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HJ 975-2018

Chinese Standard: 'HJ 975-2018'
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BASIC DATA
Standard ID HJ 975-2018 (HJ975-2018)
Description (Translated English) Solid waste - Determination of benzene and its analogies - Headspace-gas chromatography
Sector / Industry Environmental Protection Industry Standard
Classification of Chinese Standard Z25
Word Count Estimation 17,151
Administrative Organization Ministry of Ecology and Environment

HJ 975-2018
Solid waste - Determination of benzene and its analogies - Headspace-gas chromatography
National Environmental Protection Standard of the People's Republic
Determination of benzene series in solid waste
Headspace-gas chromatography
Solid waste-Determination of benzene and its analogies
- Headspace-gas chromatography
Published on.2018-11-13
2019-03-01 Implementation
Ministry of Ecology and Environment released
i directory
Foreword.ii
1 Scope..1
2 Normative references..1
3 method principle..1
4 Reagents and materials.1
5 instruments and equipment. 2
6 samples. 2
7 Analysis steps..4
8 Results calculation and representation..5
9 precision and accuracy..6
10 Quality Assurance and Quality Control.7
11 Waste treatment 7
Appendix A (normative appendix) method detection limit and lower limit of measurement 8
Appendix B (informative) method of precision and accuracy..9
Foreword
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 Waste
This standard is formulated to protect the ecological environment, protect human health, and regulate the determination of benzene in solid waste and its leachate.
This standard specifies the headspace-gas chromatography for the determination of benzene in solid waste and its leachate.
Appendix A of this standard is a normative appendix, and Appendix B is an informative appendix.
This standard is the first release.
This standard is formulated by the Department of Eco-Environmental Monitoring, the Department of Regulation and Standards of the Ministry of Ecology and Environment.
This standard was drafted. Anshan City Environmental Monitoring Center Station.
This standard is verified by. Liaoning Provincial Environmental Monitoring Experimental Center, Shenyang Environmental Monitoring Center Station, Dalian Environmental Monitoring
Center, Fushun Environmental Monitoring Center Station, Liaoyang Environmental Monitoring Station and Jinzhou Environmental Monitoring Center Station.
This standard is approved by the Ministry of Ecology and Environment on November 13,.2018.
This standard has been implemented since March 1,.2019.
This standard is explained by the Ministry of Ecology and Environment.
1 Determination of solid waste benzene series by headspace-gas chromatography
Warning. The organic solvents and standard solutions used in the experiment are volatile and toxic substances. The reagent preparation and pretreatment process should be
In a fume hood; wear protective equipment as required to avoid direct contact with skin and clothing.
1 Scope of application
This standard specifies the headspace-gas chromatography for the determination of benzene in solid waste and its leachate.
This standard applies to solid waste and its leachate in benzene, toluene, ethylbenzene, p-xylene, m-xylene, cumene,
Determination of nine benzene compounds such as o-xylene, n-propylbenzene and styrene. Other standards for benzene compounds may also be used if they are verified.
Method determination.
When the solid waste sampling amount is 2 g, the detection limit of the nine target methods is 0.004~0.006 mg/kg, the lower limit of determination.
It is 0.016~0.024 mg/kg. When the solid waste leachate sample volume is 10 ml, the method detection limit of the nine targets is
0.7~2 μg/L, the lower limit of determination is 2.8~8 μg/L. See Appendix A for details.
2 Normative references
This standard refers to the following documents or their terms. For undated references, the valid version applies to this
standard.
HJ/T 20 Technical Specifications for Sampling and Sample Preparation of Industrial Solid Waste
HJ/T 298 Hazardous Waste Identification Technical Specification
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
3 Principle of the method
At a certain temperature, the benzene series in the sample in the headspace bottle volatilizes into the upper space, generating vapor pressure and achieving thermodynamic motion.
After the state equilibrium, the benzene series in the gas phase is separated by gas chromatography and detected by a flame ionization detector. Characterized by retention time,
Quantification by external standard method.
4 reagents and materials
Unless otherwise stated, analytically pure reagents that meet national standards were used for the analysis.
4.1 Experimental water. double distilled water or water prepared by ultrapure water meter. Need to pass a blank test before use, the target is thick
The degree is below the method detection limit.
4.2 Methanol (CH3OH). pesticide residue level or equivalent. Confirm the retention time interval of the target by blank test
There is no interference peak appearing inside.
4.3 Sodium chloride (NaCl).
It was fired in a muffle furnace at 400 ° C for 4 h, cooled and transferred to a ground glass bottle and stored in a desiccator.
24.4 Phosphoric acid (H3PO4). ρ=1.69 g/ml, excellent grade.
4.5 Saturated sodium chloride solution.
Measure 500 ml of water (4.1), add phosphoric acid (4.4) to adjust pH ≤ 2, add 180 g of sodium chloride (4.3), dissolve and
Mix and store at 4 ° C or below.
4.6 Standard stock solution. ρ = 1000 mg/L, the solvent is methanol. Can be purchased directly from commercially available certified standard solutions, or standard
Material preparation.
4.7 Standard use solution 1. ρ = 10 mg/L, the solvent is methanol.
4.8 Standard use solution 2. ρ = 100 mg/L, the solvent is methanol.
4.9 Quartz sand. 0.30~0.85 mm (50 ~ 20 mesh).
It was fired in a muffle furnace at 400 ° C for 4 h, cooled and transferred to a ground glass bottle and sealed for storage.
4.10 Carrier gas. high purity nitrogen (purity ≥ 99.999%).
4.11 Gas. High purity hydrogen (purity ≥ 99.999%).
4.12 Gas. Air.
5 Instruments and equipment
5.1 Gas Chromatograph. with capillary column split/splitless inlet, programmable temperature, flame ionization detector (FID).
5.2 Column. Quartz capillary column, 30 m × 0.32 mm × 0.25 m (polyethylene glycol 20M), can also be used
It is equivalent to a capillary column.
5.3 Headspace sampler. The temperature control range of the furnace is between room temperature and 120 °C; the temperature control accuracy is ±1 °C.
5.4 Reciprocating Oscillator. The oscillation frequency is 50~250 times/min, and the oscillation amplitude is 20 mm.
5.5 Balance. The sensitivity is 0.01 g.
5.6 Sampling bottle. 60 ml or.200 ml threaded brown wide-mouth glass bottle with Teflon/silica gel liner screw cap.
5.7 Sampling equipment. shovel and stainless steel medicine spoon.
5.8 Portable refrigerator.
5.9 Microinjectors. 5 μl, 10 μl, 25 μl, 100 μl, 500 μl, 1000 μl.
5.10 Brown compact bottle. 2 ml with Teflon liner and solid screw cap.
5.11 Headspace bottle. 22 ml with gasket (PTFE/silicone) and cap (screw cap or pressure for one use)
cover).
5.12 Common instruments and equipment used in general laboratories.
6 samples
6.1 Sample collection and preservation
6.1.1 Collect and store solid waste samples in accordance with the relevant provisions of HJ/T 20 and HJ/T 298. With a shovel and not
The rust steel spoon (5.7) quickly collects the sample into the sampling bottle (5.6) and fills it as much as possible. Quickly remove the sampling bottle thread
The sample adhered to the outer surface immediately seals the sample bottle. Place the sample bottle in a portable freezer (5.8) at 4 ° C
Save it and bring it back to the lab.
36.1.2 Samples should be analyzed as soon as they are sent to the laboratory. If it cannot be analyzed immediately, it should be sealed and stored below 4 °C.
The limit is no more than 14 days. The sample storage area should be free of target interference.
Note. Do not excessively agitate solid waste during sample collection to avoid volatilization of benzene in the sample.
6.2 Preparation of samples
6.2.1 Preparation of solid waste samples
6.2.1.1 Low content sample
Weigh 2 g (accurate to 0.01 g) into the headspace bottle (5.11) and quickly add 10.0 ml to the headspace bottle.
And sodium chloride solution (4.5), immediately sealed, and oscillated at 150 times/min for 10 min on a reciprocating oscillator (5.4).
To be tested.
6.2.1.2 High content sample
If the target content is greater than 1000 μg/kg, it should be considered as a high-content sample. The high content sample is prepared as follows. take out the sample
Bottle, weigh 2 g (accurate to 0.01 g) sample into the headspace bottle (5.11), quickly add 10.0 ml to the headspace bottle
The alcohol (4.2) was immediately sealed and oscillated on a reciprocating oscillator (5.4) at a frequency of 150 times/min for 10 min. Resting
After the drop, pipette approximately 1 ml of the methanol extract into a 2 ml brown compact bottle (5.10). The extract can be placed in a freezer at 4 ° C
Saved below, the shelf life is 14 days.
After returning the extract to room temperature before analysis, add 2 g (accurate to 0.01 g) to the empty headspace vial (5.11)
Quartz sand (4.9), 10.0 ml saturated sodium chloride solution (4.5) and 10~100 μl methanol extract, immediately sealed, in the
The compound oscillator (5.4) was oscillated at a frequency of 150 times/min for 10 min to be tested.
Note 1. If the concentration of benzene in the methanol extract is high, it can be diluted with methanol.
Note 2. If the content is too low or not detected by the high content method, the sample should be re-analyzed using the low content method.
6.2.2 Preparation of solid waste leachate
Preparation of solid waste water leaching solution according to HJ/T 299; preparation of solid waste acetic acid leaching solution according to HJ/T 300
kind.
6.3 Preparation of blank samples
6.3.1 Full program blank sample
10.0 ml of saturated sodium chloride solution (4.5) and 2 g (accurate to 0.01 g) of quartz sand (4.9) in the laboratory before sampling
Put it in the headspace bottle (5.11), take it to the sampling site, unpack it, seal it, and then transport it back to the laboratory with the sample.
It was oscillated on a reciprocating oscillator (5.4) at a frequency of 150 times/min for 10 min to be tested.
6.3.2 Laboratory blank sample
6.3.2.1 Solid waste low content blank sample
Weigh 2 g (accurate to 0.01 g) quartz sand (4.9) instead of low content, and prepare low content according to 6.2.1.1
Blank sample.
46.3.2.2 Solid waste high content blank sample
Weigh 2 g (accurate to 0.01 g) quartz sand (4.9) instead of high-content samples, and prepare high content according to 6.2.1.2
Blank sample.
6.3.2.3 Blank sample of solid waste leachate
A blank sample of the leachate was prepared in the same manner as the solid waste leachate preparation (6.2.2).
7 Analysis steps
7.1 Headspace Sampler Reference Conditions
Heating equilibrium temperature 85 ° C; heating equilibrium time 50 min; sampling needle temperature 100 ° C; transmission line temperature 110 ° C; pressure
The equilibrium time was 1 min; the injection time was 0.2 min; the needle removal time was 0.4 min.
7.2 Gas Chromatograph Reference Conditions
Temperature programming. 40 ° C for 6 min, ramp up to 110 ° C at 5 ° C/min, for 1 min, then 6 ° C
The heating rate of /min is raised to.200 ° C for 3 min; the inlet temperature is 220 ° C; the detector temperature is 240 ° C; carrier gas.
Nitrogen; column flow. 1.0 ml/min; hydrogen flow. 40 ml/min; air flow. 400 ml/min; injection method. minute
Flow injection; split ratio. 10.1.
A standard chromatogram of the nine benzene series is shown in Figure 1.
1-benzene; 2-toluene; 3-ethylbenzene; 4-p-xylene; 5-m-xylene; 6-isopropylbenzene; 7-o-xylene; 8-n-propylbenzene; 9-styrene .
Figure 1 9 benzene series standard chromatogram
7.3 Establishment of the working curve
7.3.1 Establishment of solid waste working curve
Add 2 g (accurate to 0.01 g) of quartz sand (4.9), 10.0 ml of saturated sodium chloride to the headspace bottle (5.11).
Liquid (4.5), then add 0 μl, 5 μl, 10 μl, 20 μl standard solution 1 (4.7) and 5 μl, 10 μl to each bottle.
20 μl of standard use solution 2 (4.8), immediately sealed, the target compound mass is 0 μg, 0.05 μg, 0.10 μg,
A 7-point working curve series of 50.20 μg, 0.50 μg, 1.00 μg, and 2.00 μg. Prepare a sample of the prepared working curve series at
The reciprocating oscillator (5.4) is oscillated at a frequency of 150 times/min for 10 min, according to the instrument reference conditions (7.1 and 7.2).
From the low content to the high content, the sample is injected sequentially, and the target compound mass (μg) is taken as the abscissa, and the peak area or peak height is the vertical position.
Mark, establish a working curve.
7.3.2 Establishment of working curve of solid waste leachate
Add 10.0 ml of leaching agent to the headspace bottle (5.11), and then add 0 μl, 5 μl, 10 μl to each bottle.
20 μl standard use solution 1 (4.7) and 5 μl, 10 μl, 20 μl standard use solution 2 (4.8), immediately sealed to prepare the target
Compound concentrations were 0 μg/L, 5.0 μg/L, 10.0 μg/L, 20.0 μg/L, 50.0 μg/L, 100 μg/L and.200 μg/L
7-point work curve series. According to the instrument reference conditions (7.1 and 7.2), the samples are injected sequentially from low to high concentrations.
The working curve is established by taking the target compound concentration (μg/L) as the abscissa and the peak area or peak height as the ordinate.
7.4 Sample determination
Place the sample (6.2) on the headspace sampler (5.3) and follow the same instrument strip as the establishment of the working curve (7.3).
The sample was measured.
7.5 Blank test
Place the blank sample (6.3) on the headspace sampler (5.3) and follow the same instrument conditions as the sample measurement (7.4).
The measurement of the blank sample was carried out.
8 Calculation and representation of results
8.1 Calculation of results of benzene series content in solid waste
8.1.1 Calculation of results of benzene series content in low-content solid waste
The benzene content w in the low-content solid waste is calculated according to the formula (1).
w  (1)
Where. w--the content of the target compound in the sample, mg/kg;
M0 - calculate the mass of the target compound based on the working curve, μg;
M1 - sample size (wet weight), g.
8.1.2 Calculation of results of benzene series content in high content solid waste
The benzene content in the high-content solid waste is calculated according to formula (2).
SVm
Fm
w 

0 V
(2)
Where. w--the content of the target compound in the sample, mg/kg;
M0--calculate the mass of the target compound according to the working curve, μg;
6V--the volume of the methanol extract, ml;
M1--sample amount (wet weight), g;
Vs--the volume of methanol extract used for headspace determination, ml;
f -- the dilution factor of the extract.
8.2 Calculation of the results of benzene concentration in solid waste leachate
When the solid waste leachate sample is measured, the concentration of the benzene series is directly obtained from the working curve and expressed in μg/L.
8.3 result representation
The number of decimal places and the method detection limit are consistent, and up to three significant digits are reserved.
9 Precision and accuracy
9.1 precision
Six laboratories for wastewater treatment plants with content levels of 0.025 mg/kg, 0.100 mg/kg and 0.500 mg/kg
The waste sediment samples were subjected to 6 replicate measurements. the relative standard deviations in the laboratory ranged from 3.6% to 20%,
4.3%~19% and 3.0%~20%; the relative standard deviation between laboratories is 5.9%~13%, 4.1%~9.3% and
1.8%~4.7%; repeatability limits are 0.004~0.012 mg/kg, 0.017~0.037 mg/kg and 0.087~0.165 respectively
The reproducibility limits ranged from 0.004 to 0.019 mg/kg, 0.019 to 0.044 mg/kg, and 0.093 to 0.174 mg/kg, respectively.
Six laboratories for waste sludge treatment plants with concentration levels of 5.0 μg/L, 20.0 μg/L and 100 μg/L
The water leaching sample was subjected to 6 repeated measurements. the relative standard deviations in the laboratory ranged from 1.2% to 14%,
0.88%~6.1% and 0.53%~4.7%; the relative standard deviation between laboratories is 2.8%~6.2%, 1.2%~5.9% and
0.78%~4.2%; repeatability limits are 0.6~1 μg/L, 1~2.4 μg/L and 6.4~8.6 μg/L, respectively; reproducibility limits
They are 0.8~2 μg/L, 1.8~4 μg/L and 7.5~13.5 μg/L, respectively.
Six laboratories for waste sludge treatment plants with concentration levels of 5.0 μg/L, 20.0 μg/L and 100 μg/L
The acetic acid leaching sample was subjected to 6 repeated measurements. the relative standard deviations in the laboratory ranged from 2.2% to 9.7%,
1.8%~9.8% and 0.88%~8.7%; the relative standard deviations between laboratories ranged from 3.3% to 8.7% and 1.8% to 4.2%, respectively.
1.8%~6.0%; repeatability limits are 0.7~1 μg/L, 1~2.8 μg/L and 7.3~12.6 μg/L, respectively; reproducibility limit range
They are 0.8~2 μg/L, 2~3.5 μg/L and 10.6~18 μg/L, respectively.
See Appendix B for precision data.
9.2 Accuracy
Six laboratories for sewage treatment plants with spiked contents of 0.025 mg/kg, 0.100 mg/kg and 0.500 mg/kg
The samples of discarded sediments were analyzed by spike analysis. the recoveries ranged from 34.8% to 71.8%, 42.3% to 70.7%, and
65.7%~94.0%; the final recoveries of the spiked recovery were 39.1%±8.6%~67.2%±7.9%, respectively.
49.1% ± 7.1% ~ 64.1% ± 8.1% and 68.9% ± 4.8% ~ 89.8% ± 5.2%.
Six laboratories for waste sludge treatment at concentrations of 5.0 μg/L, 20.0 μg/L and 100 μg/L
The samples of water leaching were analyzed by spike analysis. the recoveries ranged from 78.1% to 96.8% and 82.9% to 103%, respectively.
90.2%~104%; the final recoveries were 83.0%±6.8%~91.3%±6.8%, 92.4%±12%~99.8%±3.1%
7 and 95.3% ± 3.6% to 99.8% ± 4.7%.
Six laboratories for waste sludge treatment at concentrations of 5.0 μg/L, 20.0 μg/L and 100 μg/L
The samples of acetic acid leaching were analyzed by spike analysis. the recoveries ranged from 79.6% to 99.0% and 83.1% to 108%, respectively.
And 87.1%~104%; the final recoveries of the spiked recovery are 86.1%±13%~93.2%±6.8%, respectively.
86.3%±6.5%~103%±7.3% and 93.9%±7.6%~ 97.9%±6.7%.
See Appendix B for accuracy data.
10 Quality Assurance and Quality Control
10.1 Blank test
A full program blank sample and a laboratory blank should be analyzed for every 20 samples or batches (less than 20/batch)
For the sample, the target compound content in the measurement results should be lower than the method detection limit.
10.2 Working curve
The working curve is drawn according to the concentration and response value of the target, and the correlation coefficient should be ≥0.995.
10.3 Calibration Confirmation
For every 20 samples or every 24 h, use the middle point of the working curve to confirm the calibration. The measured value of the target compound and the initial value
The ratio of the initial value should be in the range of 80% to 120%. Otherwise, the work curve should be redrawn.
10.4 Parallel samples
A parallel sample should be analyzed for every 20 samples or batches (less than 20/batch).
The deviation is ≤ 20%.
10.5 Matrix addition
A blank spiked sample and matrix spiked sample should be analyzed for every 20 samples or batches (less than 20/batch), empty
The recovery rate of the target in the white sample should be 70%~120%, and the recovery rate of the target in the actual sample should be 30%~135%.
Otherwise, the sample should be reanalyzed.
11 Waste treatment
The waste generated by the experiment shall be stored in a classified manner, stored in a centralized manner, and entrusted to a qualified unit for processing.
8 Appendix A
(normative appendix)
Method detection limit and lower limit of determination
Table A.1 gives the method detection limits and lower limit of determination for 2 g solid waste and 10 ml solid waste leachate.
Table A.1 Detection limits and lower limit of determination of the method
Compound name English name
Solid waste solid waste leachate
The detection limit
(mg/kg)
Lower limit of measurement
(mg/kg)
The detection limit
(μg/L)
Lower limit of measurement
(μg/L)
1 benzenebenzene 0.005 0.020 0.7 2.8
2 toluene toluene 0.005 0.020 2 8
3 ethylbenzene ethylbenzene 0.005 0.020 0.9 3.6
4 p-xylene p -xylene 0.004 0.016 0.7 2.8
5 m-xylene m -xylene 0.005 0.020 0.9 3.6
6 cumene isopropylbenzene 0.004 0.016 0.7 2.8
7 o-xylene o-xylene 0.005 0.020 1 4
8 n-propylbenzene n-propylbenzene 0.004 0.016 1 4
9 styrene styrene 0.006 0.024 0.7 2.8
9 Appendix B
(informative appendix)
Method precision and accuracy
Tables B.1 to B.6 show the precision of solid waste, solid waste water leachate and solid waste acetic acid leachate, respectively.
Degree and accuracy data.
Table B.1 Precision of the solid waste method
Serial number
Compound
name
content
(mg/kg)
Experimental room relative
standard deviation(%)
Interlaboratory
standard deviation(%)
Repeatability limit r
(mg/kg)
Reproducibility limit R
(mg/kg)
1 benzene
0.017 5.5~19 5.9 0.005 0.006
0.064 4.3~14 6.3 0.017 0.019
0.432 6.8~12 1.8 0.104 0.110
2 toluene
0.067 3.6~9.6 8.1 0.012 0.019
0.114 4.8~16 9.2 0.037 0.044
0.504 3.0~9.0 1.8 0.089 0.093
3 ethylbenzene
0.012 15~19 12 0.006 0.007
0.056 13~18 8.4 0.024 0.026
0.404 4.2~13 3.7 0.100 0.100
4 p-xylene
0.012 15~20 13 0.005 0.007
0.058 10~19 7.0 0.026 0.027
0.383 12~18 4.2 0.154 0.161
5-xylene
0.012 9.5~19 11 0.006 0.006
0.055 11~19 6.6 0.023 0.024
0.385 12~20 3.4 0.165 0.174
6 cumene
0.010 9.7~19 12 0.004 0.005
0.056 6.4~17 4.1 0.021 0.021
0.374 9.5~20 4.7 0.141 0.144
7 o-xylene
0.011 13~20 9.0 0.005 0.006
0.055 14~18 9.3 0.024 0.027
0.372 8.3~19 2.3 0.132 0.141
8 n-propylbenzene
0.010 12~19 8.7 0.004 0.005
0.056 5.6~19 8.5 0.023 0.025
0.365 8.2~19 3.3 0.129 0.136
9 styrene
0.010 6.3~19 11 0.004 0.004
0.049 11~19 7.2 0.020 0.021
0.345 4.5~12 3.5 0.087 0.087
Table B.2 Accuracy of solid waste methods
Serial number
Compound
name
content
(mg/kg)
Addition recycling
Rate range (%)
Addition recycling
Rate average (%)
Standardized recovery rate
standard deviation(%)
Scaling recovery final value
SP 2/(%)
1 benzene
0.017 61.0~71.8 67.2 4.0 67.2±8.0
0.064 60.4~70.7 64.1 4.1 64.1±8.2
0.432 84.5~88.7 86.4 1.6 86.4±3.2
2 toluene
0.067 40.0~54.0 46.9 5.0 46.9±10
0.114 52.5~69.7 59.0 7.0 59.0±14
0.504 86.5~94.0 89.8 2.6 89.8±5.2
3 ethylbenzene
0.012 40.8~55.5 49.0 5.9 49.0±12
0.056 49.1~61.7 56.3 4.7 56.3±9.4
0.404 76.3~85.5 80.9 3.0 80.9±6.0
4 p-xylene
0.012 38.6~55.9 46.2 6.2 46.2±12
0.058 52.0~62.4 58.1 4.1 58.1±8.2
0.383 71.1~80.2 76.7 3.2 76.7±6.4
5-xylene
0.012 40.7~54.5 47.8 5.3 47.8±11
0.055 51.2~59.8 55.4 3.7 55.4±7.4
0.385 72.9~80.1 77.0 2.6 77.0±5.2
6 cumene
0.010 36.3~48.4 41.8 5.1 41.8±10
0.056 53.2~59.2 56.1 2.3 56.1±4.6
0.374 70.5~79.6 74.8 3.5 74.8±7.0
7 o-xylene
0.011 39.5~51.3 44.9 4.1 44.9±8.0
0.055 49.3~63.4 54.9 5.1 54.9±10
0.372 71.9~76.6 74.4 1.7 74.4±3.4
8 n-propylbenzene
0.010 35.9~43.3 39.4 3.4 39.4±6.8
0.056 50.8~63.8 56.4 4.8 56.4±9.6
0.365 69.5~75.1 73.0 2.4 73.0±4.8
9 styrene
0.010 34.8~46.8 39.1 4.3 39.1±8.6
0.049 42.3~52.5 49.1 3.5 49.1±7.0
0.345 65.7~71.1 68.9 2.4 68.9±4.8
Table B.3 Precision of the method of solid waste water leaching
Serial number
Compound
name
concentration
(μg/L)
Experimental room relative
standard deviation(%)
Interlaboratory
standard deviation(%)
Repeatability limit r
(μg/L)
Reproducibility limit R
(μg/L)
1 benzene
4.6 3.5~8.2 3.6 0.7 0.8
19.3 1.6~6.1 4.5 2.4 3.3
98.8 1.3~3.9 0.83 8.4 8.8
2 toluene
9 3.0~7.9 6.2 1 2
23 0.93~3.3 5.9 1 4
100 1.4~4.7 1.4 8 8
3 ethylbenzene
4.5 4.1~6.7 4.9 0.6 0.9
19.7 0.88~4.4 1.2 1.8 1.8
99.8 0.55~3.7 2.4 7.0 9.2
4 p-xylene
4.5 4.7~8.1 6.0 0.7 1.0
19.4 1.2~4.7 3.9 1.9 2.7
97.3 1.0~4.3 4.2 8.0 13.5
5-xylene
4.5 1.4~8.1 2.8 0.6 0.7
19.7 1.1~3.8 2.0 1.7 1.9
99.7 0.83~3.0 1.7 6.4 7.5
6 cumene
4.4 1.7~10 6.2 0.8 1.0
19.7 1.2~4.4 2.5 1.8 2.1
98.5 1.8~4.0 2.8 7.4 10.2
7 o-xylene
4 1.2~8.5 3.0 1 1
19 1.4~4.7 3.1 2 2
99 1.8~4.6 2.0 8 9
8 n-propylbenzene
5 1.4~7.1 4.0 1 1
20 1.4~5.0 2.0 2 2
99 1.1~3.5 0.78 8 8
9 styrene
4.4 1.2~14 3.1 0.9 0.9
20.0 0.76~5.2 1.5 2.3 2.3
98.6 0.53~4.4 1.6 8.6 9.1
Table B.4 Accuracy of the method of solid waste water leaching
Serial number
Compound
name
concentration
(μg/L)
Spike recovery
range(%)
Spike recovery
Mean (%)
Standardized recovery rate
standard deviation(%)
Scaling recovery final value
SP 2/(%)
1 benzene
4.6 86.7~96.6 91.3 3.3 91.3±6.6
19.3 88.0~99.8 96.5 4.4 96.5±8.8
98.8 98.0~100 98.8 0.82 98.8±1.6
2 toluene
9 78.1~87.9 83.0 3.4 83.0±6.8
23 82.9~98.3 92.4 5.8 92.4±12
100 93.3~97.9 95.3 1.8 95.3±3.6
3 ethylbenzene
4.5 81.7~93.5 90.1 4.5 90.1±9.0
19.7 96.4~99.7 98.5 1.1 98.5±2.2
99.8 96.5~104 99.8 2.4 99.8±4.8
4 p-xylene
4.5 81.2~96.8 90.5 5.5 90.5±11
19.4 91.4~103 97.1 3.8 97.1±7.6
97.3 90.2~102 97.3 4.1 97.3±8.2
5-xylene
4.5 87.8~94.3 90.6 2.6 90.6±5.2
19.7 96.0~102 98.4 2.0 98.4±4.0
99.7 98.1~103 99.7 1.7 99.7±3.4
6 cumene
4.4 80.5~92.4 87.5 5.4 87.5±11
19.7 94.7~102 98.6 2.5 98.6±5.0
98.5 93.6~102 98.5 2.7 98.5±5.4
7 o-xylene
4 84.9~90.3 88.5 2.7 88.5±5.4
19 92.1~98.0 95.7 3.0 95.7±6.0
99 96.3~102 99.0 1.9 99.0±3.8
8 n-propylbenzene
5 83.9~92.9 89.3 3.6 89.3±7.2
20 97.6~103 99.5 2.0 99.5±4.0
99 98.6~101 99.3 0.77 99.3±1.5
9 styrene
4.4 84.8~92.1 88.6 2.7 88.6±5.4
20.0 97.3~102 99.8 1.5 99.8±3.0
98.6 96.3~100 98.6 1.6 98.6±3.2
Table B.5 Precision of the method for solid waste acetic acid leachate
Serial number
Compound
name
concentration
(μg/L)
Experimental room relative
standard deviation(%)
Interlaboratory
standard deviation(%)
Repeatability limit r
(μg/L)
Reproducibility limit R
(μg/L)
1 benzene
4.6 3.5~7.0 3.5 0.7 0.8
20.1 2.1~7.4 1.8 2.3 2.3
97.9 1.7~4.4 3.4 8.5 12.2
2 toluene
8 2.2~9.4 8.7 1 2
21 2.0~3.1 3.0 1 2
97 1.4~4.6 3.6 10 13
3 ethylbenzene
4.6 3.7~9.2 3.8 0.7 0.8
20.2 1.8~3.6 3.5 1.6 2.4
96.7 0.88~3.5 3.0 7.3 10.6
4 p-xylene
4.6 3.4~9.4 3.3 0.8 0.8
20.3 1.9~3.8 3.6 1.5 2.5
97.7 1.4~6.0 3.2 10.8 13.3
5-xylene
4.6 3.4~9.0 3.8 0.7 0.8
20.5 2.0~6.0 3.5 1.9 2.7
97.4 1.2~4.9 3.2 8.9 11.9
6 cumene
4.6 3.7~9.7 5.1 0.7 0.9
20.1 2.2~9.8 4.2 2.8 3.5
94.3 2.9~4.9 3.9 10.3 13.9
7 o-xylene
5 2.9~9.2 6.3 1 1
20 1.8~4.1 2.7 1 2
96 1.9~4.8 6.0 10 18
8 n-propylbenzene
5 3.7~9.5 3.6 1 1
20 2.2~4.4 1.8 2 2
98 1.5~4.9 1.8 11 11
9 styrene
4.6 3.9~8.4 3.4 0.7 0.8
19.2 2.0~4.1 4.0 1.5 2.5
96.8 1.1~8.7 4.7 12.6 17.1
Table B.6 Accuracy of the method for solid waste acetic acid leachate
Serial number
Compound
name
concentration
(μg/L)
Spike recovery
range(%)
Spike recovery
Mean (%)
Standardized recovery rate
standard deviation(%)
Scaling recovery final value
SP 2/(%)
1 benzene
4.6 87.8~97.2 92.5 3.3 92.5±6.6
20.1 98.4~103 101 1.9 101±3.8
97.9 94.4~103 97.9 3.4 97.9±6.8
2 toluene
8 79.6~96.7 86.1 6.3 86.1±13
21 83.1~89.6 86.3 3.2 86.3±6.4
97 88.7~98.2 93.9 3.8 93.9±7.6
3 ethylbenzene
4.6 88.8~97.4 92.4 3.5 92.4±7.0
20.2 97.0~106 101 3.5 101±7.0
96.7 93.3~102 96.7 2.9 96.7±5.8
4 p-xylene
4.6 87.1~93.5 91.3 3.0 91.3±6.0
20.3 98.7~108 101 3.7 101±7.4
97.7 92.3~102 97.7 3.2 97.7±6.4
5-xylene
4.6 87.5~96.2 92.5 3.5 92.5±7.0
20.5 96.8~106 103 3.6 103±7.2
97.4 93.8~102 97.4 3.1 97.4±6.2
6 cumene
4.6 86.7~99.0 92.0 4.7 92.0±9.4
20.1 95.4~106 101 4.3 101±8.6
94.3 88.7~98.6 94.3 3.6 94.3±7.2
7 o-xylene
5 82.5~98.1 91.2 5.8 91.2±12
20 94.9~103 98.2 2.7 98.2±5.4
96 87.1~97.2 95.5 5.8 95.5±12
8 n-propylbenzene
5 88.1~97.2 93.2 3.4 93.2±6.8
20 99.4~104 101 1.8 101±3.6
98 95.9~100 97.9 1.8 97.9±3.6
9 styrene
4.6 89.2~96.8 91.9 3.1 91.9±6.2
19.2 89.5~100 96.1 3.8 96.1±7.6
96.8 90.6~104 96.8 4.5 96.8±9.0
Related standard:   HJ 973-2018  HJ 976-2018
Related PDF sample:   HJ 693-2014  HJ 629-2011
   
 
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