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HJ 713-2014 English PDF

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HJ 713-2014: Solid wastes. Determination of volatile halohydrocarbons. Purge and trap gas chromatography mass spectrometry
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HJ 713-2014English659 Add to Cart 5 days [Need to translate] Solid wastes. Determination of volatile halohydrocarbons. Purge and trap gas chromatography mass spectrometry Valid HJ 713-2014

Standard similar to HJ 713-2014

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Basic data

Standard ID HJ 713-2014 (HJ713-2014)
Description (Translated English) Solid wastes. Determination of volatile halohydrocarbons. Purge and trap gas chromatography mass spectrometry
Sector / Industry Environmental Protection Industry Standard
Word Count Estimation 25,239
Date of Issue 11/27/2014
Date of Implementation 1/1/2015
Regulation (derived from) Ministry of Environmental Protection Notice 2014 No. 77
Issuing agency(ies) Ministry of Ecology and Environment

HJ 713-2014: Solid wastes. Determination of volatile halohydrocarbons. Purge and trap gas chromatography mass spectrometry


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Solid wastes.Determination of volatile halohydrocarbons.Purge and trap gas chromatography mass spectrometry People's Republic of China National Environmental Protection Standards Solid waste - Determination of volatile halogenated Purge and Trap - gas Chromatography/Mass Spectrometry Solid wastes-Determination of volatile halohydrocarbons- Purge and trap gas chromatography mass spectrometry (release draft) Issued on.2014-11-27 2015-01-01 implementation Issued by the Ministry of Environmental Protection i Table of Contents Preface .ii 1. Scope .1 2 Normative references .1 3 .1 The principle of the method 4 Reagents and materials 1 5. Apparatus 2 6 Sample 2 7 Procedure .3 8 Results Calculation and representation .6 9 precision and accuracy .8 10 Quality assurance and quality control ..8 11 waste treatment .9 12 Considerations .9 Appendix A (normative) object detection limit and lower limit of determination 10 Determination of Annex B (informative) object reference parameters ..12 Precision and accuracy ..14 Annex C (informative) Method

Foreword

To implement the "People's Republic of China Environmental Protection Law" and "People's Republic of China Solid Waste Pollution Prevention Law" Protecting the environment, safeguarding human health, specifications determination of volatile halogenated solid waste, the development of this standard. This standard specifies the determination of solid waste chloride and other 35 kinds of volatile halogenated Purge and Trap - gas Chromatography/Mass Spectrometry. This standard is the first release. Appendix A of this standard is a normative appendix, Appendix B and Appendix C are informative appendices. This standard is developed by the Ministry of Environmental Protection Science, Technology organization. This standard drafting of the main unit. Harbin Municipal Environmental Monitoring Center. The standard verification unit. Heilongjiang Provincial Environmental Monitoring Center, Dalian Municipal Environmental Monitoring Center, Changchun Municipal Environmental Monitoring Heart Station, Anshan Municipal Environmental Monitoring Center Station, Qiqihar Municipal Environmental Monitoring Center Station and the Daqing Municipal Environmental Monitoring Center. This standard MEP November 27, 2014 for approval. This standard since January 1, 2015 implementation. The standard explanation by the Ministry of Environmental Protection. 1 Determination of volatile halogenated solid waste Purge and Trap - gas Chromatography/Mass Spectrometry WARNING. The internal standard used in the experiments, the alternatives and the standard solution are volatile, toxic chemicals, preparation process It should be performed in a hood; the preparation of the sample should be considered whether it is hazardous solid wastes; according to the provisions of Seeking to wear protective equipment to avoid contact with skin and clothing.

1 Scope

This standard specifies the determination of volatile halogenated solid waste purge and trap/gas chromatography - mass spectrometry. This standard applies to the determination of solid waste and solid waste leaching solution of chloride and other 35 kinds of volatile halogenated hydrocarbons. Other play If validated onset halogenated also apply to this standard. The solid waste sample amount of 5 g, 35 kinds of volatile halogenated hydrocarbons detection limit of 0.2 ~ 0.4 μg/kg, detection limit Of 0.8 ~ 1.6 μg/kg. The solid waste leachate volume of 5.0 ml, the detection limit was 0.2 ~ 0.4 μg/L, measured at Limit of 0.8 ~ 1.6 μg/L. See Appendix A.

2 Normative references

The standard content of the following documents cited in the articles. For undated references, the effective version applies to this standard. HJ/T 20 industrial solid waste sampling sample preparation Technical Specifications HJ/T 299 methods for leaching toxicity of solid waste sulfuric acid nitric acid method HJ/T 300 solid waste leaching toxicity Acetic acid buffer solution method

3 PRINCIPLE OF THE METHOD

Samples of volatile halogenated hydrocarbons purged with helium, adsorption trap tube, the collection tube and heated with helium blowback Trap tube volatile halogenated hydrocarbons are thermally desorbed component after entering gas chromatography with mass spectrometer detection. root According to the retention time, the fragment ions of different mass to charge ratio and ion abundance ratio qualitative and quantitative internal standard.

4 Reagents and materials

4.1 experimental water. secondary distilled water or pure water preparation equipment. Before using the subject blank check to confirm no object or Target concentrations below detection limit. 4.2 methanol (CH3OH). pesticide grade, before use by testing to confirm no goal or target concentration is below the detection method limit. 4.3 standard stock solution. ρ = 2000 mg/L. Direct purchase a commercially available certified reference solution below -10 ℃ from light, or by reference to the manufacturer's product description. Should be used Returned to room temperature and shake well. 4.4 standard solution. ρ = 2.5 mg/L. Take the right amount of stock standard solution (4.3), appropriately diluted with methanol (4.2). 24.5 internal standard stock solution. ρ = 2000 mg/L. Selection fluorobenzene, 1-chloro-2-bromo-propane, 4-bromo-fluorobenzene as an internal standard. Direct purchase of certified reference solution, also available standard Quality preparation. 4.6 internal standard solution. ρ = 2.5 mg/L. Proper amount of internal standard stock solution (4.5), with methanol (4.2) appropriately diluted. 4.7 alternatives stock solution. ρ = 2000 mg/L. Selection dichloromethane -d2,1,2- -d4 dichlorobenzene as an alternative. Direct purchase of certified reference solution, also available standard Quality preparation. 4.8 was used as substitutes. ρ = 2.5 mg/L. Take appropriate alternatives stock solution (4.7), appropriately diluted with methanol (4.2). 4.9 4-bromo-fluorobenzene (BFB) solution. ρ = 25 mg/L, can be purchased directly certified standard solution can also be used for preparing reference material, Diluted with methanol. 4.10 quartz sand. 20 to 50 mesh. Before use by testing, confirming that no target or targets below the detection limit. 4.11 Helium. purity ≥99.999%, by deoxidizer oxygen, molecular sieve dehydration. 5. Apparatus 5.1 Sampling equipment. shovels and stainless steel spatula. 5.2 Sampling bottle. PTFE silicone liner screw cap 60 ml wide-mouth glass jar. 5.3 Vial. Teflon liner with screw cap 40 ml brown glass bottles and colorless. 5.4 Gas chromatography - mass spectrometry. EI ionization source. 5.5 Column. capillary column, length 30 m, an inner diameter of 0.25 mm, a thickness of 1.4 μm, 6% stationary phase phenyl nitrilpropionamide/94 % Dimethyl polysiloxane may be used other equivalent capillary column. 5.6 Purge and Trap Device. for the determination of solid samples and viscous liquid samples. Trap tube using 1/3Tenax, 1/3 silica gel, 1/3 mixing activated carbon adsorbents or other equivalent adsorbent. 5.7 micro syringe. 10 μl, 25 μl, 100 μl, 250 μl, 500 μl and 1000 μl. 5.8 Balance. accuracy of 0.01 g. 5.9 Reciprocating oscillator. oscillation frequency of 150 times/min, the vial can be fixed. 5.10 dense brown bottle. 2 ml, with teflon liner. 5.11 pH meter. accuracy of ± 0.05. 5.12 Portable freezer. volume 20 L, the temperature below 4 ℃. 5.13 disposable glass Pasteur pipette. 5.14 General common laboratory instruments and equipment.

6 samples

Samples collected 6.1 According to HJ/T relevant requirements of solid waste collected 20 samples. The use of sampling in the field for the determination of volatile halogenated hydrocarbons Portable VOC analyzer samples the concentration level of screening. Low concentration samples shall be collected at least three parallel samples. sampling Put in a magnetic former vial (5.3) in a stirring seal, weigh (to the nearest 0.01 g). Sampling equipment used to collect approximately 5 g 3 to sample vial, the vial quickly removed the thread and the outer surface of the adhesion of the sample vial sealed immediately. Further collection Determination of high content of a sample of solid waste leachate samples and the samples used in the sampling bottle (5.2). Placed after sample collection Portable freezer (5.12) in the back to the lab. Note 1. On-site preliminary screening of volatile halogenated hydrocarbons assay results greater than 200 μg/kg, the sample depending on the content of the sample is high. Note 2. Do not stir the sample collection of solid waste, solid waste in order to avoid volatile organic compounds. Sampling personnel must do protection work. Save 6.2 sample After the sample arrives at the lab should be analyzed as soon as possible. If not timely analysis of samples should be lower than 4 ℃ preservation, preservation of To 14 d. Sample storage area should be free of organic matter interference. 6.3 Preparation of the sample 6.3.1 Solid Waste low content in the sample After removing the vial (5.3), to be returned to room temperature, weighed (accurate to 0.01 g). Test water was added 5.0 ml (4.1), 10 μl substitute (4.8) and 10 μl internal standard (4.6), to be tested. 6.3.2 Solid Waste high content in the sample After removing the sample bottle (5.2), to be returned to room temperature, 5 g sample is weighed into a vial (5.3), and added rapidly 10.0 ml methanol (4.2), sealed, reciprocating shaker (5.9) on to 150 times/min frequency oscillation 10 min. Allowed to settle After using a disposable glass Pasteur pipette (5.13) Pipette approximately 1 ml to 2 ml extract dense brown bottle (5.10), and When necessary, the extract may be centrifuged. The extract can be placed in the freezer at 4 ℃ preservation, storage period of 14 d. After the extract was analyzed before returned to room temperature, the vial (5.3) was added 5 g of quartz sand (4.10), 5.0 ml solid Test water (4.1), 10 ~ 100 μl of methanol extract, 10 μl substitute (4.8) and 10 μl internal standard (4.6), immediately close Seal, tested. NOTE 3. If the methanol extract higher target concentration may be appropriately diluted by the addition of methanol. Note 4. If the method of analysis with high levels of concentration is too low or not detected, with a low content of the sample re-analysis method. 6.3.3 Solid waste leachate sample Executive HJ/T 299 or HJ/T 300 methods of preparing solid waste leachate samples. Take 5.0 ml leaching solution transferred to vials (5.3), add 10 μl substitute (4.8) and 10 μl internal standard (4.6), immediately sealed and tested. 6.4 Preparation of blank samples 6.4.1 Solid Waste low content of a blank sample To 5 g of quartz sand (4.10) instead of the sample according to 6.3.1 step of preparing a low content of a blank sample. 6.4.2 Solid Waste high content of a blank sample To 5 g of quartz sand (4.10) instead of the sample according to 6.3.2 step of preparing a high content of a blank sample. 6.4.2 Solid waste leachate blank sample According to HJ/T 299 or HJ/T 300 extraction method, quartz sand (4.10) instead of the sample, prepared according to step 6.3.3 Solid waste leachate blank sample.

7 Procedure

Different types of purge and trap apparatus, gas chromatography - the best working conditions for mass spectrometry different instrument shall say SHEET operate this instrument reference standard recommended conditions are as follows. 47.1 Instrument Reference conditions 7.1.1 Reference conditions purge and trap device Purge flow. 40 ml/min; purge temperature. 40 ℃; Purge time. 11 min; blow dry time. 2 min; desorption temperature Degree. 180 ℃; Desorption time. 3min; baking temperature.200 ℃; baking time. 10 min; Transfer line temperature. 110 ℃. 7.1.2 GC reference conditions Temperature program. 35 ℃ (5 min) 5 ℃/min 180 ℃ 20 ℃/min 200 ℃ (5 min); Inlet temperature. 180 ℃; injection mode. split injection (20. 1); carrier gas. helium; interface temperature. 230 ℃; column flow. 1.2ml/min. Reference conditions 7.1.3 Mass Spectrometer Ionization mode. EI; ion source temperature.200 ℃; Transfer line temperature. 230 ℃; electron acceleration voltage. 70 eV; seizure Measuring mode. Full Scan method; mass range. 35 ~ 300amu. 7.2 Calibration 7.2.1 Meter Performance Check Samples prior to analysis to deal with GC - MS performance checks. Take 4-bromo-fluorobenzene (BFB) (4.9) solution of 1 μl straight Tap into the gas chromatographic analysis. 4-bromo-fluorobenzene key ion abundances should meet the criteria specified in Table 1, or need, and some of the mass spectrometer Parameter adjustment or cleaning the ion source. Table 1 BFB ion abundance key criteria Mass ion abundance ion abundance standard quality standard 50 15% by mass of 95 to 40% by mass greater than 95 174 of 50% 75 30% by mass of 95 to 60% by mass 174 175 5% to 9% 95 base peak, 100% relative abundance of quality 174 176 95% 101% 96 95 5 mass% to 9% by mass 176 177 5% to 9% 173 of less than 2% by mass 174 - - Draw a calibration curve 7.2.2 (1) determination of solid waste a calibration curve plotting Syringe with a micro pipette were a certain amount of standard solution (4.4) and substitute the use of liquid (4.8), containing 5 g to stone Sand (4.10), 5.0 ml test water (4.1) of the vial (5.3), to prepare the target content and alternatives were 5, 10,25,50,100 ng calibration series, and were added to 10 μl internal standard solution (4.6), immediately sealed. In accordance with the instrument Reference conditions (7.1) followed by injection analysis, in response to the value of the response value target ions and quantitative internal standard quantitation ion ratio Ordinate value, the ratio of the target content (ng) internal standard content as the horizontal, a calibration curve. Figure 1 is present Under standard conditions of the instrument, the object of the chromatogram. 5 elution order. 1- dichlorodifluoromethane; 2- chloride; 3- chloride; 4- methyl bromide; 5- tetrachloroethane; 6- trichlorofluoromethane; 7-1,1- two Vinyl chloride; dichloromethane -d2 8- (1 substitute); 9- dichloromethane; 10- dichloroethylene; 11-1,1- dichloroethane; 12-2,2 - Dichloropropane; 13-cis-1,2-dichloroethylene; 14- bromochloromethane; 15- chloroform; 16-1,1,1- trichloroethane; 17- carbon tetrachloride; 18-1, 1- Dichloropropene; 19-1,2- dichloroethane; 20- fluorobenzene (internal standard 1); 21- trichlorethylene; 22-1,2- dichloropropane; 23- dibromomethane; 24- Bromochloromethane; 25- cis-1,3-dichloropropene; 26- trans-1,3-dichloropropene; 27-1--chloro-2-bromo propane (internal standard 2); 28-1, 1,2-trichloro Ethane; 29- tetrachlorethylene; 30-1,3- dichloropropane; 31- Dibromochloromethane; 32-1,2- dibromoethane; 33-1,1,1,2- tetrachloride ethane; 34- Bromoform; 35-4- Bromofluorobenzene (internal standard 3); 36-1,1,2,2- tetrachloroethane; 37-1,2,3- trichloropropane; 38-1,2- two chlorobenzene -d4 (substitute 2); 39-1,2- dibromo-3-chloropropane; 40- hexachlorobutadiene. Chromatogram of Figure 1 target (2) determination of solid waste leachate calibration curve drawing Pipette syringe with a trace amount of each standard solution (4.4) and substitute the use of liquid (4.8), containing 5.0 ml to Vial extraction agent (5.3), the preparation of the target, and alternatives concentrations were 1,2,5,10,20 μg/L of calibration system Column, and were added to 10 μl internal standard solution (4.6), immediately sealed. An apparatus according to reference conditions (7.1) followed by injection analysis, In response to the ratio of the value of the response value target ions and quantitative internal standard for quantitation ion ordinate, target concentration (μg/L) And the ratio of the concentration of the internal standard for the abscissa, the calibration curve. Figure 1 is under instrument conditions specified in this standard of object Chromatogram. 7.2.2.1 average response factor to construct a calibration curve Standard Series point i object (or substitutes) relative response factor (iRRF), according to formula (1) is calculated. (1) Where. iRRF - Standard series point i object (or substitutes) relative response factor; iA - Standard series point i object (or substitute) response quantitation ion; ISiA - Standard series point i object (or substitute) corresponding to the response of the internal standard quantitation ion; ISi - standard series target concentration, ng; i - Standard series point i object (or substitute) mass concentration ng. ISi ISi i A ARRF   i 6 average target (or substitutes) relative response factors, according to the equation (2) is calculated. (2) Where. RRF - Average object (or substitutes) relative response factor; iRRF - Standard series point i object (or substitutes) relative response factor; n - Standard Series points. RRF standard deviation, according to the equation (3) is calculated. (3) RRF relative standard deviation according to equation (4) is calculated. (4) Standard Series object (or substitutes) relative response factor (RRF) relative standard deviation (RSD) should be less than or equal 20%. 7.2.2.2 calibration curve using the method of least squares The target compound and the corresponding internal standard response value ratio of the vertical axis, the concentration ratio of the horizontal axis, the establishment of the least squares method Calibration curve, the correlation coefficient of the standard curve ≥0.990. If the correlation coefficient of the calibration curve is less than 0.990, may be employed Non-linear calibration curve fitting, but it should be at least 6 concentrations using calibration points. 7.3 Determination of the sample The prepared sample (6.3) in accordance with the instrument reference conditions (7.1) were measured. 7.4 blank test The good blank sample preparation (6.4) in accordance with the instrument reference conditions (7.1) were measured.

8 Results Calculation and representation

8.1 Qualitative Analysis In full scan mode (Scan) data collection to sample target relative retention times (RRT), secondary ion qualitative And target ion abundance ratio (Q) with a range of standard solutions qualitatively. Relative retention time in the sample with the target school Relative retention time of the compound of the difference between the standard curve shall be within ± 0.06. Sample target ion secondary qualitative and quantitative away Sub-peak area ratio of the secondary ions qualitative and quantitative ion peak area (Q sample) and the calibration curve target ratio (Q standard) relative deviation Controlled within ± 30%. According to the formula (5) calculating the relative retention time RRT ISRT RTRRT x  (5) RRF RRF i  1   RRFRRF SD 0 RRF SDRSD 7 Where. RRT-- relative retention times; RTX-- retention time of the desired compound, min; Retention time RTIS-- internal standard, min. The average relative retention time (RRT). the relative retention times of the same object in the standard series according to the average formula (6) Total Operator assisted qualitative and quantitative ion ion peak area ratio (Q) AQ  (6) Where. At-- quantification ion peak area; Aq-- auxiliary qualifier ion peak area. 8.2 Quantitative Analysis Calculated based on the response of the target and internal standard quantification ions. When the target sample quantitation ion interference, You can use the secondary ion quantitative, specific See Appendix B. 8.2.1 Calculation object (or substitute) the quality of 1m 8.2.1.1 average relative response factor calculation When the object (or substitutes) using the average relative response factor for calibration, the content of the object of 1m by the formula (7) Calculated. (7) Where. 1m - the content of the object (or substitute) of, ng; xA - object (or substitute) response quantitation ion; ISm - the amount of the internal standard, ng; ISA - and the target (or substitute) corresponding to the response of the internal standard quantitation ion; RRF - Average object (or substitutes) relative response factors. 8.2.1.2 calculated using linear or non-linear calibration curve When the target linear or non-linear calibration curve calibration, the content of the object through the corresponding calibration curve 1m Calculations. 8.2.2 low content of volatile halogenated content of the sample, according to equation (8) is calculated. m1 (8) Where.  - content in the sample target object, μg/kg; 1m - the amount in a sample object (or substitute) of, ng; m - sample volume, g. 8.2.3 a high content of volatile halogenated content of the sample, according to the equation (9) is calculated. RRFA mAm IS ISx 1 8mV fVm  1 (9) Where.  - content in the sample target object, μg/kg; 1m - the amount in a sample object (or substitute) of, ng; cV - extract volume, ml; m - sample volume, g; SV - extract used to purge the volume, ml; f - extract dilution. Results 8.2.4 Calculation of solid waste leachate The determination of solid waste leachate concentrations of volatile halogenated Richard directly from the calibration curve to g/L represents. 8.3 The results are shown Determination of solid waste, when the measurement result is less than 100 μg/kg, retained after a decimal point; when the measurement result is greater than equal to 100 μg/kg, the retention three significant figures. Determination of solid waste leachate, when the measurement result is less than 100 μg/L, reserved one decimal place; when a large measurement results Than or equal to 100 μg/when L, retained three significant figures.

9 precision and accuracy

9.1 Precision Six laboratories respectively 0.4 μg/kg, 2.0 μg/kg and 10.0 μg/kg of solid waste spiked samples were determined. real Mortem indoor relative standard deviati...

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