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HJ 786-2016 English PDF

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HJ 786-2016: Solid waste. Determination of Lead, Zinc and Cadmium. Flame atomic absorption spectrometry
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Standard ID	Contents [version]	USD	STEP2	[PDF] delivered in	Standard Title (Description)	Status	PDF
HJ 786-2016	English	329	Add to Cart	3 days [Need to translate]	Solid waste. Determination of Lead, Zinc and Cadmium. Flame atomic absorption spectrometry	Valid	HJ 786-2016

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Basic data

Standard ID	HJ 786-2016 (HJ786-2016)
Description (Translated English)	Solid waste. Determination of Lead, Zinc and Cadmium. Flame atomic absorption spectrometry
Sector / Industry	Environmental Protection Industry Standard
Classification of Chinese Standard	Z13
Word Count Estimation	14,134
Date of Issue	2016-03-29
Date of Implementation	2016-05-01
Quoted Standard	HJ/T 20; HJ/T 298; HJ/T 299; HJ/T 300; HJ 557
Regulation (derived from)	Ministry of Environmental Protection Announcement No
Issuing agency(ies)	Ministry of Ecology and Environment

HJ 786-2016: Solid waste. Determination of Lead, Zinc and Cadmium. Flame atomic absorption spectrometry

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Solid waste.Determination of Lead, Zinc and Cadmium.Flame atomic absorption spectrometry National Environmental Protection Standard of the People 's Republic of China Determination of lead, zinc and cadmium in solid wastes Flame Atomic Absorption Spectrophotometry Solid waste-Determination of Lead, Zinc and Cadmium- Flame Atomic Absorption Spectrometry 2016-03-29 released 2016-05-01 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 samples .4

8 Analysis steps

9 Results calculation and representation

10 Precision and Accuracy 11 Quality assurance and quality control 12 Waste treatment 10 13 Precautions 10 Appendix A (informative) Standard Addition Act 12 Appendix B (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 determination of lead, zinc and cadmium in solid waste and solid waste leachate. This standard. This standard specifies the flame atomic absorption spectrophotometric method for the determination of lead, zinc and cadmium in solid waste and solid waste leachate. This standard is the first release. Appendix A and Appendix B of this standard are informative. This standard is organized by the Ministry of Environmental Protection Science and Technology Standards Division. The main drafting unit of this standard. Jiangsu Province Environmental Monitoring Center, Environmental Protection Department of Environmental Standards Institute. The standard verification unit. Nanjing Environmental Monitoring Center Station, Zhejiang Province Environmental Monitoring Center, Shanghai Environmental Monitoring Center, Changzhou City Environmental Monitoring Center Station, Ma On Shan City Environmental Monitoring Center Station, Lianyungang City Environmental Monitoring Center Station. The environmental protection department of this standard approved on March 29,.2016. This standard has been implemented since May 1,.2016. This standard is explained by the Ministry of Environmental Protection. Solid waste - Determination of lead, zinc and cadmium - Flame atomic absorption spectrophotometric method Warning. nitric acid used in the experiment, perchloric acid with strong oxidizing and corrosive, hydrochloric acid, hydrofluoric acid with strong volatile And corrosive, the operation should be required to wear protective equipment, solution preparation and sample pretreatment process should be in the fume hood into Line operation.

1 Scope of application

This standard specifies the flame atomic absorption spectrophotometric method for the determination of lead, zinc and cadmium in solid waste and solid waste leachate. This standard applies to the determination of lead, zinc and cadmium in solid waste and solid waste leachate. When the amount of solid waste is 0.5 g and the volume is 25 ml after digestion, the limits of lead, zinc and cadmium 2.0 mg/kg, 2.0 mg/kg and 0.3 mg/kg, respectively. The lower limit of determination was 8.0 mg/kg, 8.0 mg/kg and 1.2 mg/kg, respectively. when The amount of lead, zinc and cadmium is limited when the volume of solid waste leachate is 50 ml and the volume is 50 ml after digestion. 0.06 mg/L, 0.06 mg/L and 0.05 mg/L, respectively. The lower limit of determination was 0.24 mg/L, 0.24 mg/L and 0.20 mg/L, respectively.

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 leachate dissolved by acid, the sample of the test element in the flame atomizer was dissociated into The ground state atom, the ground state of the vapor on the element of the hollow cathode lamp or electrodeless discharge lamp emission characteristics of the radiation line selectivity absorb. In a certain concentration range, the absorption intensity and the sample to be measured in proportion to the mass concentration.

4 interference and elimination

4.1 When the calcium content is higher than 1000 mg/L, the inhibition of cadmium absorption; calcium content of.2000 mg/L, the signal inhibition of 19%. Iron content of more than 100 mg/L, inhibition of zinc absorption, adding lanthanum nitrate can eliminate the interference of coexisting components. When the sample is salt A high level of analysis of spectral wavelengths below 350 nm occurs when non-characteristic absorption, such as high concentrations of calcium is generated by background absorption of lead The results of the determination of high. 4.2 When the sample matrix composition is complex or unknown, or spike recovery rate exceeds the scope of the method of control requirements, should be used standard The addition method is used to determine the sample and calculate the results, see Appendix A.

5 reagents and materials

Unless otherwise stated, analytical analytical reagents conforming to national standards are used in the analysis, and the test water is a newly prepared deionized water. 5.1 sulfuric acid. ρ (H2SO4) = 1.84 g/ml, excellent grade pure. 5.2 nitric acid. ρ (HNO3) = 1.42 g/ml, excellent grade pure. 5.3 hydrochloric acid. ρ (HCl) = 1.19 g/ml, excellent grade pure. 5.4 hydrofluoric acid. ρ (HF) = 1.49 g/ml, excellent grade pure. 5.5 perchloric acid. ρ (HClO4) = 1.68 g/ml, excellent grade pure. 5.6 Hydrogen peroxide. φ (H2O2) = 30%, excellent grade pure. 5.7 Metal Lead. Spectrum Pure. 5.8 Metal Zinc. Spectrum Pure. 5.9 Cadmium. Spectrum pure. 5.10 lanthanum nitrate [La (NO3) 3 · 6H2O]. excellent grade pure. 5.11 nitric acid solution. 1 9 (v/v), prepared with nitric acid (5.2). 5.12 nitric acid solution. 1 99 (v/v), prepared with nitric acid (5.2). 5.13 hydrochloric acid solution. 1 1 (v/v), prepared with hydrochloric acid (5.3). 5.14 Substrate modifier. lanthanum nitrate solution,  [La (NO3) 3 · 6H2O] = 5%. Accurately weigh 5 g (accurate to 0.01 g) lanthanum nitrate (5.10), dissolve with nitric acid solution (5.12) and set to 100 ml Capacity bottle, spare. 5.15 lead standard stock solution. ρ = 1000 mg/L. Accurately weigh 1.000 g (accurate to 0.0001 g) of metal lead (5.7), add 15 ml of nitric acid (5.2) to dissolve, if necessary Can be dissolved by heating. The whole volume into the 1000 ml volumetric flask, the water volume to the mark, shake. Transfer to a polyethylene bottle at 4 ° C Under the cold storage, sealed can be saved for two years. A commercially available standard solution (lead element or lead-containing multi-element mixing standard may also be used Solution). 5.16 zinc standard stock solution. ρ = 1000 mg/L. Accurately weigh 1.000 g (exactly to 0.0001 g) of metal zinc (5.8), add 15 ml of nitric acid (5.2) to dissolve, if necessary Can be dissolved by heating. The whole volume into the 1000 ml volumetric flask, the water volume to the mark, shake. Transfer to a polyethylene bottle at 4 ° C Under the cold storage, sealed can be saved for two years. A commercially available standard solution (zinc single element or zinc-containing multi-element mixing standard can also be used Solution). 5.17 cadmium standard stock solution. ρ = 1000 mg/L. Accurately weigh 1.000 g (accurate to 0.0001 g) of metal cadmium (5.9), add 15 ml of nitric acid (5.2) to dissolve, if necessary Can be dissolved by heating. The whole volume into the 1000 ml volumetric flask, the water volume to the mark, shake. Transfer to a polyethylene bottle at 4 ° C Under the cold storage, sealed can be saved for two years. A commercially available standard solution (cadmium single element or cadmium-containing multi-element mixing standard) can also be used Solution). 5.18 lead standard use of liquid. ρ = 100 mg/L. Accurate removal of lead standard stock solution (5.15) 10.00 ml in 100 ml volumetric flask, with nitric acid solution (5.12) constant volume to standard Line, shake well. Pro is now available. 5.19 zinc standard use of liquid. ρ = 100 mg/L. Accurate removal of zinc standard stock solution (5.16) 10.00 ml in 100 ml volumetric flask, with nitric acid solution (5.12) constant volume to standard Line, shake well. Pro is now available. 5.20 cadmium standard use of liquid. ρ = 100 mg/L. Accurate removal of cadmium standard stock solution (5.17) 10.00 ml in 100 ml volumetric flask, with nitric acid solution (5.12) constant volume to standard Line, shake well. Pro is now available. 5.21 Acetylene. purity ≥99.5%. 5.22 Air. available from air compressor or compressed air cylinders.

6 instruments and equipment

6.1 flame atomic absorption spectrophotometer. 6.2 lead hollow cathode lamp, zinc hollow cathode lamp, cadmium hollow cathode lamp. 6.3 air compressor, should be equipped with water, degreasing and dust removal device. 6.4 hot plate or graphite digestion. a temperature control function (temperature stability ± 5 ℃), the maximum temperature can be set to.200 ℃. 6.5 microwave digestion. output power of 1000 W ~ 1600 W. With programmable control function, can be temperature, pressure and time (Heating time and holding time) to monitor the whole; with security features. 6.6 Analytical balance. 0.1 mg accuracy. 6.7 Polytetrafluoroethylene crucible. 50 ml. 6.8 Screen. non-metallic sieve, 100 mesh. 6.9 General laboratory equipment and equipment commonly used.

7 samples

7.1 Sample collection and storage 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 Sample preparation 7.2.1 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 waste Product, accurately weighed 10 g (m1, accurate to 0.01 g) sample, naturally air-dried or freeze-dried, weighing again (m2, accurate to 0.01 g), grinding, all over 100 mesh sieve (6.7) standby. 7.2.2 Solid waste leachate The preparation of solid waste leachate was carried out in accordance with the relevant provisions of HJ/T 299, HJ/T 300 or HJ 557. Leaching solution if not Can be timely analysis, should be added nitric acid (5.2) acidification to pH < 2, can be stored for 14 d. 7.3 Preparation of samples 7.3.1 Solid waste samples 7.3.1.1 Electric plate digestion method Weigh the sample (m3, exact to 0.1 mg) after sieving 0.25 g to 1.00 g in a 50 ml polytetrafluoroethylene crucible (6.6) in. After wetting the sample with a small amount of water, add 5 ml of hydrochloric acid (5.3) and add about 120 ° C to the hot plate (6.3) in the fume hood Heat, so that the initial digestion of the sample, to be evaporated to about 3 ml when removed slightly cold. Add 5 ml nitric acid (5.2), 5 ml hydrofluoric acid (5.4), 3 ml perchloric acid (5.5), capped and heated at about 160 ° C for 1 h on a hot plate. Open lid, heating plate temperature control at 170 ℃ ~ 180 ℃ continue to heat, and often shake the crucible. When heated to smoke thick smoke, capped to make black organic carbide fully decomposed. After the black organic matter on the wall of the crucible disappears, open the lid, drive the white smoke and steam to the contents of the sticky. Depending on the situation, can be The above digestion procedure was repeated by adding 3 ml of nitric acid (5.2), 3 ml of hydrofluoric acid (5.4) and 1 ml of perchloric acid (5.5). When white Smoke again exhausted and the contents were viscous, remove the crucible slightly cold, add 1 ml of nitric acid solution (5.12) warm dissolved soluble The residue is transferred to the 25 ml volumetric flask and the crucible lid and the inner wall are rinsed with the appropriate amount of water. The lotion is added to 25 ml Capacity bottles, with the experimental water volume to the mark, shake, to be measured. If the digestion solution contains undissolved particles, need to be filtered, Centrifugal separation or natural settlement. Note 1. Do not expose the sample to a large number of bubbles when heating, otherwise it will cause the loss of the sample. Note 2. If the content of lead, zinc or cadmium in solid waste is high, the volume of volume determined after digestion can be determined according to the actual situation. Note 3. If the graphite digestion instrument is used instead of the hot plate to digest the sample, refer to the above steps. 7.3.1.2 Microwave digestion method Weigh the sample (m3, accurate to 0.1 mg) after sieving 0.25 g to 1.00 g in a microwave digestion tank. Wet with a small amount of water After adding 5 ml of nitric acid (5.2), 5 ml of hydrochloric acid (5.3), 3 ml of hydrofluoric acid (5.4) and 1 ml of hydrogen peroxide (5.6) According to Table 1 of the temperature program to digest. After cooling, the contents of the microwave digestion tank were transferred to 50 ml of polytetrafluoroethylene Crucible, add 1 ml of perchloric acid (5.5), placed on the hot plate 170 ℃ ~ 180 ℃ to drive white smoke, to the contents of the sticky. Remove the crucible slightly cold, add 1 ml of nitric acid solution (5.12), dissolve the soluble residue in warm, after cooling the total transfer to 25 ml Capacity bottle, with the amount of experimental water rinse the crucible lid and the inner wall, lotion into the 25 ml volumetric flask, with the experimental water volume to the mark, Shake, test. If the digestion solution contains undissolved particles, need to be filtered, centrifugal or natural sedimentation. Table 1 Solid Waste Microwave Digestion Method Heating time (min) Digestion power (W) Digestion temperature (℃) Holding time (min) 12 400 room temperature ~ 160 3 5 500 160 ~ 180 3 5 500 180 ~.200 10 7.3.2 Solid waste leachate sample 7.3.2.1 Electric plate digestion method Measure 50 ml of leachate (7.2.2) in a 150 ml Erlenmeyer flask, add 5 ml nitric acid (5.2) and shake it. In the triangular bottle mouth Insert a small funnel, placed on the hot plate at 120 ℃ heating, in the micro-boiling state of the sample heated to about 5 ml, remove the cooling. Add 3 Ml of nitric acid (5.2), add 1 ml of perchloric acid (5.5) until the digestion is complete (digestion clarification, or digestion color and transparency The degree is no longer changed), continue at 180 ° C evaporation to near dry, remove the slightly cold, add 1 ml nitric acid solution (5.12), warm dissolved Soluble residue, after cooling with the amount of experimental water leaching small funnel and the inner wall of the flask, the amount of digestion solution to 50 ml capacity Measuring bottles, with the experimental water volume to the mark, shake, to be measured. If the digestion solution contains more impurities, need to be filtered, away from Heart separation or natural settlement. 7.3.2.2 Microwave digestion method Measure 50 ml leachate (7.2.2) (according to digestion tank volume and sample concentration to determine the amount of leaching volume to take the volume, the most The final solution volume should not exceed the limit specified by the instrument) in the microwave digestion tank, add 5 ml of nitric acid (5.2), according to the instructions Require to tighten the digestion tank. Place the digestion tank on the microwave oven. According to Table 2 of the temperature program to digest. After digestion, To be digested in the microwave digestion tank to cool to room temperature after the removal. Put it into the fume hood carefully to open the lid of the digestion tank and release it In the gas. The amount of digestion solution transferred to the polytetrafluoroethylene crucible, with the amount of experimental water rinse digestion tank wall, lotion and Into the polytetrafluoroethylene crucible, in the hot plate in the state of micro-boiling heated to near dry. With the amount of experimental water rinse crucible inner wall, The contents of the crucible and lotion transferred to 50 ml volumetric flask, with the experimental water volume to the mark, shake, to be measured. If the consumer The solution contains more impurities, need to be filtered, centrifugal separation or natural settlement. Table 2 Solid Waste Leach Solution Microwave Digestion Method Heating time (min) Digestion power (W) Digestion temperature (℃) Holding time (min) 10 400 room temperature ~ 150 5 5 500 150 ~ 180 5 Note 4. Due to the large number of solid wastes, the organic matter contained a large difference, and the amount of each acid in digestion can be increased or decreased as appropriate. The temperature of the hot plate should not be too high to prevent the deformation of the PTFE crucible; sample digestion, to prevent the dry, so as to avoid the loss of element to be measured. 7.3.3 Preparation of blank samples 7.3.3.1 Solid waste blank Use empty containers to prepare solid waste blank samples according to the procedure in 7.3.1. 7.3.3.2 Solid waste leachate blank Using the experimental water prepared as a leaching agent, according to 7.2.2 preparation of solid waste leachate blank, according to the steps of 7.3.2 into Line digestion.

8 Analysis steps

8.1 Instrument reference conditions Different models of flame atomic absorption spectrophotometer the best measurement conditions are different, according to the instrument manual Test conditions. The instrument reference measurement conditions are shown in Table 3. Table 3 Instrument reference measurement conditions Elemental Lead (Pb) Zinc (Zn) Cadmium (Cd) Determination of wavelength (nm) 283.3 213.9 228.8 Passband width (nm) 0.5 1.0 0.5 Lamp current (mA) 8.0 5.0 5.0 Flame Type Acetylene - Air, Neutral Acetylene - Air, Poor Combustion Acetylene - Air, Lean Burn 8.2 Standard curve drawing 8.2.1 Lead Standard Curve Series Accurate removal of 0.00 ml, 0.50 ml, 1.00 ml, 2.00 ml, 4.00 ml, 8.00 ml and 10.0 ml lead standards (5.18) in a group of 100 ml volumetric flask, with nitric acid solution (5.12) constant volume to the marking, shake. This standard series contains Lead were 0.00 mg/L, 0.50 mg/L, 1.00 mg/L, 2.00 mg/L, 4.00 mg/L, 8.00 mg/L and 10.0 mg/L, respectively. According to the instrument reference conditions (8.1), with nitric acid solution (5.12) to adjust the instrument zero, from low concentration to high concentration followed by suction Into the standard series, measuring the corresponding absorbance, with the corresponding absorbance as the ordinate to lead standard series of mass concentration for the abscissa, Establish lead calibration curve. 8.2.2 Zinc Standard Curve Series Accurately remove 0.00 ml, 0.50 ml, 1.00 ml, 2.00 ml, 3.00 ml, 4.00 ml and 5.00 ml zinc (5.19) in a group of 100 ml volumetric flask, with nitric acid solution (5.12) constant volume to the mark, shake. This standard series contains Zinc were 0.00 mg/L, 0.50 mg/L, 1.00 mg/L, 2.00 mg/L, 3.00 mg/L, 4.00 mg/L and 5.00 mg/L, respectively. According to the instrument reference conditions (8.1), with nitric acid solution (5.12) to adjust the instrument zero, from low concentration to high concentration followed by suction Into the standard series, measuring the corresponding absorbance, with the corresponding absorbance as the ordinate to zinc standard series of mass concentration for the abscissa, Establish a calibration curve for zinc. 8.2.3 cadmium standard curve series Respectively, accurate removal of 0.00 ml, 0.50 ml, 1.00 ml, 2.00 ml, 3.00 ml, 4.00 ml and 5.00 ml cadmium Liquid (5.20) in a group of 100 ml volumetric flask, with nitric acid solution (5.12) constant volume to the mark, shake. This standard series contains Cadmium were 0.00 mg/L, 0.50 mg/L, 1.00 mg/L, 2.00 mg/L, 3.00 mg/L, 4.00 mg/L and 5.00 mg/L, respectively. According to the instrument reference conditions (8.1), with nitric acid solution (5.12) to adjust the instrument zero, from low concentration to high concentration followed by suction Into the standard series, measuring the corresponding absorbance, with the corresponding absorbance as the ordinate, cadmium standard series of mass concentration for the abscissa, Establish cadmium calibration curve. 8.3 blank sample determination Prepare a blank sample (7.3.3) and perform the same conditions as the calibration curve. 8.4 Sample determination The prepared sample (7.3.1 or 7.3.2) was subjected to the same conditions as the established calibration curve.

9 Results calculation and representation

9.1 Results calculation 9.1.1 Solid waste 9.1.1.1 Solid or dry semi-solid solid waste The content of the element to be measured in solid waste  (mg/kg) Calculated according to formula (1)       (1) Where.  - the content of the element to be measured in the solid waste, mg/kg;  - Check the mass concentration of the element in the sample by the calibration curve, mg/L; 0_1 - Mass concentration in the laboratory blank sample, mg/L; 0V - volume of the sample after digestion, ml; 1m - the amount of solid waste sample weighed before drying, g; 2m - the quality of solid waste samples after drying, g; 3m - the amount of sample to be sintered after grinding, g. 9.1.1.2 Semi-solid solid waste with or without drying The content of the element to be measured in solid waste  (mg/kg) Calc...

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