|
US$259.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email.
HJ 851-2017: Water quality - Determination of methomyl and methomyl-oxime - High performance liquid chromatography
Status: Valid
| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivered in | Standard Title (Description) | Status | PDF |
| HJ 851-2017 | English | 259 |
Add to Cart
|
3 days [Need to translate]
|
Water quality - Determination of methomyl and methomyl-oxime - High performance liquid chromatography
| Valid |
HJ 851-2017
|
PDF similar to HJ 851-2017
Basic data | Standard ID | HJ 851-2017 (HJ851-2017) | | Description (Translated English) | Water quality - Determination of methomyl and methomyl-oxime - High performance liquid chromatography | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Word Count Estimation | 11,182 | | Date of Issue | 2017-08-28 | | Date of Implementation | 2017-11-01 | | Regulation (derived from) | MEP Notice No. 41 | | Issuing agency(ies) | Ministry of Ecology and Environment | HJ 851-2017: Water quality - Determination of methomyl and methomyl-oxime - High performance liquid 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.
(Determination of water quality methicillin and methomyloxime by liquid chromatography)
National Environmental Protection Standard of the People 's Republic of China
Determination of water quality of methomyl and methomyl
Liquid chromatography
Water quality - Determination of methomyl and methomyl-oxime
- High performance liquid chromatography
2017-08-28 released
2017-11-01 implementation
Issued by the Ministry of Environmental Protection
i directory
Preface .ii
1 Scope of application 1
2 normative reference document 1
Principle of the method 1
4 interference and elimination
5 reagents and materials
6 instruments and equipment
7 samples
8 Analysis Step 2
Results and Representation 3
10 precision and accuracy
11 Quality assurance and quality control
12 Waste treatment
Appendix A (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,
The protection of human health, regulate the water Dudu Wei and methomyl oxime determination method, the development of this standard.
This standard specifies the determination of methotrexate and methotrexate in water by liquid chromatography.
This standard is the first release.
Appendix A to this standard is an informative appendix.
This standard is organized by the Environmental Monitoring Department of the Ministry of Environmental Protection and the Department of Science and Technology Standards.
The main drafting unit of this standard. Qingdao Environmental Monitoring Center Station and Qingdao University of Technology.
The main verification unit of this standard. Ministry of Agriculture, agricultural quality and safety supervision and inspection test center (Qingdao), Shandong Province Environmental Supervision
Measuring center station, Jinan City Environmental Monitoring Center Station, Tai'an City Environmental Protection Monitoring Station, Liaoning North Environmental Testing Technology Co., Ltd.
Division and Qingdao in a monitoring Limited.
The environmental protection department of this standard approved on August 28,.2017.
This standard has been implemented since November 1,.2017.
This standard is explained by the Ministry of Environmental Protection.
Determination of water quality of methomyl and methotrexate by liquid chromatography
Warning. methomyl and methomyloxime has some toxicity, the standard solution should be prepared in the operation of the fume hood, the operation should be in accordance with regulations
It is required to wear protective equipment to avoid contact with skin and clothing.
1 Scope of application
This standard specifies the determination of methotrexate and methotrexate in water by liquid chromatography.
This standard applies to the determination of methomyl and methotrexate in surface water, groundwater, domestic sewage and industrial waste water.
When the injection volume was 50 μl, the detection limit of methomyl and methomyloxime was 1 μg/L, and the lower limit of determination was 4 μg/L.
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 surface water and wastewater monitoring
Technical specification for groundwater environmental monitoring
3 Principle of the method
The methotrexate and methotrexate in water were injected directly by liquid chromatography with an ultraviolet detector. According to the reservation
Qualitative and external standard method.
4 interference and elimination
When the organic matter coexisting in the water sample interferes with the determination of the target compound can be determined by changing the chromatographic conditions, so that methomyl and methomyl
Separate from the disturbance, or remove the water sample with n-hexane extraction to remove part of the interference, take the water phase for analysis.
5 reagents and materials
Unless otherwise stated, analytical analytical reagents conforming to national standards are used in the analysis. The test water is pure water containing no organic matter.
5.1 Hydrochloric acid. ρ (HCl) = 1.18 g/ml.
5.2 hydrochloric acid solution. c (HCl) = 0.1 mol/L.
Accurately remove 3.1 ml of hydrochloric acid (5.1) in a small amount of water and dilute to 1 L.
5.3 sodium hydroxide (NaOH). excellent grade pure.
5.4 Sodium hydroxide solution. c (NaOH) = 0.1 mol/L.
Accurately weighed 4.0 g of sodium hydroxide dissolved in a small amount of water, diluted to 1 L.
5.5 Acetonitrile (CH3CN). Liquid Chromatography Pure.
5.6 methomyl. purity ≥ 98%.
5.7 methomyloxime. purity ≥ 98%.
5.8 methomyl and methomyloxime mixed standard stock solution. ρ = 100 μg/ml.
Were weighed 0.010 g (exact to 0.1 mg) methotrexate (5.6) and methotrexate (5.7), dissolved in acetonitrile (5.5)
To 100 ml, frozen at 4 ℃, protected from light, can be stored for 12 months, or directly to buy a certified standard solution.
5.9 Methomyl and methomyloxime mixed standard liquid. ρ = 10.0 μg/ml.
2 Accurately remove 1.00 ml of methomyl and methotrexate standard stock solution (5.8) and dilute to 10 ml with water.
6 instruments and equipment
6.1 Sampling vials. 100 ml brown glass jar with a mouth plug.
6.2 Liquid Chromatograph. with UV detector or diode array detector.
6.3 Columns. 5 μm ODS with a column length of 25 cm, an internal diameter of 4.6 mm, or other equivalent columns.
6.4 Micro Samplers. 10 μl, 50 μl and 100 μl.
6.5 Filtration. 0.22 μm Teflon or nylon microporous membrane.
6.6 Common laboratory equipment and equipment.
7 samples
7.1 Sample collection and storage
Samples were collected according to the relevant regulations of HJ/T 91 and HJ/T 164. After sample collection, use hydrochloric acid solution (5.2) or sodium hydroxide solution
(5.4) adjusted to pH 4 ~ 6, protected from light, within 8 d analysis is completed.
7.2 Sample preparation
The water sample was filtered through a 0.22 μm filter (6.5) and placed in a 2 ml vial and tested.
Note. For samples containing organic matter, take 10 ml of water samples, with 2 ml of n-hexane extraction, take the water phase for determination.
7.3 Preparation of blank samples
The sample was prepared in the same manner as in Sample Preparation Step (7.2).
8 Analysis steps
8.1 Chromatographic reference conditions
Mobile phase B. water flow rate. 1.0 ml/min; column temperature. 30 ℃; detection wavelength. 232 nm; injection volume.
50 μl. The elution procedure is shown in Table 1.
Table 1 elution program
Time (min) A (%) B (%)
Note. After elution time of 6 min for cleaning the column, the cleaning time can be adjusted according to the complexity of the actual sample.
8.2 Calibration curve establishment
3 to take appropriate amount of methomyl and methomyloxime mixed standard use of liquid (5.9), diluted with experimental water to prepare at least 5 concentration points
Of the standard series, the concentration of methomyl and methomyloxime were 5.0, 50.0, 100, 500 and 1000 μg/L, respectively
degree). From the low concentration to high concentration in turn to the standard series of samples into the standard series of solutions of the target compound concentration for the abscissa,
Corresponding to the peak height or peak area for the vertical axis, the establishment of calibration curve.
8.3 Determination
The sample to be tested (7.2) was subjected to the same conditions as the calibration curve.
8.4 blank test
The blank sample to be measured (7.3) was measured under the same conditions as the sample.
9 Results calculation and representation
9.1 Qualitative analysis
According to the retention time of the target compound in the sample and the target compound in the standard series. If necessary, the use of standard samples Tim
Addition, different wavelength absorption ratio or scanning ultraviolet absorption spectroscopy and other methods to assist the qualitative.
The standard chromatograms of methomyl and methomyl oxime are shown in Fig. 1 under the chromatographic reference conditions (8.1) specified in this standard.
1-methomyl oxime; 2-methomyl.
Figure 1 Standardized chromatogram of methomyl and methotrexate
9.2 Quantitative analysis
The mass concentration of the target compound in the water sample is calculated according to the following formula.
aA (1)
Where. - mass concentration of the target compound in the water sample, μg/L;
A - the peak area or peak height of the target compound;
a - the intercept of the calibration curve;
b - the slope of the calibration curve;
f - the dilution factor of the water sample.
9.3 The result is shown
When the determination is greater than or equal to 100 μg/L, the data retain the three significant digits; when the determination is less than 100 μg/L, the retention
4 to integer bits.
10 precision and accuracy
10.1 precision
6 laboratories were charged with blank water, surface water and domestic sewage with a concentration of 10.0 μg/L, 100 μg/L, 800
μg/L samples were subjected to six repeated determinations. the relative standard deviations in the laboratory were. 0.8% ~ 7.3%, 0.3% ~
4.3%, 0.1% ~ 2.9%, respectively. The relative standard deviations were 6.0% ~ 9.1%, 4.3% ~ 6.5%, 7.8% ~ 8.2%, respectively
The reproducibility limit r is. 2 ~ 3 μg/L, 13 ~ 19 μg/L, 176 ~ 184, and the reproducibility limit r is. 1 μg/L, 6 ~ 7 μg/L, 18 ~ 36 μg/L
μg/L; the relative standard deviations in the laboratory were. 1.4% ~ 12%, 0.4% ~ 5.0%, 0.1% ~ 1.9%; laboratory
The relative standard deviations were. 3.0% ~ 9.9%, 4.2% ~ 6.7%, 6.2% ~ 7.9%, the repeatability r was 1 ~ 2 μg/L, 6 ~ 8
μg/L, 16 ~ 24 μg/L; reproducibility R. 2 ~ 3 μg/L, 13 ~ 20 μg/L, 141 ~ 181 μg/L.
The concentration of methicillin was 125 μg/L, 296 μg/L, 741 μg/L and the concentration of methomyloxoxom was 106 μg/L,
μg/L, 249 μg/L of industrial wastewater samples were subjected to six repeated determinations. the relative standard deviations in the laboratory were.
1.3% ~ 8.4%, 0.1% ~ 4.2%, 0.2% ~ 2.8%; the relative standard deviation between the laboratory were. 10%, 3.4%, 6.1%
L = 37 μg/L, 32 μg/L, 130 μg/L, and the expression of rituximab in the range of 15 μg/L, 15 μg/L, 29 μg/L,
The relative standard deviations in the laboratory were 0.6% ~ 11%, 0.3% ~ 3.6%, 0.5% ~ 8.3%, respectively. The relative standard deviation
The reproducibility limit r was. 28 μg/L, 10 μg/L, 29 μg/L,
44 μg/L, 71 μg/L.
10.2 Accuracy
6 laboratories were charged with blank water, surface water and domestic sewage with a concentration of 10.0 μg/L, 100 μg/L, 800
μg/L samples were analyzed and determined. the recoveries of methomyl were. 82.0% ~ 113%, 91.4% ~ 112%, 84.1% ~
The recoveries were 99.3% ± 18.0% ~ 102% ± 17.0%, 98.7% ± 8.4% ~ 101% ± 12.0%
98.6% ± 14.4% ~ 99.1% ± 16.2%. The recoveries of Madduoxime were 82.5% ~ 115%, 93.2% ~ 113%, 90.4%
~ 100% ± 19.8% ~ 106% ± 6.6%, 99.0% ± 10.6% ~ 101% ± 8.2%, and the recoveries were 100%
100% ± 13.2% ~ 101% ± 16.4%.
The concentration of methomyladol was 21 μg/L,.199 μg/L, 646 μg/L and the concentration of methomyloxoxom was 6 μg/L, 43 μg/L,
142 μg/L of industrial wastewater samples were labeled with methomyl and methotrexate 100 μg/L were measured by spiked determination.
The recoveries were 94.3% ~ 112%, 80.6% ~ 106% and 84.2 ~ 117%, respectively. The final recoveries were. 102% ± 14.4%
95.9% ± 18.2%, 95.3% ± 22.4%, respectively. The recoveries of spiradoxime were 93.3% ~ 109%, 92.7% ~ 115%, 92.8% ~
The final recoveries were 101% ± 13.0%, 104% ± 18.0% and 100% ± 13.6% respectively.
Details of precision and accuracy are given in Appendix A.
11 quality assurance and quality control
11.1 blank test
Every 20 samples or per batch (less than 20 samples) should be at least one lab blank, blank in the end of methomyl and methomyl
Of the concentration should be lower than the method detection limit.
11.2 Initial calibration
The correlation coefficient of the calibration curve is ≥0.995.
11.3 Standard curve verification
5 per 20 samples or per batch (less than 20 samples) should be measured with a calibration curve in the middle of the standard solution, the results
And the relative deviation of the concentration of the curve should be ≤ 15%. Otherwise, a new calibration curve should be established.
11.4 parallel samples
Every 10 samples or each batch (less than 10 samples) should be a parallel sample, parallel to the relative deviation of ≤ 15%.
11.5 matrix spikes
Every 20 samples or each batch (less than 20 samples) should be a matrix plus standard sample, the matrix spike recovery rate should be controlled at 80% ~
Within 120% of the range.
12 Waste treatment
The organic waste generated in the experiment should be collected and kept collectively and entrusted with qualified units for processing.
6 Appendix A
(Informative)
Method of precision and accuracy
Tables A.1 and A.2 give the precision and accuracy of the method, respectively.
Table A.1 The precision of the method
Sample type compound
average value
(Μg/L)
Relative standards in the laboratory
deviation(%)
Inter-laboratory relative
standard deviation(%)
Repetitive limit r
(Μg/L)
Reproducibility R
(Μg/L)
Blank water
Methomyl
10 1.1 to 5.0 8.3 1 3
99 1.0 to 3.6 4.3 6 13
793 0.2 to 1.2 8.2 18 182
Methomyl oxime
10 1.9 to 4.2 8.7 1 3
99 1.1 to 4.1 5.4 8 17
801 0.3 to 1.7 6.7 24 153
Surface water
Methomyl
10 0.8 to 7.3 9.1 1 3
100 0.6 to 3.8 6.5 6 19
791 0.1 to 2.9 7.8 36 176
Methomyl oxime
11 2.2 ~ 12 3.0 2 2
101 0.8 to 3.9 4.2 6 13
813 0.1 to 1.3 6.2 16 141
life
Sewage
Methomyl
10 1.0 to 7.1 6.0 1 2
101 0.3 to 4.3 6.1 7 18
794 0.4 ~ 2.2 8.2 28 184
Methomyl oxime
10 1.4 to 4.1 9.9 1 3
100 0.4 ~ 5.0 6.7 8 20
806 0.1 to 1.9 7.9 22 181
industry
Waste water
Methomyl
125 1.3 to 8.4 10 15 37
296 0.1 to 4.2 3.4 15 32
741 0.2 to 2.8 6.1 29 130
Methomyl oxime
106 0.6 ~ 11 7.9 16 28
145 0.3 to 3.6 10.6 10 44
249 0.5 to 8.3 9.4 29 71
7 Table A.2 Method of accuracy
Sample type compound
Sample concentration
(Μg/L)
Spiked concentration
(Μg/L)
Spiked recovery rate
range(%)
The final value of the recoveries
2 ±
S (%)
Blank water
Methomyl
0 10.0 90.4 ~ 113 102 ± 17.0
0 100 96.8 to 104 98.7 ± 8.4
0 800 91.2 ~ 114 99.0 ± 16.2
Methomyl oxime
0 10.0 89.6 ~ 115 103 ± 18.0
0 100 93.2 to 106 99.0 ± 10.6
0 800 92.4 ~ 112 100 ± 13.2
Surface water
Methomyl
0 10.0 82.0 ~ 107 99.3 ± 18.0
0 100 91.4 to 110 99.7 ± 13.0
0 800 88.7 to 110 98.6 ± 14.4
Methomyl oxime
0 10.0 102 to 112 106 ± 6.6
0 100 97.1 to 107 101 ± 8.2
0 800 96.3 ~ 111 101 ± 10.8
life
Sewage
Methomyl
0 10.0 93.7 to 110 101 ± 12.4
0 100 96.7 to 112 101 ± 12.0
0 800 84.1 to 108 99.1 ± 16.2
Methomyl oxime
0 10.0 82.5 ~ 111 100 ± 19.8
0 100 94.2 to 113 100 ± 13.4
0 800 90.4 to 114 101 ± 16.4
industry
Waste water
Methomyl
21 100 94.3 ~ 112 102 ± 14.4
199 100 80.6 ~ 106 95.9 ± 18.2
646 100 84.2 ~ 117 95.3 ± 22.4
Methomyl oxime
6 100 93.3 ~ 109 101 ± 13.0
43 100 92.7 ~ 115 104 ± 18.0
142 100 92.8 ~ 111 100 ± 13.6
Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of HJ 851-2017_English be delivered?Answer: Upon your order, we will start to translate HJ 851-2017_English as soon as possible, and keep you informed of the progress. The lead time is typically 1 ~ 3 working days. The lengthier the document the longer the lead time. Question 2: Can I share the purchased PDF of HJ 851-2017_English with my colleagues?Answer: Yes. The purchased PDF of HJ 851-2017_English will be deemed to be sold to your employer/organization who actually pays for it, including your colleagues and your employer's intranet. Question 3: Does the price include tax/VAT?Answer: Yes. Our tax invoice, downloaded/delivered in 9 seconds, includes all tax/VAT and complies with 100+ countries' tax regulations (tax exempted in 100+ countries) -- See Avoidance of Double Taxation Agreements (DTAs): List of DTAs signed between Singapore and 100+ countriesQuestion 4: Do you accept my currency other than USD?Answer: Yes. If you need your currency to be printed on the invoice, please write an email to [email protected]. In 2 working-hours, we will create a special link for you to pay in any currencies. Otherwise, follow the normal steps: Add to Cart -- Checkout -- Select your currency to pay.
|