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HJ 827-2017: Water quality -- Determination of carbamates pesticides by Ultra performance liquid chromatography–triple quadrupole mass spectrometry
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Water quality -- Determination of carbamates pesticides by Ultra performance liquid chromatography–triple quadrupole mass spectrometry
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HJ 827-2017
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Basic data | Standard ID | HJ 827-2017 (HJ827-2017) | | Description (Translated English) | Water quality -- Determination of carbamates pesticides by Ultra performance liquid chromatography�Ctriple quadrupole mass spectrometry | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Word Count Estimation | 31,369 | | Date of Issue | 4/25/2017 | | Date of Implementation | 6/1/2017 | | Regulation (derived from) | Ministry of Environment Protection Announcement 2017 [16] | | Issuing agency(ies) | Ministry of Ecology and Environment | HJ 827-2017: Water quality -- Determination of carbamates pesticides by Ultra performance liquid chromatography–triple quadrupole mass spectrometry
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Water quality-Determination of carbamates pesticides by Ultra
Performance liquid chromatography-triple quadrupole mass spectrometry
National Environmental Protection Standard of the People 's Republic of China
Determination of water - based urethane - based pesticides
Ultra High Performance Liquid Chromatography - Triple Quadrupole Mass Spectrometry
2017-03-30 released
2017-05-01 Implementation
Ministry of Environmental Protection released
Directory
Foreword
1 Scope of application
2 normative reference documents
3 Principle of the method
4 reagents and materials
5 instruments and equipment
6 samples
7 Analysis steps
8 Calculation and representation of results
9 precision and accuracy
10 quality assurance and quality control
11 Waste treatment ..10
Appendix A (normative) method of detection limit and lower limit of determination
Appendix B (informative) method of precision and accuracy
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 Water Pollution,
Protect the human health, regulate the water carbamate pesticide monitoring methods, the development of this standard.
This standard specifies ultra performance liquid chromatography - triple quadrupole mass spectrometry for the determination of 15 carbamate pesticides in water.
This standard is the first release.
Appendix A of this standard is a normative appendix, Appendix B is an informative appendix.
This standard is formulated by the Environmental Monitoring Division of the Ministry of Environmental Protection and the Standards Division of Science and Technology.
The main drafting unit of this standard. Jiangsu Province Environmental Monitoring Center.
The standard method of verification unit. Zhejiang Zhoushan marine ecological environment monitoring station, Dalian Environmental Monitoring Center, Jinan City Environmental Monitoring
Measuring center station, Zhenjiang City Environmental Monitoring Center Station, Taizhou City Environmental Monitoring Center Station, Shimadzu Enterprise Management (China) Co., Ltd. Shanghai Analysis Center.
The environmental protection department of this standard approved on March 30,.2017.
This standard has been implemented since May 1,.2017.
This standard is explained by the Ministry of Environmental Protection.
Determination of water - based urethane - based pesticides
Ultra High Performance Liquid Chromatography - Triple Quadrupole Mass Spectrometry
Warning. Carbamate pesticides are toxic organic substances, the experimental operation should avoid contact with skin and clothing. Solution preparation and sample preparation
The process should be carried out in a fume hood.
1 Scope of application
This standard specifies ultra performance liquid chromatography - triple quadrupole mass spectrometry for the determination of 15 carbamate pesticides in water.
This standard applies to surface water, groundwater, domestic sewage and industrial wastewater in the end of methomyl, methotrexate, 3-hydroxy carbofuran, residual
Kill Granville, evil worm Granville, Carbaryl, mixed kill Granville, speed off Granville, Zhong Dingwei, Mengxue Granville, chloride kill Granville, grams of Budweiser, isoprene,
Determination of 15 carbamate pesticides in.
When the injection volume is 2.0μl, the detection limit of direct injection is 0.1 ~ 2 μg/L, the lower limit is 0.4 ~ 8 μg/L, see Appendix A.
When the sampling volume is 100 ml, the volume of concentrated volume is 1.0 ml, the injection volume is 2.0 μl, the detection limit of solid phase extraction is 0.002 ~
0.031 μg/L, the lower limit of determination is 0.008 ~ 0.124 μg/L, see Appendix A.
2 normative reference documents
The contents of this standard refer to the terms of the following documents. For undated references, the valid version applies to this standard.
Technical specification for surface water and wastewater monitoring
Technical specification for groundwater environmental monitoring
3 Principle of the method
The carbamate pesticides in water were enriched by direct injection or solid phase extraction using ultra-high performance liquid chromatography-triple quadrupole mass spectrometry
Separation detection. According to the retention time and characteristic ion characterization, the internal standard method is quantified.
4 reagents and materials
Unless otherwise stated, the use of the use of national standards in line with the excellent grade pure reagent, the experimental water for the new preparation of pure water without the target.
4.1 Sulfuric acid. ρ (H2SO4) = 1.84 g/ml.
4.2 Sodium hydroxide (NaOH).
4.3 Formic acid (HCOOH).
4.4 methanol (CH3OH), pesticide residues.
4.5 sulfuric acid solution. 1 1
Measure 50 ml of concentrated sulfuric acid (4.1) and slowly add to 50 ml of water.
4.6 Sodium hydroxide solution. ρ (NaOH) = 0.4 g/ml
Weigh 40 g of sodium hydroxide in water, set to 100 ml.
4.7 Formic acid solution. 1 1000
Remove 1 ml of formic acid (4.3) in 1000 ml of water.
4.8 standard solution
All of the following standard solutions should be returned to room temperature and shaken after use.
4.8.1 Standard solution for carbamate compounds. ρ = 100 μg/ml
Can be purchased commercially available standard solution, the components include methomyl, methomyl voxime, 3-hydroxy carbofuran,
Naphthalene, mixed kill Granville, speed off Granville, Zhong Dingwei, Mengxue Granville, chloride kill Granville, grams of Budweiser, isoprene, pest control, anti-pirimicarb, solvent
Methanol. The stock solution is stored at or below 4 ° C and is protected from light or by reference to the manufacturer's product description.
4.8.2 urethane compounds Standard use of liquid.
The amount of carbamate stock solution (4.8.1) was diluted with methanol (4.4) so that the concentration of methomyl oxime was 20 μg/ml,
The concentration of chlorpyrifos, chlorhexidine, soutalogin and gentaine was 2.0 μg/ml, and the resistance to pirimicarb, carbofuran, isoprene and pest control was
1.0 μg/ml, methotrexate, 3-hydroxy carbofuran, propoxurate, maltose, carbaryl, mixed with a concentration of 4.0 μg/ml (reference concentration).
The use of liquid in the following 4 ℃ cold storage sealed light preservation, shelf life of two months.
4.8.3 Internal standard stock solution. ρ = 100 μg/ml
The internal standard for the carnoside-D7, carbofuran-D3, pest control Viola-D3, methomyl-D3, you can buy commercially available standard solution, solvent
Methanol. 4 ℃ below the cold seal to keep away from light or refer to the manufacturer's product description.
4.8.4 Internal standard liquid.
The amount of internal standard stock solution (4.8.3) was diluted with methanol (4.4), making the concentration of 0.5 μg/ml (reference concentration)
The concentration of Dewei-D3, Carbaryl-D7 and carbofuran-D3 was 2.0 μg/ml (reference concentration). Internal standard use of liquid below 4 ℃ cold storage
Sealed light preservation.
4.9 Nitrogen. Purity ≥ 99.99%.
4.10 filter. material is 0.22 μm Teflon or other equivalent material.
5 instruments and equipment
5.1 Ultra High Performance Liquid Chromatography/Triple Quadrupole Mass Spectrometer with Electrospray Ionization Source (ESI).
5.2 Columns. 1.7 μm ODS C18 with a column length of 50 mm, an internal diameter of 2.1 mm, or other similar performance columns.
5.3 solid phase extraction device. automatic or manual, flow rate can be adjusted.
5.4 Solid phase extraction column. The filler is divinylbenzene and N-vinylpyrrolidone copolymer or equivalent extraction column, the specification is 6 ml/500 mg.
5.5 Concentration device. nitrogen blowing concentrator or other types of equipment equivalent performance.
5.6 Microinjector. 10 μl, 50 μl, 100 μl, 250 μl, 1.0 ml.
5.7 General laboratory equipment and equipment commonly used.
6 samples
6.1 sample collection and preservation
The collection and storage of water samples are carried out in accordance with the relevant provisions of HJ/T 91 and HJ/T 164.
Prepare the water sample with a pre-washed clean and dry mill brown glass bottle (250 ml), and the sample bottle should be completely filled with no air bubbles.
With sulfuric acid solution (4.5) or sodium hydroxide solution (4.6) to adjust its neutral, water samples below 4 ℃ cold storage preservation. Determination of more
Wei and methomyloxime should be completed within 3 days of analysis, determination of other components should be completed within 7 days of analysis.
6.2 Preparation of the sample
6.2.1 Direct injection method
The water samples were returned to room temperature and filtered through a 0.22 μm filter. The 1.0 mL sample was removed and 10.0 μl of the internal standard was added (l 4.8.4)
Mix the test.
6.2.2 solid phase extraction method
The solid phase extraction column (5.4) was activated with 10 ml of methanol (4.4) and 10 ml of water, and the column
Surface does not reveal the surface. A sample of 100 ml of water was taken and passed through a solid phase extraction column at a flow rate of less than 5 ml/min (about 1-2 drops/sec)
The volume of water sample can be appropriately reduced according to the actual situation. And then 10 ml of experimental water leaching column, remove the column to retain the weak impurities,
The column was then dried with nitrogen (4.9). And eluted with 10 ml of methanol (4.4) at a flow rate of about 3 ml/min (about 1 drop/sec)
Of the column, collecting the eluent. The eluate was concentrated (5.5) to near dryness (note that the liquid level was slightly fluctuated) and the conversion solvent was water
And fixed to 1.0 ml, and finally add the internal standard liquid 10.0 μl (4.8.4), after mixing filter (4.10) filter, placed in the vial,
To be tested.
Note. samples containing a large amount of non-volatile salts should be purified by solid phase extraction.
6.3 Preparation of blank sample
The samples were prepared in the same manner as in the sample preparation (6.2.1 or 6.2.2) to prepare a direct injection method.
Phase extraction of blank samples.
7 Analysis steps
7.1 Instrument reference conditions
7.1.1 Ultra High Performance Liquid Chromatograph Reference Conditions
Mobile phase. mobile phase A solution of formic acid 1 1000 (4.7), mobile phase B methanol (4.4), gradient elution program in Table 1.
Flow rate. 0.3 ml/min
Column temperature. 40 ° C
Injection volume. 2.0 μl
Table 1 Liquid Chromatography Mobile Phase Gradient Elution Procedure
7.1.2 Mass spectrometer reference conditions
Positive ion mode, ionization voltage. 5500 V, ion source heating gas temperature. 550 ° C. Detection of multi-ion reaction monitoring
(MRM), the specific conditions shown in Table 2.
Note. For different mass spectrometry equipment, the parameters may be different, before the determination of the mass spectrometry parameters should be optimized to the best.
Table 2 Monitoring conditions for the multi-ion reaction of the target compound
Compound Monitoring Ion Pair (m/z) Dwell Time/ms Cone Voltage/V Collision Voltage/V Quantitative Internal Standard
Note. with * for the quantitative ion pair
7.1.3 Instrument tuning
According to the instrument manual in the specified time and frequency of liquid chromatography/tandem mass spectrometer for the quality of the instrument and the resolution of the school
Positive, where the number of mass deviation of the instrument within ± 0.5Da, the mass spectral peak half width of 0.6Da ~ 0.9Da between to ensure that the instrument in the most
Good test state.
Note. Da, Dalton Dalton's abbreviation, referring to the name of the atomic mass unit.
7.2 Establishment of standard curve
Take a certain amount of carbamate standard use of the liquid (4.8.2), with water prepared at least 5 concentration points of the standard series (reference quality
Concentration in Table 3), respectively, take 1.0mL prepared standard series, add the standard standard use of liquid (4.8.4) 10.0 μl, after mixing
There is a brown sample bottle, to be tested.
From the low concentration to the high concentration, the standard series solution was sequentially injected with the concentration of the target component in the standard series solution and the concentration of the internal standard
Is the abscissa, and the ratio of the corresponding peak area (or peak height) to the peak area (or peak height) of the internal standard is the ordinate,
curve.
Table 3 reference point for the standard curve of carbamate pesticides
7.3 Determination of samples
Take the test sample (6.2) and measure it according to the same instrument analysis conditions as the calibration curve. When the water sample concentration exceeds the standard
The linear range of the curve should be re-sampled and properly diluted and the sample prepared and reconstituted according to (6.2).
7.4 blank test
The measurement of the blank sample (6.3) was carried out under the same conditions as the test sample (7.1).
Note. for the anti-pirimicin, speed off Granville, carbofuran, isopropyl alcohol, chloride kill Granville, Zhong Dingwei, pest control Wei, Meng kill Granville and other target components, according to actual
Increased linear concentration range.
Calculation and representation of results
8.1 Qualitative analysis
The retention time of the target component in the sample was measured in accordance with the parent ion and daughter ion determined in Table 2, and the retention time of the target component in the sample
The absolute value of the relative deviation of the retention time should be less than 2.5%; and the relative abundance of the qualitative daughter ions of each component in the sample to be measured (Ksam,
(1) The relative abundance (Kstd, see formula 2) in the standard solution corresponding to the concentration is compared, and the deviation
In the range of maximum allowable deviation specified in Table 4, it is determined that there is a corresponding analyte in the sample. 15 kinds of carbamates
Drug and four kinds of internal standard total ion current diagram shown in Figure 1.
Where. Ksam - the relative abundance of the qualitative ion in a group of samples,%;
A2 - the peak area (or peak height) of the qualitative daughter ion in the second component of a component in the sample;
A1 - the peak area (or peak height) of the quaternary ion of a component in the sample.
Where. Kstd - the relative abundance of the qualitative daughter ion in a standard sample,%;
Astd2 - the peak area (or peak height) of the qualitative daughter ion of a second component in a standard sample;
Astd1 - the peak area (or peak height) of the quaternary ion of a component in a standard sample.
Table 4 Maximum allowable deviation of relative ion abundance at qualitative confirmation
1. methomyl oxime; 2. methomylide; 3. methomyl-D3; 4. pirimicarb; 5. 3-hydroxy carbofuran; 6. speed off Viagra; 7. Budweiser; 9. grams of Budweiser -D3; 10. evil worms
11. Carbendazim; 12. Carbaryl-D7; 13. Isoprocarb; 14. Mixed kill Granville; 15. Chloride kill Granville; 16. Zhong Dingwei; 17. Pest control Viagra; Insect Wei-D3; 19. fierce kill Granville
Figure 1 15 kinds of carbamate pesticides and four kinds of internal standard total ion chromatogram
8.2 Quantitative analysis
The target compound was qualitatively identified and quantified by the internal standard method according to the peak area of the quantitative ion.
8.3 Calculation of results
The mass concentration of the target in the sample is given by equation (3).
(3)
Where. ρ - mass concentration of the target in the sample, μg/L;
Ρ1 - the concentration of the target in the sample from the standard curve, μg/L;
V1 - the volume of the sample, mL;
V - water sample volume, mL;
F - dilution factor.
8.4 The result is shown
8.4.1 Direct injection method
When the determination is greater than or equal to 100 μg/L, the data retain the three significant digits; when the result is less than 100 μg/L,
The remainder of the target data is reserved for one decimal place.
8.4.2 Solid phase extraction
When the result is greater than or equal to 1 μg/L, the data retains three significant digits; when the result is less than 1 μg/L, it remains three digits after the decimal point.
9 precision and accuracy
9.1 precision
9.1.1 Direct injection method
6 laboratories were tested for carbamate-containing pesticides with a concentration of 2.00 μg/L, 20.0 μg/L, 80.0 μg/L
A blank spiked sample was subjected to six replicates.
The relative standard deviations in the laboratory were 1.5% ~ 12%, 0.4% ~ 9.2%, 1.2% ~ 9.6%, respectively. The relative standard between laboratories
The reproducibility limits were. 0.1 ~ 2 μg/L, 0.6 ~ 17 μg/L, and the range of reproducibility was 3.5% ~ 12%, 2.9% ~ 13%
2.1 ~ 52 μg/L, and the reproducibility range was 0.1 ~ 3 μg/L, 0.7 ~ 22 μg/L and 2.4 ~ 64 μg/L.
Six laboratories tested the actual sample of carbamate-containing pesticides with a concentration of 5.00 μg/L and 80.0 μg/L (in carnaquose)
The samples were subjected to six repeated determinations.
The relative standard deviations in the laboratory were 0.7% ~ 15.8% and 0.5% ~ 17.7%, respectively. The relative standard deviations were.
2.2% ~ 13.2%, 1.7% ~ 24.7%. The reproducibility limit was. 0.1 ~ 5 μg/L, 1.9 ~ 74 μg/L; the reproducibility limit was 0.2 ~
6 μg/L, 3.5 to 94 μg/L.
9.1.2 Solid phase extraction
The concentration of carbamate-containing pesticides in the six laboratories was 0.040 μg/L, 0.200 μg/L, 0.800 μg/L,
Of the unified blank spiked water samples were carried out 6 times repeated determination.
The relative standard deviations in the laboratory were 2.5% ~ 15%, 3.3% ~ 13%, 1.8% ~ 10%, respectively. The relative standard deviation between the laboratory
The difference was as follows. 3.1% ~ 15%, 3.9% ~ 15%, 3.1 ~ 14%, repeatability range. 0.002 ~ 0.037 μg/L, 0.009 ~ 0.139
Μg/L, 0.025 ~ 0.675 μg/L, and the reproducibility range was 0.002 ~ 0.037 μg/L, 0.016 ~ 0.154 μg/L, 0.032 ~ 0.703 μg/L.
6 laboratories for the actual concentration of 0.100 μg/L carbamate pesticide concentration of 0.800 μg/L (in methylene chloride)
Standard samples were subjected to six replicates.
The relative standard deviations in the laboratory were 1.4% ~ 24.5% and 1.3% ~ 12.6%, respectively. The relative standard deviations between the laboratory were.
3.0% ~ 20.4%, 2.6% ~ 18.0%, the repeatability limit was 0.004 ~ 0.092 μg/L, 0.023 ~ 0.630 μg/L; reproducibility limit
The range is 0.005 ~ 0.140 μg/L, 0.027 ~ 1.00 μg/L.
9.2 Accuracy
9.2.1 Direct injection method
Six laboratories conducted a uniform sample of carbamate-containing pesticide concentrations of 5.00 μg/L and 80.0 μg/L
The recoveries were as follows. 76.5% ~ 111%, 78.7% ~ 120%.
9.2.2 Solid phase extraction
Six laboratories conducted a uniform sample of carbamate-containing pesticide concentrations of 0.100 μg/L and 0.800 μg/L (in methylene chloride)
The recoveries were as follows. 72.1% ~ 112%, 74.5% ~ 121%.
The specific precision and accuracy of the results are given in Appendix B.
10 quality assurance and quality control
10.1 blank analysis
Each laboratory at least do a laboratory blank, laboratory blanks detected in each target compound concentration should not exceed the method of inspection
Limit.
10.2 Calibration
Each batch should be drawn with a standard curve, the correlation coefficient should be ≥ 0.995, otherwise the standard curve should be redrawn.
A standard curve of intermediate standard points should be measured for every 20 samples or each batch (less than 20 samples).
The relative deviation between the result and the concentration should be ≤ 20%, otherwise the standard curve should be redrawn.
10.3 parallel sample determination
Each pair of 20 samples or batches (less than 20 samples/batch) need to be a parallel double sample, the parallel two-way determination of the relative deviation
Poor ≤ 20%.
Determination of the recoveries of spiked samples
Each of the 20 samples or each batch (less than 20 samples/batch) need to do a matrix plus standard sample, plus standard sample with the original sample in the complete phase
With the same test conditions for analysis. The recovery rate of the standard method should be between 70% and 115%, and the solid phase extraction method
Rate should be between 60% and 120%.
11 Waste treatment
Waste and waste generated during the course of the experiment shall be collected and kept and commissioned by qualified units for processing.
Appendix A
(Normative appendix)
Method of detection limit and determination of the lower limit
Table A.1 gives the detection limits and the lower limit of the target compound in this method. The solid phase extraction method is shown in 100 ml water samples.
Table A.1 Method of detection limit and lower limit of determination
Appendix B
(Informative)
Method of precision and accuracy
Table B.1 shows the precision and reproducibility of the direct injection method when the blank water sample is measured.
Table B.1 Blank water samples plus standard determination of precision summary table (direct injection method)
Table B.6 shows the accuracy criteria for the solid phase extraction method.
Table B.6 Summary of Accuracy (Solid Phase Extraction)
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