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Solid waste. Determination of organic phosphorous pesticides. Gas chromatography
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Basic data
| Standard ID | HJ 768-2015 (HJ768-2015) |
| Description (Translated English) | Solid waste. Determination of organic phosphorous pesticides. Gas chromatography |
| Sector / Industry | Environmental Protection Industry Standard |
| Word Count Estimation | 17,194 |
| Date of Issue | 2015-11-20 |
| Date of Implementation | 2015-12-15 |
| Quoted Standard | HJ/T 20; HJ/T 298; HJ/T 299; HJ/T 300 |
| Regulation (derived from) | Ministry of Environment Announcement 2015 No.73 |
| Issuing agency(ies) | Ministry of Ecology and Environment |
| Summary | This Standard specifies the determination of solid waste and leachate of organophosphorus pesticides by gas chromatography. This Standard applies to the determination of the leaching solution of organophosphorus pesticides and 12 kinds of solid waste, including Profenophos, phorate, dimethoate, diazinon, phorate, IBP, methyl parathion, MA pull parathion, chlorpyrifos, parathion, ethyl parathion and phenthoate. If verified, this standard is also applicable to the determination of other organophosphate pesticides. |
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HJ 511|HJ 768-2015: Solid waste. Determination of organic phosphorous pesticides. Gas chromatography
---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 organic phosphorous pesticides.Gas chromatography
2015-11-20 release
2015-12-15 implementation
National Environmental Protection Standard of the People 's Republic of China
Determination of organophosphorus pesticides in solid wastes
Gas chromatography
Solid Waste-Determination of Organic Phosphorous Pesticides-
Gas Chromatography
Ministry of Environmental Protection released
Directory
Preface ii
1 Scope of application
2 normative reference documents
3 Principle of the method
4 interference and elimination
5 reagents and materials 1
6 instruments and equipment 2
7 Sample 3
8 Analysis steps
9 Results Calculations and Representations 6
10 precision and accuracy
11 quality assurance and quality control
12 Waste treatment
Appendix A (normative appendix) method detection limit and lower limit of measurement
Appendix B (Normative Appendix) Purification of samples
Appendix C (informative) Auxiliary Qualitative Column Reference Conditions 11
Appendix D (informative) Method Precision and Accuracy 12
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,
Protection of human health, regulate solid waste and its leaching solution of organophosphorus pesticide determination method, the development of this standard.
This standard specifies the determination of solid waste and its leaching solution of organophosphorus pesticide gas chromatography.
This standard is the first release.
Appendix A and B of this standard are normative appendices, Appendix C, Appendix D are informative appendices.
This standard is organized by the Ministry of Environmental Protection Science and Technology Standards Division.
The main drafting unit of this standard. Shanghai Environmental Monitoring Center.
The standard verification unit. Suzhou City Environmental Monitoring Center Station, Shanghai Huangpu District Environmental Monitoring Station, Shanghai Textile Energy Conservation and Environmental Protection Center, on
City Putuo District Environmental Monitoring Station, Shanghai Qingpu District Environmental Monitoring Station, Shanghai Songjiang District Environmental Monitoring Station.
The Environmental Protection Department of this standard approves on November 20,.2015.
This standard is implemented as of December 15,.2015.
This standard is explained by the Ministry of Environmental Protection.
Solid waste - Determination of organophosphorus pesticides - Gas chromatographic method
Warning. The organic solvent used in the test, the standard substances are toxic substances, the solution preparation, pre-treatment process should be in the fume hood
To carry out the operation; according to the provisions of the requirements of wearing protective equipment, to avoid contact with skin and clothing.
1 Scope of application
This standard specifies the determination of solid waste and its leaching solution of organophosphorus pesticide gas chromatography.
This standard is applicable to the determination of 12 organophosphorus pesticides in solid waste and its leachate, including propenbromide, phorate, dimethoate, diazepine
Agriculture, B, mixed with phosphorus, different rice blast net, methyl parathion, malathion, chlorpyrifos, parathion, rice feng and ethionin. If verified,
This standard can also be applied to the determination of other organophosphorus pesticides.
Determination of solid waste, when the sampling volume of 10.0 g, 12 kinds of organophosphorus pesticide method detection limit of 0.6 μg/kg ~ 1.2 μg/kg, under the determination of
Limited to 2.4 μg/kg to 4.8 μg/kg. Determination of solid waste leachate, when the sampling volume of 100 ml, 12 kinds of organophosphorus pesticide method detection
Limited to 0.2 μg/L to 0.3 μg/L, the determination of the lower limit of 0.8 μg/L ~ 1.2 μg/L. See Appendix A. for details.
2 normative reference documents
The contents of this standard refer to the following documents or their terms. For undated references, the valid version applies to 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
3 Principle of the method
Solid waste or solid waste leaching solution of organic phosphorus pesticides extracted by organic solvents, the extract was concentrated by volume and then by gas chromatography
From the flame photometric detector to determine the time to qualitative, external standard method.
4 interference and elimination
When the extract contains interferences, the appropriate cleaning method can be used to remove the interference, recommended purification method see Appendix B. Can also be used
Auxiliary column or gas chromatography-mass spectrometry (GC/MS) is further characterized. The characteristics of the auxiliary characterization column and the chromatographic reference are described in Appendix C.
5 reagents and materials
Unless otherwise stated, analytical analytical reagents conforming to the relevant standards are used for the analysis, and the test water is a new preparation for the absence of the target
Sub-water.
5.1 n-hexane (C6H14). chromatographic purity.
5.2 Acetone (CH3COCH3). Chromatographic pure.
5.3 dichloromethane (CH2Cl2). chromatographic purity.
5.4 Sodium chloride (NaCl).
5.5 n-Hexane - Acetone Mixed Solvent. 9 1 (v/v).
Mixed with n-hexane (5.1) and acetone (5.2) at a volume ratio of 9. 1.
5.6 Standard stock solution. ρ =.200 mg/L.
Can be directly purchased commercially available standard solution; can also be prepared with standard materials, preparation of the solvent is n-hexane (5.1). Including propyl bromide,
Phorate, dimethoate, dibenzoyl, phiophosphate, different rice blast net, methyl parathion, malathion, chlorpyrifos, parathion, rice feng and ethidium
phosphorus.
5.7 standard use of liquid. ρ = 5.00 mg/L.
Add 3 900 μl of n-hexane (5.1) to a 4 ml brown bottle and add 100 μl of standard stock solution (5.6) to mix.
5.8 anhydrous sodium sulfate (Na2SO4). baked at 400 ℃ for 4 h, placed in a dryer to cool to room temperature, transferred to the grinding glass bottle,
In the dryer to save.
5.9 Diatomite. 100 mesh to 400 mesh, baked at 400 ℃ for 4 h, placed in a dryer to cool to room temperature, transferred to the grinding glass bottle, in the
Dryer in the preservation.
5.10 Quartz sand. 20 mesh to 50 mesh, baked at 400 ℃ for 4 h, placed in a dryer to cool to room temperature, transferred to the grinding glass bottle, in the dry
Cooler to save.
5.11 filter paper. the speed of qualitative filter paper.
5.12 paper sleeve. with Soxhlet extraction device.
5.13 nitrogen (N2). purity ≥99.999%.
5.14 Hydrogen (H2). purity ≥99.999%.
6 instruments and equipment
6.1 Gas Chromatograph. with split/splitless inlet with flame photometric detector (FPD).
6.2 Column. 30 m x 0.25 mm x 0.25 μm, ultra low loss (5% phenyl) -methylpolysiloxane capillary column; or 30 m x 0.32 mm x
0.25 [mu] m, (14% cyano-phenyl) -methylpolysiloxane capillary column, or other equivalent capillary column.
6.3 Extraction equipment. Soxhlet extractor or pressurized fluid extractor.
6.4 Concentration device. nitrogen blowing concentrator or other enrichment device.
6.5 separatory funnel. with PTFE (PTFE) piston.
6.6 Microinjectors. 10 μl, 25 μl, 100 μl, 250 μl, 500 μl and 1 000 μl.
6.7 Common laboratory equipment and equipment.
7 samples
7.1 Collection and storage of samples
Samples are collected and stored in accordance with the relevant regulations of HJ/T 20 and HJ/T 298.
After the sample is collected, it must be sealed and stored in a pre-washed and dried brown glass bottle for analysis as soon as possible. If not immediately analyzed, should be at 4 ℃
The following cold storage preservation, storage period of not more than 7 d. The sample extract is kept in cold storage for a period of no more than 40 days.
Note 1. try to avoid stirring when collecting samples, so as to avoid the degradation or volatilization of organophosphorus pesticides in solid waste.
7.2 Preparation of the sample
7.2.1 Preparation of solid waste leachate samples
7.2.1.1 Leaching
A sample of solid waste leachate was prepared in accordance with the relevant provisions of HJ/T 299 or HJ/T 300.
7.2.1.2 Extraction
Take the solid waste leachate (7.2.1.1) 100 ml in the separatory funnel (6.5), add appropriate amount of sodium chloride (5.4) shake, add 20 ml
Dichloromethane (5.3) was shaken and allowed to stand, and the organic phase was removed through a funnel equipped with an appropriate amount of anhydrous sodium sulfate (5.8), washed with dichloromethane (5.3)
The sodium sulfate was thoroughly washed and the organic phase was collected. The extraction was repeated twice as described above, and the organic phase was combined and collected in a concentrated tube to be concentrated.
Note 2. The amount of leachate can be appropriately reduced according to the organic pollutant content. The leachate should be extracted immediately.
Note 3. Emulsification of the extract can be demolished using mechanical separation or centrifugation.
7.2.1.3 Concentration and purification
7.2.1.3.1 Concentration
When concentrated using a nitrogen blower, the bath temperature was 35 ° C. Concentrate to 10 ml, add 10 ml of n-hexane (5.1), continue to concentrate to 1.0 ml.
Other suitable enrichment methods may also be used such as KD concentration, rotary evaporation enrichment, and the like.
7.2.1.3.2 Purification
If there is matrix interference in the sample, silica gel column and silica gel solid phase extraction column can be used for purification, see Appendix B. If you pass the test
Card, other suitable purification methods may also be used.
7.2.2 Preparation of solid waste samples
7.2.2.1 Water-based liquid solid waste
Weigh 10.0 g (accurate to 0.1 g) sample, add 90 ml of water, mix it all into the separatory funnel (6.5), the rest according to 7.2.1.2
And 7.2.1.3.
7.2.2.2 Oily liquid solid waste
Weigh 10.0 g (accurate to 0.1 g) sample, add 30 ml of dichloromethane (5.3), mix it all into the separatory funnel (6.5)
Add 100 ml of water, the rest according to 7.2.1.2 and 7.2.1.3 steps.
7.2.2.3 Solid and semi-solid waste
7.2.2.3.1 Dehydration
Weigh 10.0 g (accurate to 0.1 g) sample, add the appropriate amount of anhydrous sodium sulfate (5.8), the sample dry and mix well into the flow sand, spare.
If a pressurized fluid extractor is used, it is dehydrated with diatomaceous earth (5.9).
Note 4. Immediately after sample preparation, extraction should be performed to reduce the degradation of organophosphorus pesticides. It is not suitable to prepare samples by air drying, grinding, crushing, etc.
For hard solid waste samples that can not be agitated and can only be crushed, etc., the degradation of organophosphorus pesticides should be taken into account.
Note 5. The sampling volume can be adjusted according to the type of sample, pollutant content, extraction method. For samples with high levels of organic pollutants, sampling may be appropriately reduced
the amount.
7.2.2.3.2 Extraction
Separate the solid waste sample from 7.2.2.3.1 into the paper sleeve (5.12) and add 100 ml of n-hexane-acetone mixed solvent (5.5)
The extraction rate was controlled at 6 times/h for 16 h ~ 18 h. The extract was collected in a concentrated tube and concentrated. If verified, can also make
Use other suitable extraction methods.
Note 6. Ultrasonic extraction is not suitable for this method.
7.2.2.3.3 Concentration and purification
7.2.2.3.3.1 Concentration
When concentrated using a nitrogen blower, the bath temperature was 35 ° C. The extract was concentrated to 1.0 ml and tested. KD can also be used to concentrate, rotary steaming
Such as enrichment and other suitable enrichment methods.
Note 7. When the nitrogen is concentrated, the extract is concentrated to about 1.0 ml. If the concentration continues, with the reduction of the volume of the extract, consideration should be given to the loss of organophosphorus pesticides
Lost
Note 8. high content of organic pollutants in the sample, may be appropriate to increase the volume of fixed volume.
7.2.2.3.3.2 Purification
With the purification procedure of 7.2.1.3.2.
8 Analysis steps
8.1 Gas Chromatographic Reference Conditions
Oven temperature program. 60 ℃ for 0.5 min, to 70 ℃/min temperature to 100 ℃, 45 ℃/min temperature to 180 ℃ to 20
℃/min to.200 ℃ and kept for 6.5 min, heated to 280 ℃ at 45 ℃/min and kept for 10 min; inlet temperature..200 ℃;
Injection method. no split injection; FPD detector temperature. 250 ℃. Gas flow. nitrogen 1.5 ml/min, hydrogen 75 ml/min, air
300 ml/min.
8.2 Calibration
(5.7), diluted with n-hexane (5.1) to make the target compound concentration of 0.00 μg/L, respectively,
20 μg/L, 100 μg/L, 250 μg/L, 500 μg/L, 1 000 μg/L and 2 000 μg/L respectively. The assay was carried out under the recommended chromatographic conditions (8.1)
The calibration curve was plotted with the mass concentration of each component as the abscissa and the peak area (or peak height) of the component as the ordinate.
Note 9. Adjust the calibration curve according to the actual situation of the sample.
8.3 reference chromatogram
According to the gas chromatographic reference conditions (8.1) analysis, 12 organophosphorus pesticides in the ultra-low loss (5% phenyl) - methyl polysiloxane chromatography
The reference chromatogram on the column is shown in Fig.
The order of the peak. 1-propyl bromophosphate; 2-phorate; 3-dimethoate; 4-diazinon; 5-B; Malathion; 9 - chlorpyrifos;
10-parathion; 11-rice fengshen; 12-ethoxifen.
Figure 1 12 organic phosphorus pesticide reference chromatogram
8.4 Determination
The prepared sample (7.2) was measured according to the gas chromatographic reference conditions (8.1).
8.5 blank test
Solid waste leachate blank. Weigh 100.0 g of quartz sand (5.10), prepare the sample according to 7.2.1, according to gas chromatography
Condition (8.1).
Solid waste blank. Weigh 10.0 g of quartz sand (5.10) and prepare the sample according to 7.2.2 according to the gas chromatographic reference conditions (8.1)
To be measured.
9 Results calculation and representation
9.1 Target compound Qualitative
According to the retention time of the components of the standard substance. If you have any questions about the results, you can use a second column or gas chromatography - qualitative
(GC/MS), the chromatograms of 12 organophosphorus pesticides on the secondary qualitative column are shown in Appendix C.
9.2 Result calculation
9.2.1 Calculation of component concentration in solid waste leachate
The target compound is quantified by the external standard method. The target compound concentration ρ (μg/L) in the solid waste leachate is calculated according to the formula (1)
Count.
X V
V × = ρρ (1)
Where. ρ - the concentration of the target compound in the leachate, μg/L;
Xρ - the mass concentration of the target compound calculated from the calibration curve, μg/L;
XV - extract concentration volume, ml;
IV - leachate sampling volume, ml.
9.2.2 Calculation of component content in solid waste
The target compound is quantified by the external standard method and the target compound content ω (μg/kg) in the solid waste is calculated according to the formula (2).
Xm
V × = ρω (2)
Where. ω - the content of the target compound, μg/kg;
Xρ - the mass concentration of the target compound calculated from the calibration curve, μg/L;
XV - extract concentration volume, ml;
M - solid waste sample mass (wet weight), g.
9.3 The result is shown
9.3.1 Determination of solid waste leachate, when the determination of less than 100 μg/L, to retain the decimal point after a bit; when the determination is greater than or equal to 100
Μg/L, retain three valid digits.
9.3.2 Determination of solid waste, when the determination results less than 100 μg/kg, retained a decimal point after a; when the determination is greater than or equal to 100 μg/kg,
Keep three valid digits.
10 precision and accuracy
10.1 Precision
Six laboratories were tested for the concentration of organophosphorus pesticides at 2.0 μg/kg, 10.0 μg/kg and 25.0 μg/kg of quartz sand (5.10)
To be measured. The relative standard deviations in the laboratory were 0.55% ~ 24%, 0.84% ~ 23% and 1.7% ~ 21%, respectively.
The quasi-deviations range from 9.0% to 15%, 5.0% to 23% and 3.8% to 14%, respectively. The reproducibility limits range from 0.4 μg/kg to 0.7 μg/kg, 2.0
Μg/kg ~ 3.4 μg/kg and 4.6 μg/kg to 7.1 μg/kg respectively. The reproducibility limits ranged from 0.7 μg/kg to 1.0 μg/kg, 2.7 μg/kg to 7.2 μg/kg and
4.9 μg/kg to 13.7 μg/kg.
The standard lead unit was used to determine the solid waste leachate with an organophosphorus pesticide concentration of 0.5 μg/L, 2.0 μg/L and 10.0 μg/L.
The relative standard deviations in the laboratory range from 11% to 18%, 6.8% to 16% and 11% to 16%, respectively.
10.2 Accuracy
Six laboratories were used to measure the ash and sludge solid waste samples. Plus scalar of 10.0 μg/kg, the target compound
The recoveries were 67.3% ~ 93.0%. The final recoveries of the target compounds were 67.3% ± 12% ~ 93.0% ± 25%.
The standard compiling unit was used for the determination of the ash leaching solution by adding the standard scale of 5.0 μg/L and the recoveries of the target compound
To 43.5% to 86.8%.
Refer to Appendix D for details on precision and accuracy.
11 quality assurance and quality control
11.1 Calibration curve
Calibration with a linear fitting curve shall have a correlation coefficient greater than or equal to 0.999, otherwise the calibration curve should be redrawn.
11.2 Calibration Verification
Each batch of samples (up to 20 samples) was calibrated before calibration using the calibration curve at the midpoint of the calibration curve.
Poor should be controlled within 30%, otherwise the calibration curve should be redrawn.
11.3 blank
Each batch of sample (up to 20 samples) should be a laboratory blank and the target compound concentration in the blank result should be less than the method detection limit.
11.4 parallel sample determination
Each batch of samples (up to 20 samples) should be at least one parallel measurement, the parallel sample determination of the relative deviation should be less than 30%.
11.5 Actual sample spikes and spikes are parallel
Each batch of sample (up to 20 samples) should be subjected to at least one actual sample spike and one plus spike. The actual sample spiked recovery rate
Should be between 50% to 140%, plus standard parallel to the determination of the relative deviation of the results should be less than 30%. If the recovery rate does not meet the requirements, and increase
Standard parallel meet the requirements, then the sample exists matrix effect, need to be noted in the results.
12 Waste treatment
All wastes produced in the test shall be managed in accordance with the relevant provisions and shall be properly labeled and entrusted with qualified units for processing.
Appendix A
(Normative appendix)
Method detection limit and lower limit of determination
Schedule A method detection limit and lower limit of determination
Solid waste solid waste leachate
Serial number compound
Detection limit (μg/kg) Lower limit (μg/kg) Detection limit (μg/L) Lower limit (μg/L)
1 propyl bromide 0.8 3.2 0.3 1.2
2 phorate 0.8 3.2 0.2 0.8
3 dimale 1.2 4.8 0.3 1.2
4 Diazine 0.7 2.8 0.2 0.8
5 B-Phorate 1.2 4.8 0.2 0.8
6 different rice blast net 1.2 4.8 0.2 0.8
7 methyl parathion 1.2 4.8 0.3 1.2
8 malathion 0.7 2.8 0.2 0.8
9 chlorpyrifos 0.6 2.4 0.3 1.2
10 parathion 1.1 4.4 0.3 1.2
11 rice abundance 0.7 2.8 0.3 1.2
12 ethionophos 0.8 3.2 0.2 0.8
Appendix B
(Normative appendix)
Sample purification
B.1 Reagents and materials
Unless otherwise stated, analytical reagents that meet the relevant criteria are used during the analysis.
B.1.1 N-Hexane (C6H14). Chromatographic Purification.
B.1.2 Ethyl acetate (CH3COOC2H5). Chromatographic pure.
B.1.3 Dichloromethane (CH2Cl2). Chromatographic purity.
B.1.4 Methanol (CH3OH). Chromatographic Purification.
B.1.5 anhydrous sodium sulfate (Na2SO4). analytical grade, baked at 400 ℃ for 4 h, placed in a dryer to cool to room temperature, transferred to the grinding glass
The bottle is kept in a dryer.
B.1.6 Silicone Adsorbent. 100 mesh to.200 mesh. The silica gel adsorbent was washed with methanol (B.1.4), and after the methanol was completely volatilized,
The spreaders were spread out in the pan and had a thickness of less than 10 mm and activated at 130 ° C for at least 16 h. After the activation of the dryer into the cooling 30 min, into the
Grinding glass bottles, stored in the dryer.
B.1.7 glass column. diameter 20 mm, length 10 cm ~ 20 cm, with PTFE valve, the bottom with a sieve plate.
B.1.8 Quartz glass wool. 400 ℃ baking 1 h.
B.1.9 Solid phase extraction column. 1 g, silica gel packing.
B.2 Purification steps
When the sample needs to be purified, it is recommended to use silica gel chromatography column and silica gel solid phase extraction column two purification methods. You can also use other suitable net
Method.
B.2.1 silica gel column purification
B.2.1.1 Preparation of silica gel column
The quartz glass wool (B.1.8) was filled in the bottom of the glass column (B.1.7), 10 mm thick anhydrous sodium sulfate (B.1.5) was added,
Into the 10 g silica gel adsorbent (B.1.6), tap the column wall, fill the silica gel adsorbent, then add 10 mm thick anhydrous sodium sulfate, and finally
Dichlorometh...
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