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Solid waste - Determination of 47 organophosphorous and pyrethroid pesticides - Gas chromatography mass spectrometry
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HJ 963-2018
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Standard similar to HJ 963-2018 HJ 870 HJ 662 HJ 298 HJ 951 HJ 950
Basic data Standard ID | HJ 963-2018 (HJ963-2018) | Description (Translated English) | Solid waste - Determination of 47 organophosphorous and pyrethroid pesticides - Gas chromatography mass spectrometry | Sector / Industry | Environmental Protection Industry Standard | Classification of Chinese Standard | Z13 | Word Count Estimation | 39,346 | Date of Issue | 2018-07-29 | Date of Implementation | 2019-01-01 | Regulation (derived from) | Ministry of Ecology and Environment Announcement No. 27 of 2018 | Issuing agency(ies) | Ministry of Ecology and Environment |
HJ 963-2018: Solid waste - Determination of 47 organophosphorous and pyrethroid pesticides - Gas chromatography mass spectrometry ---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Solid waste - Determination of 47 organophosphorous and pyrethroid pesticides - Gas chromatography mass spectrometry
National Environmental Protection Standard of the People's Republic
Solid waste organophosphorus and pyrethroids
Determination of 47 pesticides by gas chromatography-mass spectrometry
Solid waste -Determination of 47 organophosphorous and pyrethroid
Pesticides- Gas chromatography mass spectrometry
Published on.2018-07-29
2019-01-01 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.3
7 Analysis steps..5
8 Results calculation and representation..8
9 Precision and accuracy 10
10 Quality Assurance and Quality Control..10
11 Waste treatment.11
Appendix A (Normative Appendix) Method Detection Limit and Lower Measurement Limit..12
Appendix B (informative) Characteristic ions of target compounds..16
Appendix C (informative) Method Precision and Accuracy 18
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
Protect the environment, protect human health, and regulate 47 kinds of pesticides such as organophosphorus and pyrethroids in solid waste and its leachate
The method of determination is to develop this standard.
This standard specifies the gas phase color of 47 pesticides such as organophosphorus and pyrethroids in solid waste and its leachate.
Spectral-mass spectrometry.
Appendix A of this standard is a normative appendix, and Appendix B~Appendix C is an informative appendix.
This standard is the first release.
This standard is formulated by the Environmental Monitoring Department and the Science and Technology Standards Department.
This standard was drafted. Zhejiang Environmental Monitoring Center.
This standard is verified by. Jiangsu Environmental Monitoring Center, Hubei Environmental Monitoring Center Station, Hangzhou Environmental Monitoring Center
Station, Ningbo Environmental Monitoring Center, Shaoxing Environmental Monitoring Center Station and Jiaxing Environmental Protection Monitoring Station.
This standard is approved by the Ministry of Ecology and Environment on July 29,.2018.
This standard has been implemented since January 1,.2019.
This standard is explained by the Ministry of Ecology and Environment.
1 Determination of 47 pesticides such as organophosphorus and pyrethroids in solid waste
Gas chromatography-mass spectrometry
Warning. The organic solvents and reference materials used in the experiment are toxic and hazardous substances, standard solution preparation and sample preparation.
The process should be carried out in a fume hood; protective equipment should be worn as required to avoid direct contact with skin and clothing.
1 Scope of application
This standard specifies the gas phase of 47 pesticides such as organophosphorus and pyrethroids in solid waste and its leachate.
Chromatography-mass spectrometry.
This standard applies to the determination of 47 pesticides such as organophosphorus and pyrethroids in solid waste and its leachate. its
His organophosphorus and pyrethroid pesticides have also been verified by this method.
Under the condition of selective ion (SIM), when the solid waste sample volume is 10.0 g and the constant volume is 1.0 ml, the target
The detection limit of the method is 0.2-0.9 mg/kg, and the lower limit of determination is 0.8-3.6 mg/kg. Solid waste leachate sample
When the product volume is 500 ml and the volume is 1.0 ml, the detection limit of the target is 0.006-0.02 mg/L. The lower limit of determination is
0.024 ~ 0.08 mg/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 782 solid waste organic matter extraction pressurized fluid extraction
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
After extraction, purification, concentration and constant volume of organophosphorus and pyrethroid pesticides in solid waste and its leachate,
It was separated by gas chromatography and detected by mass spectrometry. Qualitative according to mass spectrum, retention time, fragment ion mass-to-charge ratio and abundance ratio
Standard method of quantification.
4 reagents and materials
Analytically pure reagents in accordance with national standards were used for analysis, unless otherwise stated.
The pure water of the standard.
4.1 Acetone (C3H6O). pesticide residue level.
24.2 n-Hexane (C6H14). pesticide residue grade.
4.3 Dichloromethane (CH2Cl2). pesticide residue grade.
4.4 Acetonitrile (C2H3N). pesticide residue grade.
4.5 Hexane-acetone mixture. 1 1.
4.6 Acetonitrile-toluene mixture. 3 1.
4.7 Standard stock solution. pyrethroids, organophosphorus and heterocyclic pesticides, ρ=500 mg/L.
Commercially available certified standard solutions can be purchased directly or formulated with standard materials. Store as required by the standard solution certificate.
4.8 Internal standard stock solution. ρ=1000 mg/L.
Select tetrachloromethylene xylene (TCMX) as the internal standard solution, you can directly purchase the commercially available certified standard solution, or use the standard
Quasi-substance preparation.满足-d10, phenanthrene-d10, can also be used on the premise that the method requirements are met and the target compound is not interfered with.
Other internal standards such as 䓛-d12 and 芘-d12.
4.9 Mass spectrometry tuning solution. decafluorotriphenylphosphine (DFTPP), ρ = 5 mg/L.
Commercially available certified standard solutions can be purchased directly or prepared with standard materials and diluted with dichloromethane (4.3).
4.10 anhydrous sodium sulfate (Na2SO4). excellent grade pure.
Bake in a muffle furnace at 450 ° C for 4 h, cool, and seal in a ground glass bottle.
4.11 Diatomaceous earth. 0.6 to 0.9 mm (30 to 20 mesh).
Bake in a muffle furnace at 450 ° C for 4 h, cool, and seal in a ground glass bottle.
4.12 Quartz sand. 150 ~ 830 μm (200 ~ 100 mesh).
Bake in a muffle furnace at 450 ° C for 4 h, cool, and seal in a ground glass bottle.
4.13 Graphitized carbon black packing cartridge. 500 mg/6 ml.
4.14 Aminopropyl bonded silica packing cartridge. 500 mg/3 ml.
4.15 High purity nitrogen. purity ≥99.999%.
4.16 High purity helium. purity ≥99.999%.
5 Instruments and equipment
5.1 Gas Chromatography-Mass Spectrometry. The gas chromatograph section has a split/splitless inlet for temperature programming. Mass spectrometry
There is an electron bombardment ionization (EI) source.
5.2 Column. quartz capillary column, 30 m × 0.32 mm × 0.25 μm, stationary phase is 14% cyanopropyl phenyl-86%
Polysiloxane, or other equivalent column.
5.3 Extraction device. Soxhlet extractor, pressurized fluid extraction device or other equivalent extraction device.
5.4 Concentration device. Rotary evaporator, nitrogen blowing concentrator or other similar concentrating device.
5.5 purification device
5.5.1 Gel chromatograph. with UV detector, the purification column packing is neutral, porous polystyrene divinyl benzene gel,
Or the same size of filler.
5.5.2 Solid phase extraction equipment. manual or automatic.
5.6 Brown glass bottle. 500 ml, 1000 ml.
5.7 Common instruments and equipment used in general laboratories.
36 samples
6.1 Sample collection and preservation
Collection and storage of solid waste samples were carried out in accordance with the relevant regulations of HJ/T 20 and HJ/T 298. Sample collection after cleaning
Store in a brown brown ground glass jar. It should be refrigerated, protected from light and sealed during transportation. If it cannot be analyzed in time, it should be 4 °C
Refrigerated, protected from light, sealed and stored for less than 7 days.
6.2 Sample preparation
6.2.1 Solid and semi-solid solid waste
Weigh about 10 g (accurate to 0.01 g) of the sample, add an appropriate amount of anhydrous sodium sulfate (4.10), dry the sample, mix well
It is sandy and ready for use. Dehydrated with diatomaceous earth (4.11) if extracted with pressurized fluid.
6.2.2 Aqueous liquid solid waste
Weigh approximately 10 g (accurate to 0.01 g) of the sample, add 90 ml of water, mix and transfer to the separatory funnel.
6.2.3 Oily liquid solid waste
Weigh about 10 g (accurate to 0.01 g) of the sample, add 30 ml of dichloromethane (4.3), mix and transfer to the liquid
In the funnel, add 100 ml of water.
6.2.4 Solid waste leachate
Preparation of solid waste leachate according to the relevant requirements of HJ/T 299 or HJ/T 300. The leachate is cold at 4 ° C
Storage, protection from light, sealed storage, analysis of organophosphorus pesticides in leachate should be completed within 2 days, analysis of the leaching solution
Pyrethroids and heterocyclic pesticides need to be extracted within 7 days.
6.3 Preparation of samples
6.3.1 Preparation of solid and semi-solid waste samples
6.3.1.1 Extraction
The Soxhlet extraction or pressurized fluid extraction is selected for the extraction of the target.
a) Soxhlet extraction
Transfer all the dehydrated sample (6.2.1) to the extraction cup of the automatic Soxhlet extractor with.200300 ml.
The hexane-acetone mixture (4.5) is extracted for more than 8 h, and the reflux rate is controlled at 4-6 times/h. After cooling, the extract is concentrated.
Reduce the volume to 5 ml and analyze it for purification.
b) pressurized fluid extraction
Transfer the dehydrated sample (6.2.1) to the extraction cell and extract it with a pressurized fluid extraction device.
After cooling, the extract was concentrated to a volume of 5 ml and to be purified for analysis. Recommended extraction conditions. pressure 1500 psi, temperature 120 ° C,
The solvent n-hexane-acetone mixture (4.5) was extracted, 100% filled in the extraction cell mode, and allowed to stand at high temperature and high pressure for 5 min, and cycled three times.
Or set and optimize the extraction conditions according to HJ 782.
4 The sample extract was refrigerated at 4 ° C, protected from light, sealed and stored, and analyzed within 30 days.
Note 1. Other equivalent extraction methods can also be used if the quality control requirements of this method are met.
Note 2. Solvent conversion is carried out according to the solvent at the time of purification.
6.3.1.2 Purification of extract
According to the actual situation, choose one of the following purification methods for purification.
a) gel permeation chromatography purification
Perform instrument calibration according to the conditions of use of the instrument. Make sure the extract is free of suspended matter before purging. Converting solvent to solvent
For the methylene chloride (4.3) phase, 5.0 ml of the extract was loaded onto the gel permeation chromatography and used in accordance with the procedure.
The alkane (4.3) is rinsed, and it can also be rinsed with other suitable solvents, paying attention to the conversion of the solvent.
The collected eluent was concentrated to less than 1 ml with a concentration unit (5.4), and the internal standard was added to a volume of 1.0 ml to be analyzed.
b) solid phase extraction column purification
The extract was further concentrated to 1.0 ml for solid phase extraction column purification. Add in the graphitized carbon black packing column (4.13)
1 g of anhydrous sodium sulfate (4.10) was placed, and an aminopropyl bonded silica packing cartridge (4.14) was placed in series below. 4 ml acetonitrile before use -
The toluene mixture (4.6) was pre-rinsed in a series column. Transfer the sample to the purification column with 25 ml of acetonitrile-toluene mixture (4.6)
Rinse. The collected eluent was concentrated to less than 1 ml, and the internal standard was added to a volume of 1.0 ml to be analyzed.
Note. Other equivalent purification methods can also be used if the quality control requirements of this method are met.
6.3.2 Preparation of samples of solid waste leachate
Divide 500 ml of the leachate into a separatory funnel, extract with 30 ml of dichloromethane (4.3) each time, and extract three
The extract is dehydrated by anhydrous sodium sulfate (4.10), collected in a concentrated bottle, concentrated to 1.0 ml, and if necessary, press
Step 6.3.1.2 for purification. The extract was refrigerated at 4 ° C, protected from light, sealed and stored, and analyzed within 30 days.
6.3.3 Preparation of samples of aqueous liquid solid waste
Prepare samples of aqueous liquid solid waste according to the procedure in 6.3.2.
6.3.4 Preparation of oily liquid solid waste samples
Prepare the sample of oily liquid solid waste according to the procedure of 6.3.2.
6.4 Preparation of blank samples
6.4.1 Blank sample of solid waste
Replace the sample with quartz sand and perform the solid waste blank in the same procedure as the preparation of the solid waste sample (6.3.1).
Preparation of the sample.
6.4.2 Blank sample of solid waste leachate
Replace the sample with quartz sand and carry out the solid waste in the same procedure as the preparation of the solid waste leachate sample (6.3.2).
Preparation of a blank sample of the leachate.
57 Analysis steps
7.1 Instrument Reference Conditions
7.1.1 Gas Chromatography Reference Conditions
Temperature programmed. 40 ° C for 1 min, 30 ° C/min to 130 ° C, and then 5 ° C/min to 250 ° C,
The temperature was raised to 280 ° C at 10 ° C/min for 8 min. Inlet temperature. 270 ° C; injection method. split injection, minute
Flow ratio. 10.1. Carrier gas. helium gas; flow rate. 1.4 ml/min.
7.1.2 Mass Spectrometry Reference Conditions
Ion source. EI source; ion source temperature. 230 ° C; interface temperature. 280 ° C. Ionization energy. 70 eV; scanning side
Type. Select ion scanning mode (SIM), full scan mode (SCAN) for qualitative reference. Solvent delay time. 4.3 min.
See Appendix B for the selection of quantitative and auxiliary qualifier ions for each target.
7.2 Calibration
7.2.1 Instrument performance check
Prior to sample analysis, a 1 l mass spectrometry tuning solution (4.9) was injected directly to instrumentalize the gas chromatography-mass spectrometry system.
It can be checked that the abundance of the obtained mass ions should meet the requirements of Table 1, otherwise recalibration is required.
Table 1 Tetrafluorotriphenylphosphine (DFTPP) ion abundance evaluation table
Mass-to-charge ratio ion abundance standard mass-to-charge ratio abundance standard
51 strength is 30%~60% of 198 fragments.199 strength is 5%~9% of 198 fragments
68 2% strength less than 69 fragments 275 10% to 30% strength 198 fragments
70 strength less than 69 fragments of 2% 365 intensity greater than 1% of 198 fragments
127 40%~60% of the intensity of 198 fragments 441 exists but does not exceed the strength of 443 fragments
197 1% strength less than 198 fragments 442 strength greater than 40% of 198 fragments
198 base peak, relative intensity 100% 443 intensity is 17%~23% of 442 fragments
7.2.2 Preparation and determination of the standard series
Take 6 2 ml vials and add 976, 970, 960, 940, 880 and 780 μl of n-hexane (4.2) or two
Methyl chloride (4.3), then add 4.0, 10.0, 20.0, 40.0, 100,.200 μl standard stock solution A or B (4.7),
Finally, add 20.0 μl of internal standard stock solution (4.8) and mix. Formulated into 6 standard series of different concentrations, see Table 2.
Other suitable internal standard substances can also be used according to the principle of retention time.
According to the retention time of pesticides and related chemicals and the nature of pesticides, pesticides are divided into 2 groups, of which group A
It includes 10 pyrethroid pesticides, and Group B includes 37 organophosphorus and heterocyclic pesticides. The name of the specific compound is attached.
Record B.
6 Table 2 Preparation of standard series of pyrethroids, organophosphorus and heterocyclic pesticides
Standard Series CS-1 CS-2 CS-3 CS-4 CS-5 CS-6
Standard stock solution of pyrethroid pesticides (μl) (Group A) 4.0 10.0 20.0 40.0 100.200
Standard stock solution of organophosphorus and heterocyclic pesticides (μl) (Group B) 4.0 10.0 20.0 40.0 100.200
Internal standard use liquid volume (μl) 20.0 20.0 20.0 20.0 20.0 20.0
Constant volume (ml) 1.0 1.0 1.0 1.0 1.0 1.0
Internal standard (TCMX) concentration (mg/L) 20.0 20.0 20.0 20.0 20.0 20.0
Standard Series Concentration (mg/L) 2.0 5.0 10.0 20.0 50.0 100
According to the instrument reference conditions (7.1), the total ion chromatogram of the mass spectrometry of each target at different concentrations was obtained and recorded.
The retention time of each target and the peak area of the quantitative ion mass spectrum peak. The total ion current map of each target standard substance is shown in Figure 1 and
2.
5 .0 0 1 0 .0 0 1 5 .0 0 2 0 .0 0 2 5 .0 0 3 0 .0 0 3 5 .0 0
Time - - >
Abundance
TIC . 2 0 1 8 0 3 1 9 - 0 5 .D \\ data .ms
3, 4
6, 7
Internal standard
TCMX
Time (min)
Peak order. 1-transmethrin; 2-bifenthrin; 3-methrin; 4-cypermethrin; 5-pyrethrin; 6-permethrin; 7-cis chlorofluorocyanide Pyrethroid; 8-
Cypermethrin; 9-fenvalerate; 10- deltamethrin.
Figure 1 Total ion chromatogram of 10 pyrethroid pesticides
75 .0 0 1 0 .0 0 1 5 .0 0 2 0 .0 0 2 5 .0 0 3 0 .0 0
Time - - >
Abundance
TIC . 2 0 1 8 0 3 2 0 - 1 5 .D \\ data .ms
4 4 , 4 5
4 1 - 4 3
3 9 , 4 0
Internal standard
TCMX
3 0 - 3 4
2 2 - 2 7
twenty one
1 3 - 1 5
Time (min)
Peak order. 11-dichlorvos; 12-speed phosphorus; 13-endophosphorus (OS); 14-worm phosphorus; 15-fenke phosphorus; 16-methyl phosphate; 17-phosphorus; 18-two Azine
19; Ethyl Phosphate; 20-Dimethoate; 21-Spirulina; 22-chlorpyrifos; 23-methyl parathion; 24-toxin phosphorus; 25-amphophos; 26-phosphos; - Mala Sulfur
Phosphorus; 28-pustrin; 29-parathion; 30-bred phosphorus; 31-methylphosphorus sulfone; 32-phosphonium; 33-propiophos; 34-defattphos; 35- insecticidal; Adiamine
Phosphorus; 37-trisphosphine; 38-potentiated ether; 39-fipronil; 40-fungosporin; 41-fensulfuron sulfone; 42-endosulfan sulfate; 43-bromodecyl ester; 44-bromobenzene Phosphorus; 45-benzene
Phosphorus; 46-pyrazol; 47-floxacin.
Figure 2 Total ion current map of 37 organophosphorus pesticides and heterocyclic pesticides
7.2.3 Calculation of average relative response factor
The relative response factor (RRFi) of the i-th target of the standard series is calculated according to formula (1).
IS
IS
i C
RRF (1)
Where. iRRF -- the relative response factor of the i-th target in the standard series;
iA - the peak area of the i-th target in the standard series;
ISA - the peak area of the internal standard;
ISC - concentration of internal standard, mg/L;
iC -- The concentration of the i-th target in the standard series, mg/L.
The average relative response factor RRF of the target is calculated according to formula (2).
RRF
RRF
I
1 (2)
Where. RRF - the average relative response factor of the target;
iRRF - the relative response factor of the i-th target in the standard series;
n--Standard series points.
The standard deviation (SD) of 8RRF is calculated according to formula (3).
RRFRRF
SD
(3)
The relative standard deviation (RSD) of the RRF is calculated according to equation (4).
0
RRF
SD
RSD (4)
The relative standard deviation (RSD) of the relative response factors for the standard series of targets should be ≤ 20%.
7.2.4 Establishment of the standard curve
Taking the target concentration as the abscissa, the product of the peak area of the target and the corresponding internal standard concentration and the corresponding internal standard peak
The ratio of the product is the ordinate and a standard curve is established.
7.3 Specimen determination
The measurement of the sample (6.3) was carried out in accordance with the same instrument reference conditions as the standard curve. If the substance to be tested in the sample
The concentration is outside the range of the standard curve and should be re-measured after dilution.
7.4 Blank test
The blank sample (6.4) was measured in the same manner as in the sample measurement (7.3).
8 Calculation and representation of results
8.1 Qualitative analysis
The retention time (RRT) of the target in the sample, the auxiliary ion and the target ion abundance ratio are compared with the standard sample.
Sex.
The relative deviation of the retention time of the target compound in the sample from the retention time in the standard solution should be controlled within ±3%;
Auxiliary Qualitative Ion and Quantitative Ion Abundance Ratios of Target Compounds in Samples and Auxiliary Qualitative Ions and Quantitative Deviation in Standard Solutions
The sub-abundance ratio relative deviation should be within ±30%.
8.2 Quantitative analysis
8.2.1 Calculation of results of targets in solid waste samples
Calculate the concentration of the target in the solid waste sample using the average relative response factor according to formula (5);
The quasi-curve calculates the concentration of the target in the solid waste sample according to formula (6).
RRFA
iIS
IS 1w (5)
In the formula.
Wi--the concentration of the target in the sample, mg/kg;
Ai - the peak area of the target quantitative ion in the sample;
9ISA - the peak area of the internal standard quantitation ion in the sample;
IS -- the concentration of the internal standard in the sample, mg/L;
iRRF - the average relative response factor of the target;
V1 - sample volume, ml;
M--sample amount, g;
F--dilution factor.
Xi 1w (6)
In the formula.
Wi--the concentration of the target in the sample, mg/kg;
X - the concentration of the target in the sample obtained from the standard curve, mg/L;
V1 - sample volume, ml;
M--sample amount, g;
F--dilution factor.
8.2.2 Calculation of the results of the target in the leachate
Calculate the concentration of the target in the solid waste leaching solution using the average relative response factor according to formula (7);
The standard curve calculates the concentration of the target in the solid waste leachate according to formula (8).
RRFA
iIS
IS 1 (7)
In the formula.
i--the concentration of the target in the sample, μg/L;
Ai--the peak area of the target quantitative ion in the sample;
ISA - the peak area of the internal standard quantitation ion in the sample;
IS -- the concentration of the internal standard in the sample, mg/L;
iRRF - the average relative response factor of the target;
V1 - sample volume, ml;
V--sampling volume, L;
F--dilution factor.
Xi 1 (8)
In the formula.
i--the concentration of the target in the sample, μg/L;
X - the concentration of the target in the sample obtained from the standard curve, mg/L;
V1 - sample volume, ml;
V--sampling volume, L;
F--dilution factor.
8.3 result representation
The retention of the number of digits after the decimal point is consistent with the method detection limit, and up to 3 significant digits are retained.
9 Precision and accuracy
9.1 precision
Uniform samples of pesticide content of 1.0 mg/kg and 5.0 mg/kg in sludge solid waste samples from six laboratories
The measurements were made. the relative standard deviations in the laboratory were 1.8% to 32%, 0.068% to 13%, respectively;
The deviations were 4.4%~30%, 3.9%~24%, respectively; the repeatability limits were 0.1~0.6 mg/kg, 0.3~0.8 mg/kg, respectively;
The sexual limits were 0.2-0.9 mg/kg and 0.6-3.0 mg/kg, respectively. A laboratory has a pesticide content of sludge solid waste samples.
The 10.0 mg/kg sample was tested 6 times with a relative standard deviation ranging from 3.6% to 8.2%.
The six laboratories have pesticide contents of 0.020 mg/L and 0.100 mg/L in the sludge solid waste leachate samples.
Uniform samples were measured. the relative standard deviations in the laboratory were 1.5% to 31%, 0.76% to 15%, respectively;
The standard deviations were 6.0%~34%, 4.3%~27%, respectively; the repeatability limits were 0.004~0.01 mg/L, 0.001~0.02 respectively.
The reproducibility limits are 0.005~0.02 mg/L and 0.02~0.06 mg/L, respectively. Leaching of sludge solid waste in a laboratory
The sample with a pesticide content of 0.200 mg/L in the liquid sample was measur...
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