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HJ 714-2014 English PDF

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HJ 714-2014: Solid wastes. Determination of volatile halohydrocarbons. Headspace gas chromatography mass method
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HJ 714-2014English629 Add to Cart 5 days [Need to translate] Solid wastes. Determination of volatile halohydrocarbons. Headspace gas chromatography mass method Valid HJ 714-2014

Standard similar to HJ 714-2014

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Basic data

Standard ID HJ 714-2014 (HJ714-2014)
Description (Translated English) Solid wastes. Determination of volatile halohydrocarbons. Headspace gas chromatography mass method
Sector / Industry Environmental Protection Industry Standard
Word Count Estimation 24,292
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 714-2014: Solid wastes. Determination of volatile halohydrocarbons. Headspace gas chromatography mass method


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Solid wastes.Determination of volatile halohydrocarbons.Headspace gas chromatography mass method People's Republic of China National Environmental Protection Standards Solid waste - Determination of volatile halogenated Headspace - gas Chromatography/Mass Spectrometry Solid wastes-Determination of volatile halohydrocarbons -Headspace Gas chromatography mass method (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 headspace/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. Headspace 1 solid waste volatile halogenated hydrocarbons - 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 solid waste chloride and other volatile halogenated headspace/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 verified onset halogenated hydrocarbons can also be applied to this standard. The solid waste sample amount of 2 g, 35 kinds of volatile halogenated hydrocarbons detection limit of 2 ~ 3 μg/kg, detection limit is 8 ~ 12 μg/kg; the solid waste leachate volume of 10.0 ml, the detection limit was 0.7 ~ 1.5 μg/L, detection limit of 2.8 to 6.0 μg/L. See Appendix A.

2 Normative references

This standard refers to the contents of the following documents or the terms. For undated references, the effective version suitable For 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

Under certain temperature conditions within the sample vial of volatile halogenated hydrocarbons to the headspace volatiles, have some steamed Pressure and achieve liquid-solid three phase, vapor samples taken after entering gas chromatography with mass spectrometer detection. according to Retention time fragment ion mass to charge ratio and different ion abundance ratios of qualifier 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 goals or objectives Concentrations below the detection limit. 4.2 methanol (CH3OH). pesticide grade, before use by testing to confirm no goal or target concentration below detection method The limit. 4.3 phosphoric acid. pure class distinctions. 4.4 Sodium chloride (NaCl). excellent pure, at 400 ℃ in a muffle furnace bake 4 h, the dryer to cool to room temperature and placed, Stored in a grinding mouth brown glass bottles sealed. 4.5 based modifier. phosphoric acid (4.3) dropwise to a 100 ml test water for adjusting the pH value of less than 2; then add 36 g of sodium chloride (4.4) were mixed. At 4 ℃ stored for up to 6 months. 4.6 standard stock solution. ρ = 2000 mg/L. Direct purchase a commercially available certified reference solution. The following -10 ℃ from light, or by reference to the manufacturer's product description. Should be used Returned to room temperature and shake well. 24.7 standard solution. ρ = 20 mg/L. Take the right amount of stock standard solution (4.6) with methanol (4.2) appropriately diluted. 4.8 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. 4.9 internal standard solution. ρ = 25 mg/L. The proper amount of the internal standard stock solution (4.8), with methanol (4.2) appropriately diluted. 4.10 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. 4.11 alternatives to the use of liquid. ρ = 25 mg/L. The appropriate amount of stock solution substitute (4.10), methanol (4.2) appropriately diluted. 4.12 4-bromo-fluorobenzene (BFB) solution. ρ = 25 mg/L. It can be purchased directly certified standard solution can also be used in preparing a standard, diluted with methanol. 4.13 quartz sand. 20 to 50 mesh, before use by testing to confirm no goal or target concentration below the detection limit. 4.14 Helium. purity ≥99.999%, by deoxidizer oxygen, molecular sieve dehydration. 5. Apparatus 5.1 Sampling equipment. shovels and stainless steel spatula. 5.2 Sampling bottles. a Teflon liner 60 ml screw brown glass bottle. 5.3 Gas chromatography - mass spectrometry. EI ionization source. 5.4 Column. capillary column, length 30 m, an inner diameter of 0.25 mm, a thickness of 1.4 μm, the stationary phase is 6% nitrilpropionamide phenyl/94% Dimethyl polysiloxane may be used other equivalent capillary column. 5.5 Empty Autosampler. with the top bottles, gaskets. 5.6 bottles. 22 ml, with teflon gaskets sealing cap top bottles (with Headspace Sampler match), caps (spiro Capping or single-use gland). 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, can be fixed vial. 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 following temperature reached 4 ℃. 5.13 General common laboratory instruments and equipment.

6 samples

Samples collected 6.1 According to HJ/T relevant requirements of solid waste collected 20 samples. Portable VOC detector on solid sampling site The level of concentration of the sample were screened, and tags. All samples shall be collected at least three parallel samples. Samples were collected as soon as possible mining Vials (5.2) and as full as possible, quickly removed the sample bottles and threaded outer surface adhesion of the sample, seal sampling bottles. 3 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. Save 6.2 sample After sample collection into a portable freezer (5.12) in. After reaching the laboratory, should be analyzed as soon as possible. If not timely analysis, Samples should be lower than 4 ℃ preservation, storage period of 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 Taken out of the laboratory sample bottles (5.2) returned to room temperature, 2 g sample was weighed vial (5.6) was added 10.0 ml Matrix modifiers (4.5), 2.0 μl substitute (4.11) and 4.0 μl internal standard (4.9), immediately sealed. 10 min oscillations of the sample Product mix, to be tested. Note 2. For special sample sampling amount can be adjusted to ensure that the vial headspace is consistent with the calibration series. 6.3.2 Solid Waste high content in the sample Preliminary site screening of volatile halogenated hydrocarbons assay results greater than 200 μg/kg, the sample depending on the content of the sample is high. real Remove the indoor test sample bottle (5.2) returned to room temperature, weighed 2 g sample gently into the headspace vial (5.6) was added 10.0 ml Methanol (4.2), immediately sealed. Shaken at room temperature 10 min, allowed to settle back, take 2.0 ml to 2 ml extract dense brown Bottle (5.10), the seal. The extract can be placed in the freezer at 4 ℃ preservation, storage period of 14 d. Analysis Sample recovery Complex to room temperature, with a micro-syringe (5.7) take the appropriate amount of the extract was injected into the quartz sand containing 2 g (4.13), 10.0 ml substrate Now close modifier (4.5) headspace vial (5.6), and 2.0 μl substitute (4.11) and 4.0 μl internal standard (4.9) after Sealed and shaken 10 min the sample mix tested. Note 3. If the methanol extract target higher concentrations can be used appropriately diluted 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 Preparation of solid waste leachate sample leaching execution HJ/T 299 or HJ/T 300 method. Take 10.0 ml leaching solution transferred Headspace vial (5.6), and 4.0 μl used as substitutes solution (4.11) and 10 μl internal standard solution (4.9), immediately sealed, Tested. 6.4 Preparation of blank samples 6.4.1 Solid Waste low content of a blank sample With 2 g of quartz sand (4.13) 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 With 2 g of quartz sand (4.13) instead of the sample according to 6.3.2 step of producing high levels 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 (4.13) instead of the sample, prepared according to step 6.3.3 Solid waste leachate blank sample.

7 Procedure

Different models headspace sampler, gas chromatography - different optimum operating conditions of the mass spectrometer, the instrument shall be in accordance with the instructions for use Book operate this instrument reference standard recommended conditions are as follows. 7.1 Instrument Reference conditions 7.1.1 Headspace means the reference conditions 4 equilibration time. 30 min; equilibrium temperature. 60 ℃; injection time. 0.04 min; transfer line temperature. 100 ℃. 7.1.2 GC reference conditions Temperature program. 35 ℃ (5 min) 5 ℃/min 180 ℃ 20 ℃/min 200 ℃ (5 min); Jin Inlet temperature. 180 ℃; injection mode. split injection (20. 1); carrier gas. helium; interface temperature. 230 ℃; column flow. 1.2 ml/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) (4.12) solution of 1 μl Direct injection gas chromatographic analysis, the BFB spectrum should meet the requirements specified in Table 1 or a reference to the manufacturer's instructions. 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 mass 95 30% 60% 175 mass 174 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 - - 7.2.2 Calibration curve plotting (1) determination of solid waste a calibration curve plotting To 5 vial were added successively 2 g of quartz sand (4.13), 10.0 ml matrix modifiers (4.5), with micro injection Respectively Pipette a quantity of standard solution (4.7) and used as substitutes solution (4.11), the preparation of the target content and alternatives stars Do 20,40,100,200,400 ng to the standard series, and were added 4 μl internal standard solution (4.9), immediately sealed. Fully shaking for 10 min, in accordance with the instrument reference conditions (7.1) followed by injection analysis in response to the value of the object of quantitative ion and The ratio of the response of the internal standard quantitation ion for the vertical axis, and the ratio of the target content (ng) internal standard content as the horizontal, Calibration curve. Figure 1 is under instrument conditions specified in this standard chromatogram target. Elution order. 1- dichlorodifluoromethane; 2- chloride; 3- chloride; 4- methyl bromide; 5- tetrachloroethane; 6- trichlorofluoromethane; 7-1,1- two 5 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- o-dichlorobenzene - 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 To 5 vial was added sequentially 10.0 ml extraction agent, using a micro syringe, respectively Pipette a certain amount of standard solution (4.7) and used as substitutes solution (4.11), and alternatives target formulation concentrations were 5,10,25,50,100 μg/L Standard series, and were added to 10 μl internal standard solution (4.9), immediately sealed. Fully shaking for 10 min, in accordance with the instrument Reference conditions (7.1) followed by injection analysis, in response to the response of the target ion and quantitative internal standard quantitation ion values The ratio of the vertical axis to the target concentration (μg/L) ratio of the concentration of the internal standard for the abscissa, the calibration curve. Target The chromatogram shown in Figure 1. 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. Average object (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 RRF i  1 ISi ISi i A ARRF   i   RRFRRF SD 6RRF 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, and to be 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 scan mode (the Scan) data acquisition, the target compound in the sample relative retention time (the RRT), an auxiliary characterization Ion and target ion abundance ratio (Q) with a range of standard solutions qualitatively. Sample relative retention target compound Relative retention time difference between the time the calibration curve of the compound should be within ± 0.06. Assisted qualitative sample target compound Qualitative and quantitative secondary ion ion ion peak area of the quantitation ion and the peak area ratio (Q sample) and the standard curve than the target compound (Q standard) relative deviation controlled within ± 30%. According to the formula (5) calculating the relative retention time RRT ISRT RTRRT x  (5) 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 standard range of the average value of the same objective compound According to the formula (6) Computer-Aided 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, 0 RRF SDRSD 7 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 the desired compound content in the sample (μg/kg), according to equation (8) is calculated. m1 (8) Where.  - content in the sample target object, μg/kg; 1m - the amount of the calibration curve obtained in the investigation object (or substitute) of, ng; m - sample volume, g. 8.2.3 content high content of the sample target (μg/kg), according to the equation (9) calculated. mV fVm c1  (9) Where.  - content in the sample target object, μg/kg; 1m - the amount of the calibration curve obtained in the investigation object (or substitute) of, ng; cV - extract volume, ml; m - sample volume, g; SV - used to extract headspace volume, ml; ƒ-- extract dilution liquid. Results 8.2.4 Calculation of solid waste leachate The determination of solid waste leachate concentration of target 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 g/kg, reserved one decimal place; when the measurement result is greater than equal to 100 g/kg, the retention three significant figures. RRFA mAm IS ISx 1 8 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 ...

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