HJ/T 299-2007 English PDF (HJT299-2007)

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HJ/T 299-2007: Solid waste. Extraction procedure for leaching toxicity. Sulphuric acid and nitric acid method
HJ/T 299-2007
HJ
ENVIRONMENTAL PROTECTION INDUSTRY STANDARD
OF THE PEOPLE'S REPUBLIC OF CHINA
Solid waste - Extraction procedure for leaching toxicity -
Sulfuric acid and nitric acid method
ISSUED ON: APRIL 13, 2007
IMPLEMENTED ON: MAY 1, 2007
Issued by: State Environmental Protection Administration
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Terms and definitions ... 4
3 Principle ... 4
4 Reagents ... 5
5 Instruments and equipment ... 5
6 Sample storage and handling ... 6
7 Leaching steps ... 6
8 Quality assurance ... 8
9 Implementation of the standard ... 9
Appendix A (Informative) Diagram of Zero-Headspace Extraction Vessel (ZHE) ... 10
Solid waste - Extraction procedure for leaching toxicity -
Sulfuric acid and nitric acid method
1 Scope
This standard specifies the leaching procedures and quality assurance measures for the
leaching toxicity of solid waste.
This standard applies to the identification of leaching toxicity of organic and inorganic
substances in solid waste and its recycled products, as well as soil samples. Samples
containing non-water-soluble liquids are not applicable to this standard.
2 Terms and definitions
The following terms and definitions apply to this standard.
2.1 leaching
The process by which soluble components dissolve and change from the solid phase to
the liquid phase.
2.2 leaching toxicity
When solid waste comes into contact with water, the leached harmful substances
migrate and transform, polluting the environment. This hazardous characteristic is
called leaching toxicity.
2.3 initial liquid phase
For samples where both liquid and solid phases are evident, the liquid that is obtained
through filtration prior to the leaching steps.
3 Principle
This method uses a nitric acid/sulfuric acid mixed solution as an extractant to simulate
the process in which harmful components in waste are leached from the waste and enter
the environment under the influence of acid precipitation when the waste is disposed of
through irregular landfill or storage, or when the waste is reused in the land after non-
hazardous treatment.
4 Reagents
4.1 Reagent water: Use pure water that meets the requirements of the analytical method
standard of the substance to be tested.
4.2 Sulfuric acid ρ(H2SO4) = 1.84 g/ml, guaranteed reagent.
4.3 Nitric acid: ρ(HNO3) = 1.42 g/ml, guaranteed reagent.
4.4 1% nitric acid solution: Prepare by diluting concentrated nitric acid (4.3).
4.5 Extractant
4.5.1 Extractant 1#: Add a mixture of concentrated sulfuric acid and concentrated nitric
acid in a mass ratio of 2:1 to reagent water (about 2 drops of the mixture per 1 L of
water) to adjust the pH value to 3.20±0.05. This extractant is used to determine the
leaching toxicity of heavy metals and semi-volatile organic compounds in samples.
4.5.2 Extractant 2#: Reagent water, used to determine the leaching toxicity of cyanide
and volatile organic compounds.
5 Instruments and equipment
5.1 Oscillation equipment: a rotary oscillator with a rotation speed of (30±2) r/min.
5.2 Extraction container
5.2.1 Zero-Headspace Extraction Vessel (ZHE): 500~600 ml, a special device used to
leach volatile substances from samples.
5.2.2 Extraction bottle: 2 L wide-mouth bottle with a screw cap and inner cap, used to
leach non-volatile and semi-volatile substances in the sample. The extraction bottle
shall be made of an inert material that cannot leach or absorb the components contained
in the sample. When inorganic substances are analyzed, glass bottles or polyethylene
(PE) bottles can be used; when organic substances are analyzed, glass bottles or
polytetrafluoroethylene (PTFE) bottles can be used.
5.3 Filtration device
5.3.1 Zero-Headspace Extraction Vessel (ZHE): Analyze the volatile substances in the
sample, and use ZHE for filtration.
5.3.2 Vacuum filter or positive pressure filter: with a volume of ≥1 L.
5.3.3 Filter membrane: glass fiber filter membrane or microporous filter membrane,
tests.
7.2 Sample crushing
The sample particles shall be able to pass through a sieve with an aperture of 9.5 mm.
Large particles can be reduced in size by crushing, cutting or milling.
When determining the volatile organic compounds in a sample, a ruler shall be used to
measure the particle size to avoid loss of the components to be measured during sieving;
the sample and the tools used to reduce the particle size shall be cooled, and exposure
of the sample to the air shall be avoided as much as possible.
7.3 Leaching steps for volatile organic compounds
7.3.1 Cool the sample to 4 °C, weigh 40~50 g of the sample on a dry basis, and quickly
transfer it to the ZHE (5.3.1). Install the ZHE and slowly pressurize it to remove the
headspace.
7.3.2 When the sample contains an initial liquid phase, connect the leachate collection
device (5.5) to the ZHE, slowly increase the pressure until no more filtrate flows out,
collect the initial liquid phase, and store it in a refrigerator.
7.3.3 If the dry solid percentage in the sample is less than or equal to 9%, the initial
liquid phase obtained is the leachate and is analyzed directly; if the dry solid percentage
is greater than 9% of the total sample volume, continue with the following leaching
steps and mix the obtained leachate with the initial liquid phase for analysis.
7.3.4 Calculate the required volume of extractant based on the water content of the
sample and the liquid-to-solid ratio of 10:1 (L/kg). Add extractant 2# using the
extractant transfer device (5.6), install the ZHE, and slowly pressurize to remove the
headspace. Close all valves.
7.3.5 Fix the ZHE on the rotary oscillator (5.1), adjust the speed to (30±2) r/min, and
oscillate at (23±2) °C for (18±2) hours. After the oscillation stops, remove the ZHE and
check whether the device is leaking (if the ZHE device is leaking, resample for
leaching), collect the leachate with the same leachate collection device (5.5) that
collected the initial liquid phase, and store it in a refrigerator for analysis.
7.4 Leaching steps for substances other than volatile organic compounds
7.4.1 If the sample contains an initial liquid phase, filter the sample using a pressure
filter (5.3.2) and a filter membrane (5.3.3). If the dry solid percentage is less than or
equal to 9%, the initial liquid phase obtained is the leachate and is analyzed directly; if
the dry solid percentage is greater than 9%, leach from the filter residue according to
7.4.2, and mix the initial liquid phase with the leachate for analysis.