HJ 786-2016Solid waste. Determination of Lead, Zinc and Cadmium. Flame atomic absorption spectrometry (English PDF)

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 reagents conforming to national standards are used in the analysis, and the test water is a newly prepared deionized water.

5.1 sulfuric acid. rho (H2SO4) = 1.84 g/ml, excellent grade pure.

5.2 nitric acid. rho (HNO3) = 1.42 g/ml, excellent grade pure.

5.3 hydrochloric acid. rho (HCl) = 1.19 g/ml, excellent grade pure.

5.4 hydrofluoric acid. rho (HF) = 1.49 g/ml, excellent grade pure.

5.5 perchloric acid. rho (HClO4) = 1.68 g/ml, excellent grade pure.

5.6 Hydrogen peroxide. phi (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. rho = 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. rho = 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. rho = 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. rho = 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. rho = 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. rho = 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 °C), the maximum temperature can be set to.200 °C.

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

9 Results calculation and representation