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GB 5085.3-2007Identification standards for hazardous wastes -- Identification for extraction toxicity (English PDF)

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Issued by

General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China

Level / Type

National · Mandatory

Issue date

April 25, 2007

Implementation date

October 1, 2007

Scope

GB 5085.3-2007 (Identification standards for hazardous wastes -- Identification for extraction toxicity) is available as an English-translated PDF.

GB 5085.3-2007 — This standard specifies the toxicity characteristic leaching to hazardous waste identification standard. This standard applies to any production, life and other activities generated solid waste leaching toxic identification.

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Document preview — GB 5085.3-2007

National Standard of the People's Republic of China

ICS: 13.030.50
Classification: Z 70
Replacing: GB 5085.3-1996

Issued by: General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China

Appendix E solid waste arsenic, antimony, bismuth, selenium Atomic Fluorescence Spectrometry32

Foreword

To implement the "People's Republic of China Environmental Protection Law" and "People's Republic of China Solid Waste Pollution Prevention Law"

Environmental pollution prevention caused by hazardous waste, strengthen the management of hazardous waste, protect the environment, protect human health, the development of

This standard.

This standard is part of the national hazardous waste identification standard. National hazardous waste identification standard solid waste

Hazardous characteristics Technical indicators hazardous characteristics standard technical specifications of solid waste are hazardous waste, required by law

Hazardous waste management. National Hazardous Waste Identification standard consists of the following seven criteria consists of.

1, hazardous waste identification standard General

2 Identification standard for hazardous wastes Identification corrosion

3, hazardous waste identification standard acute toxicity screening

4 Identification of hazardous waste leaching toxic identification standard

5 Identification standard for hazardous wastes Identification Flammability

6, hazardous waste identification standard differential reactivity

7, hazardous waste identification standard differential toxic substance content

This standard "Identification standard for hazardous wastes - Identification for extraction procedure toxicity" (GB 5085.3-1996) has been revised, the main

It reads.

- Based on the original identification of the standard 14 projects, an increase of 37 identification projects. New projects mainly organic

Class of toxic substances.

- Modify the leaching of toxic substances.

- Modify the Analytical Methods section identification project.

According to relevant laws and regulations, the standard shall be enforceable.

This standard was proposed by the State Environmental Protection Administration of Science, Technology.

This standard was drafted. Chinese Research Academy of Environmental Sciences, Institute of solid waste pollution control technology, environmental standards research

The.

This standard SEPA March 27, 2007 for approval.

This standard since October 1, 2007 implementation, "Identification standard for hazardous wastes - Identification for extraction procedure toxicity" (GB

5085.3-1996) is abolished.

This standard is interpreted by the State Environmental Protection Administration.

Identification standard for hazardous waste leaching toxic identification

1 Scope

This standard specifies the toxicity characteristic leaching to hazardous waste identification standard.

This standard applies to any production, life and other activities generated solid waste leaching toxic identification.

2 Normative references

The following documents contain provisions which, through reference in this Part of GB 5085 and become the standard terms. Undated

Reference documents, the latest versions apply to this standard.

HJ/T 299 methods for leaching toxicity of solid waste sulfuric acid nitric acid method

HJ/T 298 Identification of Hazardous Waste Technical Specifications

3 Identification Standard

The solid waste leachate HJ/T 299 prepared a danger to any ingredients than listed in Table 1 Concentration

Limit, it is determined that the solid waste is a hazardous waste leaching toxicity characteristics.

Table 1 leaching toxic identification standard value

Item No. Hazardous Components Hazard leaching solution concentration limit (mg/L) Analysis

Inorganic elements and compounds

1 copper (Cu total count) 100 Appendix A, B, C, D

2 zinc (Zn total count) 100 Appendix A, B, C, D

3 Cadmium (Cd total count) 1 Appendix A, B, C, D

4 Lead (total lead) 5 Appendix A, B, C, D

5 Total chromium 15 Appendix A, B, C, D

Chromium 6 (hexavalent) 5 GB/T 15555.4-1995

7 alkyl mercury may not be detected 1 GB/T 14204-93

8 Mercury (Hg total count) 0.1 Appendix B

9 beryllium (beryllium total count) 0.02 Appendix A, B, C, D

10 Ba (barium total count) 100 Appendix A, B, C, D

11 Nickel (Ni total count) 5 Appendix A, B, C, D

Total 12 silver and 5 in Appendix A, B, C, D

13 Arsenic (total arsenic meter) 5 Appendix C, E

14 selenium (total selenium meter) 1 Appendix B, C, E

15 inorganic fluorides (excluding calcium fluoride) 100 Appendix F

16 cyanide (CN- in dollars) APPENDIX G

Organic pesticides

Item No. Hazardous Components Hazard leaching solution concentration limit (mg/L) Analysis

17 DDT 0.1 Appendix H

18 BHC 0.5 Appendix H

19 8 Appendix I dimethoate

20 pairs of parathion 0.3 Appendix I

Methyl parathion 0.2 21 Appendix I

22 5 Appendix I malathion

23 Chlordane 2 Appendix H

HCB 24 5 Appendix H

25 APPENDIX 3 H toxaphene

Mirex 26 0.05 Appendix H

Non-volatile organic compounds

Nitrobenzene 27 20 Appendix J

28 20 Appendix K dinitrobenzene

29 pairs of 5-nitro chlorobenzene Appendix L

5-nitro-2,4-dichlorobenzene 30 Appendix L

31 pentachlorophenol and sodium pentachlorophenol (PCP to count) 50 Appendix L

32 Phenol 3 Appendix K

33 6 Appendix K 2,4-dichlorophenol

34 2,4,6-trichlorophenol 6 Appendix K

35 Benzo (a) pyrene 0.0003 Appendix K, M

Dibutyl phthalate, butyl 2 Appendix K 36

Octyl phthalate 37 3 Appendix L

38 Appendix N PCBs 0.002

Volatile Organic Compounds

Benzene 39 1 Appendix O, P, Q

40 Toluene 1 Appendix O, P, Q

Ethylbenzene 41 4 Appendix P

Xylene 42 4 Appendix O, P

43 chlorobenzene 2 Appendix O, P

44 1,2-dichlorobenzene 4 Appendix K, O, P, R

45 1,4-dichlorobenzene 4 Appendix K, O, P, R

46 Acrylonitrile 20 Appendix O

47 3 Appendix Q chloroform

CTC 48 0.3 Appendix Q

49 3 Appendix Q trichlorethylene

50 PCE 1 Appendix Q

Note 1. "not detected" means methylmercury < 10ng/L, ethyl mercury < 20ng/L.

4 Experimental Method

4.1 sampling sites and sampling methods according to HJ/T 298 performed.

4.2 Samples of inorganic elements and their compounds (except hexavalent chromium, inorganic fluorides, cyanides outside) pretreatment method reference

Appendix S; sample pretreatment methods and hexavalent chromium compounds See Appendix T.

Pretreatment methods of organic samples refer to Appendix 4.3 U, V, W.

4.4 Determination of harm each component of the project, in addition to implementation of the provisions of the standard analytical methods, the Zanan specified in Appendix enforcement methods

Line; After specific hazards for the determination of the national environmental protection standard component items released, according to standard regulations.

5 of Standards

This standard by the people's governments above the county level environmental protection administrative department responsible for overseeing implementation.

Appendix A solid wastes by inductively coupled plasma atomic emission element Spectrometry

Solid Waste - Determination of Elements

- Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES)

1 Scope

This method is applicable to solid waste and solid waste leaching solution of silver (Ag), aluminum (Al), arsenic (As), barium (Ba), beryllium (Be),

Calcium (Ca), cadmium (Cd), cobalt (Co), chromium (Cr), copper (Cu), iron (Fe), potassium (K), magnesium (Mg), manganese (Mn),

Sodium (Na), Nickel (Ni), lead (Pb), antimony (Sb), strontium (Sr), thorium (Th), titanium (Ti), thallium (Tl), vanadium (V),

Inductively coupled plasma atomic zinc (Zn) and other elements of Emission Spectrometry.

The method detection limits and measurement wavelength of various elements are shown in Table 1.

Table 1 Recommended measuring element and wavelength detection limit

Determination Element Wavelength (nm) detection limit (mg/L) was measured Element Wavelength (nm)

The detection limit

(Mg/L)

308.21 0.1 Cu 327.39 0.01 Al 396.15 0.09 238.20 0.03

As 193.69 0.1 Fe 259.94 0.03

233.53 0.004 K 766.49 0.5 Ba 455.40 0.003 279.55 0.002

313.04 0.0003 Mg 285.21 0.02 Be 234.86 0.005 257.61 0.001

317.93 0.01 Mn 293.31 0.02 Ca 393.37 0.002 Na 589.59 0.2

214.44 0.003 Ni 231.60 0.01 Cd 226.50 0.003 Pb 220.35 0.05

238.89 0.005 Sr 407.77 0.001 Co 228.62 0.005 334.94 0.005

205.55 0.01 Ti 336.12 0.01 Cr 267.72 0.01 V 311.07 0.01

Cu 324.75 0.01 Zn 213.86 0.006

May exist when this method uses the main interference in Table 2.

Table 2-element interference

Determination of elements measurement wavelength (nm) interference element determination of elements

Measurement wavelength

(Nm) interference element

308.21 Mn, V, Na 202.55 Fe, Mo Al

396.15 Ca, Mo 267.72 Mn, V, Mg

As 193.69 Al, P

283.56 Fe, Mo

313.04 Ti, Se Cu 324.7 Fe, Al, Ti Be

234.86 Fe Mn 257.61 Fe, Al, Mg

Ba 233.53 Fe, V Ni 231.60 Co

315.89 Co Pb 220.35 Al Ca 317.93 Fe 290.88 Fe, Mo

214.44 Fe 292.40 Fe, Mo

226.50 Fe

311.07 Ti, Fe, MnCd

228.80 As Zn 213.86 Ni, Cu

Co 228.62 Ti Ti 334.94 Cr, Ca

Principle 2

ICP-AES measurement sample may be multi-element content at the same time. When the argon gas by a plasma torch, radiofrequency occur

Unit alternating electromagnetic field generated by ionizing accelerate and collide with other argon atoms. This chain reaction so that more argon atoms ionized form

Atoms, ions, electrons particles are mixed gas, i.e., plasma. Filtered or treated sample digestion through the injector device is materialized materialized

By argon carrier gas into a plasma torch, the vaporized sample molecules are gasified at a high temperature plasma torch, ionization, excitation. different

Atomic elements in the excitation or ionization may emit a characteristic spectrum, the plasma emission spectroscopy is used to qualitative determination of element present in the sample

Su. The intensity and spectral characteristics were determined from concentration, compared with the standard solution, can be quantitatively determined content of each element in the sample.

3 Reagents and materials

3.1 Reagent water as GB/T 6682 provided a water.

3.2 nitric acid (HNO3), rho = 1.42g/ml, pure class distinctions.

3.3 hydrochloric acid (HCl), rho = 1.19g/ml, pure class distinctions.

3.4 (1 + 1) nitrate solution with nitric acid (3.1).

3.5 argon gas cylinder, purity of not less than 99.9%.

3.6 standard solution.

3.6.1 preparation unit standard stock solution. can be purchased from commercial establishments authority or formulated with ultra-pure chemical reagents and metal ( > 99.99%)

To 1.00mg/ml of the standard stock solution. A commercially available metal plate-like, linear, granular, spongy, or powder and the like. In order to facilitate the weighing,

Need to chip (except powdered), cuttings should be cut to prevent the contamination or lathe to cut, usually first with dilute HCl or dilute HNO3

Quickly washed to remove surface metal oxide and the deposited soil, and then washed with water. Dry quickly, acetone and other strong volatility available

Solvent was further washed to remove moisture, and finally with pure dry nitrogen or argon. Stock solution preparation acidity is maintained at 0.1mol/L or more (see

table 3).

Table 3 single-element standard stock solution preparation method

Element concentration (mg/ml) Preparation method

Al 1.00 Weigh 1g of aluminum, with 150mlHCl (1 1) was dissolved by heating, boiling, cooling water volume to 1L

Zn 1.00 Weigh 1g of zinc metal, with 40mlHCl dissolved, boiled, cooled water to the 1L

Ba 1.00 Weigh 1.5163g anhydrous BaCl2 (250 °C drying 2h), with 20ml (1 1) HNO3 dissolved in water to 1L

Be 0.1 Weigh 0.1g metal beryllium, heating 150mlHCl (1 1) was dissolved, after cooling water to the 1L

Ca 1.00 Weigh 2.4972gCaCO3 (110 °C drying 1h), dissolved in 20ml water until completely dissolved solution of HCl, plus 10mlHCl, boiled to remove CO2, after cooling water to the 1L

Co 1.00 Weigh 1g cobalt metal with 50ml (1 1) HNO3 dissolved by heating, cooling water volume to 1L

Cr 1.00 Weigh 1g chromium, heated and dissolved 30mlHCl (1 1) at, after cooling water to the 1L

Cu 1.00 Weigh 1g of copper, is heated and dissolved 30mlHNO3 (1 1), the cooling water to the 1L

Fe 1.00 Weigh 1g metallic iron dissolved 150mlHCl (1 1), after the cooling water volume to 1L

K 1.00 Weigh 1.9067gKCl (at 400 ~ 450 °C burning to no crackling) was dissolved in water, water volume to 1L

Mg 1.00 Weigh 1g of magnesium, adding 30ml of water was added slowly 30mlHCl, until completely dissolved, boiled, cooled water to the 1L

Na 1.00 Weigh 2.5421gNaCl (at 400 ~ 450 °C burning to no crackling) was dissolved in water, water volume to 1L

Ni 1.00 Weigh 1g of nickel, with 30mlHNO3 (1 1) is heated and dissolved, after cooling water to the 1L

Pb 1.00 Weigh 1g metallic lead, with 30mlHNO3 (1 1) is heated and dissolved, after cooling water to the 1L

Sr 1.00 Weigh 1.6848gSrCO3 with 60mlHCl (1 1) is heated and dissolved, after cooling water to the 1L

Ti 1.00 Weigh 1g titanium, heating 100mlHCl (1 1) was dissolved, after cooling water to the 1L

After V 1.00 Weigh 1g of vanadium metal, heated and dissolved with 30ml of water, concentrated to near dryness, 20mlHCl cooling water to the 1L

Cd 1.00 Weigh 1g metal cadmium, dissolved 30mlHNO3, water volume to 1L

Mn 1.00 Weigh 1g of manganese metal, heating 30mlHCl (1 1) was dissolved, after cooling water to the 1L

As 1.00 Weigh 1.3203gAs2O3, with 20ml10% of NaOH dissolved (a little heat), diluted with water to a solution of HCl to slightly acidic, add 5mlHCl (1 1), then with water to 1L

3.6.2 single element formulation intermediate standard solution. dispensing the single-element standard stock solution, the Cu, Cd, V, Cr, Co, Ba, Mn,

Ti and Ni 10 Elements diluted to 0.10mg/ml; the Pb, As and Fe diluted to 0.5mg/ml; diluted to Be 0.01mg/ml of

Single element intermediate standard solution. When diluted, supplemented with a certain amount of the corresponding acid, the solution pH is maintained at 0.1ml/L or more.

3.6.3 preparation of multi-element mixed standard solution. For the determination of many elements simultaneously, streamline operations procedures, mutual interference between elements must be in accordance with

The nature of the case with a standard solution with a single element of the intermediate standard solution, grouping formulated as multi-element mixed standard solution. Because of the standard solution

Fluid properties and performance of the instrument and the sample under test project requirements are different, grouping elements are not the same. Table 4 lists the methods of the present article

Member grouping table of elements under reference. Acidity mixed standard solution should be consistent with the acidity of the sample solution.

Table 4 multi-element mixed standard solution grouping

I II III

Element concentration (mg/L) concentration of the element (mg/L) concentration of the element (mg/L)

Ca 50 K 50 Zn 1.0

Mg 50 Na 50 Co 1.0

Fe 10 Al 50 Cd 1.0

Ti 10 Cr 1.0

V 1.0

Sr 1.0

Ba 1.0

Be 0.1

Ni 1.0

Pb 5.0

Mn 1.0

As 5.0

4 instruments, equipment and working conditions

4.1 Instrument

Inductively coupled plasma emission spectrometer and general laboratory equipment and the corresponding auxiliary equipment. Common inductively coupled plasma emission

Multi-channel spectrometer is usually divided into two kinds of formula and a sequential scan.

4.2 Working conditions

Usually when the instrument using a common gas atomizer, simultaneous determination of many elements of the operating parameters are shown in Table 5.

Table 5 Operating parameters eclectic range

High-frequency power

Rate (kW)

Reflected power

(W)

Observation height

(Mm)

Carrier gas flow

(L/min)

Plasma gas

Flow (L/min)

Injection volume

(Ml/min)

Measuring time

(S)

1.0 ~ 1.4 < 1.0 ~ 56 ~ 16 ~ 1.5 1.0 ~ 1.5 1.5 ~ 3.0 20 1

5 sample collection, preservation and pretreatment

5.1 All sample containers should be used previously with detergent, acid washed and reagents, plastic and glass containers. If you want to analyze easily

Selenium, antimony and arsenic compounds volatile, to use a special container (such as a container for volatile organic analysis).

5.2 water sample must be acidified with nitric acid to a pH of less than 2.

5.3 Non-aqueous samples should be kept refrigerated and analyzed as soon as possible.

5.4 When analyzing samples of soluble arsenic, does not require refrigeration, it should be stored away from light, temperature should not exceed room temperature.

5.5 silver standard and sample should be stored in a brown bottle and placed in the dark.

6 of eliminate interference

By ICP-AES interference normally present can be divided into two categories. one is the spectral interference, including the continuous background and overlapping lines dry

Scrambling, the other non-spectral interference, including interference chemical ionization interference, physical interference and the solvent interference in the actual analysis

Process various kinds of interference difficult to completely separate. Under normal circumstances, it must be compensated and corrected.

In addition, general physical interference by the viscosity and surface tension of the sample level change caused; especially when the sample contains large amounts of soluble salts or sample

Product acidity is too high, it will interfere with the determination. The easiest way to eliminate such interference is to dilute the sample.

6.1 Interference matrix element

Optimization of test conditions to select the optimum operating parameters, no doubt less interference effects by ICP-AES, but due to the complex composition of wastewater,

Between a large number of elements and trace element contents vary greatly, so the interference from the large number of elements can not be ignored. Table 2 lists the analyte in the proposed

The main spectral interferences Analysis wavelengths.

6.2 Interference correction

Correction interference between elements in many ways, the chemical effect is obvious enrichment separation methods can improve the detection ability of the elements, but the operating procedures

Burdensome and easy introduction of the reagent blank; matrix matching method (similar to the sample preparation and matrix component standard solution) results are quite satisfactory.

This method for sample matrix components fixed determination, it is the ideal way to eliminate the interference, but there is a high purity reagents difficult problem to solve,

Wastewater matrix composition and unpredictable, in actual analysis, the preparation of the working standard solution will be very troublesome; and relatively simple project

Before the commonly used method is background subtraction method (with tests to determine the location and manner of background-subtracted) and interference coefficient method, when there is a single element interference

When, according to the formula

- =

Obtained interference factor. Where iK is the interference coefficient; 'Q is interfering elements plus the element content analysis; Q is

Analysis of the content of elements; iQ is the content of interfering elements. Through a series of elements known to interfere with the content of the element in the analysis solution preparation wavelength bits

Set measured 'Q, according to the above...

END: Draft Version (GB 5085.3-2007)

......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — all pages — is available in the English PDF.

Referenced standards

Normative references

GB 5085

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