Home Cart Quotation About-Us
www.ChineseStandard.net
SEARCH

HJ 768-2015 English PDF

US$399.00 · In stock
Delivery: <= 4 days. True-PDF full-copy in English will be manually translated and delivered via email.
HJ 768-2015: Solid waste. Determination of organic phosphorous pesticides. Gas chromatography
Status: Valid
Standard IDUSDBUY PDFLead-DaysStandard Title (Description)Status
HJ 768-2015399 Add to Cart 4 days Solid waste. Determination of organic phosphorous pesticides. Gas chromatography Valid

Similar standards

HJ 511   HJ 945.3   HJ 943   

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: 17,185
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.

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

(N......
Image     

Tips & Frequently Asked Questions:

Question 1: How long will the true-PDF of HJ 768-2015_English be delivered?

Answer: Upon your order, we will start to translate HJ 768-2015_English as soon as possible, and keep you informed of the progress. The lead time is typically 2 ~ 4 working days. The lengthier the document the longer the lead time.

Question 2: Can I share the purchased PDF of HJ 768-2015_English with my colleagues?

Answer: Yes. The purchased PDF of HJ 768-2015_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+ countries

Question 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 Sales@ChineseStandard.net. 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.