg, and the determination limit was 1.6 mg/kg ~ 12.8 mg/kg.

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. 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

Solid waste or solid waste leaching solution by microwave digestion pretreatment, the use of inductively coupled plasma mass spectrometer for inspection Measured, according to the elements of the spectrum or characteristic ions for qualitative, internal standard method quantitative.

4 interference and elimination

4.1 Mass spectrum interference Mass spectrometry interference mainly includes isotope interference, polyatomic ion interference, oxide and double charge interference. The same amount Isotope interference can be corrected using the interference correction equation or by chemical separation of the sample before analysis except. Commonly used mass count interference correction equation is shown in Appendix B-1. Polyatomic ion interference is the most important source of interference for ICP-MS. It can use the interference correction equation, instrument optimization and Collision reaction pool technology to eliminate. Common polyatomic ion disturbances are given in Appendix B-2. Oxide interference and double charge interference can reduce the degree of interference by adjusting the instrument parameters. 4.2 non-mass spectral interference Non-mass spectral interference mainly includes matrix suppression interference, space charge effect interference, physical effect interference and so on. Non-mass spectrometry The degree of interference is related to the nature of the sample matrix and can be eliminated by means of internal standard method, instrument condition optimization or standard addition method.

5 reagents and materials

Unless otherwise stated, the use of the use of national standards in line with the excellent grade pure chemical reagents, experimental water for the new preparation Ion water. 5.1 hydrochloric acid. ρ (HCl) = 1.19 g/ml, excellent grade pure or high purity. 5.2 nitric acid. ρ (HNO3) = 1.42 g/ml, excellent grade pure or high purity. 5.3 hydrofluoric acid. ρ (HF) = 1.49 g/ml. 5.4 Hydrogen peroxide. ω (H2O2) = 30%. 5.5 Nitric acid solution. 2 98. 5.6 nitric acid solution. 5 95. 5.7 single element standard stock solution. ρ = 1.00 mg/ml. Can be prepared with high purity metal (purity greater than 99.99%) or metal salts (reference or high purity reagent) formulated 1.00 mg/ml A standard stock solution containing nitric acid solution (5.5), or a commercially available standard solution. 5.8 multi-element standard stock solution. ρ = 100 mg/L. Use a nitric acid solution (5.5) to dilute the single element standard stock solution (5.7), or purchase a multi-element mixed standard solution directly. 5.9 Multi-element standard solution. ρ = 1.00 mg/L. The standard stock solution (5.7 or 5.8) was diluted with nitric acid solution (5.5). 5.10 Internal standard standard stock solution. ρ = 10.0 mg/L. Should choose 6Li, 45Sc, 74Ge, 89Y, 103Rh, 115In, 185Re, 209Bi for the internal standard elements. Can be purchased directly to prove The standard solution was prepared and the medium was nitric acid solution (5.5). 5.11 mass spectrometer tuning solution. ρ = 10.0 μg/L. A solution containing Li, Y, Be, Mg, Co, In, Tl, Pb and Bi elements should be used as the tuning solution for the mass spectrometer. Can be purchased directly to prove the standard solution preparation. Note 1. All elements of the standard solution should be prepared in sealed polyethylene or polypropylene bottles. 5.12 argon. purity of not less than 99.99%.

6 instruments and equipment

6.1 Inductively Coupled Plasma Mass Spectrometer (ICP-MS). The mass range that can be scanned is 6 amu to 240 amu at 10% Peak height should be between 0.6 amu ~ 0.8 amu. 6.2 microwave digestion device. with programmable power setting function, microwave digestion power of 1200 W or more, with PTFE Ethylene or equivalent material microwave digestion tank. 6.3 balance. the amount of 0.1 mg. 6.4 nylon screen. 0.15 mm (100 mesh). 6.5 Membrane. water microporous membrane, pore size 0.45μ m. 6.6 acid circuit. temperature ≥ 150 ℃. 6.7 Common laboratory equipment and equipment.

7 samples

7.1 Acquisition and storage The collection and storage of solid wastes are carried out in accordance with the relevant provisions of HJ/T 20 and HJ/T 298. 7.2 Sample preparation 7.2.1 Solid waste leachate The preparation of the leachate was carried out according to the relevant provisions of HJ/T 299, HJ/T 300 and HJ 557. 7.2.2 Solid waste The preparation of solid waste samples was carried out in accordance with the relevant provisions of HJ/T 20. For solid waste or dry semi-solid solids Waste sample, accurately weighed 10 g sample (m1, accurate to 0.01 g), natural air-dried or freeze-dried, weighing again (m2, Accurate to 0.01 g), grinding, all over 0.15 mm (100 mesh) nylon sieve (6.4) spare. 7.3 Preparation of samples 7.3.1 Solid waste leachate sample Remove the solid waste leachate 25.0 ml, placed in the digestion tank, add 4 ml of nitric acid (5.2) and 1 ml of hydrochloric acid (5.1), Place the digestion tank in the microwave digestion device (6.2) for digestion. The recommended sample digestion procedure is given in Appendix B-3. Digest after cooling To the room temperature, carefully open the lid of the digestion tank, and then put the digestion tank on the acid analyzer (6.6), at 150 ℃ exposure to acid The internal solution was dried and cooled to room temperature. The inside solution was dissolved with deionized water and the solution was transferred to a 50 ml volumetric flask. Deionized water to 50 ml. The filter (6.5) was filtered before filtration or the supernatant was used for the determination. 7.3.2 Solid waste samples For solid samples or dry semi-solid samples, we sample 0.1 g to 0.2 g (m3) of sieved samples (7.2.2); In liquid or non-dry solid samples, directly weighed the sample 0.2 g (m3), accurate to 0.0001 g. Place the sample in digestion (5.1), 4 ml of nitric acid (5.2), 1 ml of hydrofluoric acid (5.3) and 1 ml of hydrogen peroxide (5.4) were added to the mixture The digestion tank is placed in a microwave digestion device (6.2) for digestion. The recommended sample digestion procedure is given in Appendix B-3. After digestion to cool to At room temperature, carefully open the lid of the digestion tank and place the digestion tank in the acid reflux (6.6), at 150 ° C. The internal solution was dried and cooled to room temperature. The inside solution was dissolved with deionized water and the solution was transferred to a 50 ml volumetric flask. Deionized water to 50 ml. The filter (6.5) was filtered before filtration or the supernatant was used for the determination. Note 2. For special matrix samples, if the digestion of the digestion solution is not complete, may be appropriate to increase the amount of acid. Note 3. If other quality control and quality assurance requirements can be met by verification, other digestion methods such as hot plates can also be used. 7.4 blank sample Instead of the sample with deionized water, the same procedure and reagent preparation were used to prepare a blank sample.

8 Analysis steps

8.1 Instrument operation reference conditions Different models of the best working conditions of different instruments, the standard mode and the reaction pool mode should be in accordance with the instrument operating instructions operating. 8.2 Instrument tuning After igniting the plasma, the instrument is warmed up for 30 minutes. Use the mass spectrometer to tune the solution (5.11) to the instrument's sensitivity, Oxide and double charge to adjust, in the instrument's sensitivity, oxide, double charge to meet the requirements of the conditions, the mass spectrometer to The relative standard deviation of the intensity of the elemental signal contained in the tuning solution is less than or equal to 5%. In the range of mass values covering the elements to be measured Line quality correction and resolution check if the quality correction result differs from the true value by more than ± 0.1 amu or the tuning element signal Resolution in the 10% peak height corresponding to the peak width of more than 0.6 amu ~ 0.8 amu range, should be in accordance with the instructions of the instrument Try to correct the quality to the correct value. 8.3 Calibration curve is established Respectively, take a certain volume of multi-element standard use of liquid (5.9) and the standard standard reserve solution (5.10) in the volumetric flask, Diluted with nitric acid solution (5.5) to prepare metal concentrations of 0 μg/L, 10.0 μg/L, 20.0 μg/L, 50.0 Μg/L, 100 μg/L, 500 μg/L calibration series. The internal standard standard stock solution (5.10) can be added directly to the calibration series , Can also be added online via the peristaltic pump before the sample is atomized. The concentration of the selected internal standard should be much higher than the internal standard contained in the sample itself Element concentration, the commonly used internal standard concentration range of 50.0 μg/L ~ 1000 μg/L. Determination by ICP-MS to each element The concentration of the abscissa, the response value and the internal standard response value of the ratio of the vertical axis, the establishment of calibration curve. Calibration curve concentration The range can be adjusted according to the measurement needs. 8.4 Specimen determination Before each sample is measured, rinse the system with nitric acid solution (5.6) until the signal is minimized until the analytical signal is stabilized Can begin to be measured. The prepared samples were added to the same standard of internal standard as the calibration curve. Under the same instrumental analysis conditions To be measured. If the concentration of the element to be measured in the sample exceeds the calibration curve, it needs to be re-measured by dilution, Acid solution (5.5). 8.5 blank sample determination The blank sample was measured according to the same measurement conditions as the sample.

9 Results calculation and representation

9.1 The mass concentration xp of the metal element to be measured in the sample is calculated according to the formula (1). (1) Where. Xρ - concentration of metal element to be measured in the sample, μg/L; Ax - Quantum ion response value of metal element to be measured; Ais - the response value of the internal standard quantitative ion corresponding to the metal element to be measured; Isρ - concentration of internal standard elements, μg/L; K-dilution factor A - the intercept of the calibration curve; B - the slope of the calibration curve. 9.2 Calculation of solid waste determination results 9.2.1 Solid and dry semi-solid solid waste The content of metal elements to be measured in solid waste (mg/kg) is calculated according to formula (2). Is A a) A Is Xk - × = X (2) Where. Ω - content of metal elements to be measured in solid waste, mg/kg; Xρ - the concentration of the metal element to be measured in the test sample is calculated from the calibration curve, μg/L; 0ρ - the concentration of metal elements to be measured in the blank sample, μg/L; V - volume of the sample after digestion, ml; 1m - the amount of sample weighed, g; 2m - the mass of the dried sample, g; 3m - the quality of the sample after sieving, g. 9.2.2 Liquid and non-dry semi-solid solid waste The content of metal elements in solid waste (mg/kg) is calculated according to formula (3). (3) Where. Ω - the content of metal elements to be measured in solid waste, mg/kg; Xρ - Calculate the concentration of the metal element to be measured in the sample by the calibration curve, μg/L; 0ρ - the concentration of the metal element to be measured in the blank sample, μg/L; V - volume of the sample after digestion, ml; 3m - Weigh the quality of the sample, g. 9.3 Calculation of determination results of solid waste leachate The concentration ρ (μg/L) of the metal element to be measured in the solid waste leaching solution is calculated according to the formula (4). (4) Where. Ρ - content of metal element to be measured in solid waste leachate, μg/L; Xρ - Calculate the concentration of the metal element to be measured in the sample by the calibration curve, μg/L; 0ρ - the concentration of the metal element to be measured in the blank sample, μg/L; 1V - leachate sampling volume, ml; 2V - volume of the sample after digestion, ml. 9.4 The result is shown For solid waste, when the result is less than 10 mg/kg, one after the decimal point is retained; when the result is greater than or equal At 10 mg/kg, three valid digits are retained. () 10x V Ρ ρω - × = × () X V Ρ ρρ - × = () 10x V m Mm Ρ ρω - × = × × For solid waste leachate, when the determination is less than 10 μg/L, one after the decimal point is retained; when the result is greater than Or equal to 10 μg/L, retain three significant digits. 10 precision and accuracy 10.1 Precision Six laboratories were the actual solid waste samples were measured, the metal elements of the laboratory relative standard deviation 0.0% ~ 41%, the relative standard deviation between the laboratory is 3.5% ~ 44%, the repeatability r is 0.2 mg/kg ~ 66.1 mg/kg, The reproducibility limit was 0.4 mg/kg to 186 mg/kg. Six laboratories were the actual solid waste leachate samples were measured, the elements of the laboratory relative standard deviation And the relative standard deviation was 2.3% ~ 30%, the repeatability r was 0.7 μg/L ~ 117 μg/L, Reproducibility R was 2.3 μg/L ~ 121 μg/L. 10.2 Accuracy Six laboratories, respectively, solid waste, solid waste leaching solution of the actual sample spiked and certified standard substances were measured. The recoveries of the spiked samples in the solid samples were 75.0% ~ 125%, and the recoveries were (85.0 ± 19) % ~ (111 ± 24)%. The relative error of the reference material in the laboratory was -6.7% ~ 5.7%, and the relative error between the (-2.7 ± 2.5)% ~ (1.6 ± 7.0)%. The recovery rate of the solid waste leaching solution in the laboratory was 75.5% ~ 124%, and the recoveries were as follows. (84.2 ± 17)% ~ (111 ± 25)%. There is a relative error of -55% ~ 28% in laboratory, and the relative error between laboratories (-46 ± 20)% to (7.8 ± 30)%. Details of the precision and accuracy of each metal element are given in Appendix C. 11 quality assurance and quality control 11.1 At least two blank samples should be analyzed for each batch. Blank values should meet one of the following conditions to be considered acceptable (2) less than 10% of the standard limit; (3) lower than the minimum test of each batch 10% of the value. 11.2 The standard curve shall be established for each analysis, and the correlation coefficient of the curve shall be greater than 0.999. 11.3 Each time 10 samples were analyzed, the intermediate concentration of the calibration curve should be analyzed, and the measured result was opposite to the actual concentration Poor should be ≤ 10%, otherwise you should find the cause or re-establish the calibration curve. After each batch of samples is analyzed, the curve should be the most Low point of the analysis, the measured results and the actual concentration of the relative deviation of ≤ 30%. 11.4 In each analysis, the response value of the internal standard in the sample should be between 70% and 130% of the calibration curve response value, otherwise The instrument drift or interference generated, should be found after the reanalysis of the reasons. If it is matrix interference, need to be diluted after the test If the sample contains the internal standard elements, the need to replace the internal standard or increase the internal standard element concentration. 11.5 in each batch of samples, should be analyzed at least one reagent blank (2% nitric acid) spikes, the spiked recovery rate should be 80% ~ 120% between. It is also possible to use a certified standard sample instead of a spike, which shall be within the range of the standard requirements. 11.6 each batch of samples should be measured at least a matrix spike and a matrix repeat spikes, the determination of the spiked recovery rate should be 75% ~ 125% between the two spiked samples measured within the deviation of less than 20%. If not in the scope, should consider the existence of matrix interference, Suspension can be eliminated by diluting the sample or increasing the internal standard concentration. 12 Waste treatment The waste and waste generated during the experiment shall be kept in a closed container and stored in a qualified unit. Reason. 13 Precautions 13.1 Analysis of the containers used are (1 1) HNO3 solution soak for 24 h, washed with deionized water before use. 13.2 When adding acid solution to the digestion tank, observe the reaction in the tank. If there is a severe chemical reaction, And then sealed the tank. 13.3 For suspected solid waste, first scan the sample with semi-quantitative analysis to determine the concentration of metal element to be measured To avoid high concentrations of sample contamination of the instrument. 13.4 When using microwave digestion samples, pay attention to the use of temperature an...

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