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HJ 716-2014 English PDF

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HJ 716-2014: Water qualiy. Determination of nitroaromatics. Gas chromatography mass spactrometry
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Basic data

Standard ID HJ 716-2014 (HJ716-2014)
Description (Translated English) Water qualiy. Determination of nitroaromatics. Gas chromatography mass spactrometry
Sector / Industry Environmental Protection Industry Standard
Classification of Chinese Standard Z16
Word Count Estimation 21,271
Date of Issue 11/27/2014
Date of Implementation 1/1/2015
Quoted Standard GB 17378.3; HJ/T 91; HJ/T 164
Regulation (derived from) Ministry of Environmental Protection Notice 2014 No. 77
Issuing agency(ies) Ministry of Ecology and Environment
Summary This standard specifies the liquid-liquid extraction Determination of nitrobenzene compounds and solid phase extraction/gas chromatography - mass spectrometry. This standard applies to surface water, groundwater, measurement of industrial wastewater, sewa

HJ 716-2014: Water qualiy. Determination of nitroaromatics. Gas chromatography mass spactrometry


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Water qualiy.Determination of nitroaromatics.Gas chromatography mass spactrometry People's Republic of China National Environmental Protection Standards Water quality - Determination of nitrobenzene compounds Gas chromatography - mass spectrometry Water quality - Determination of nitroaromatics - Gas chromatography mass spectrometry (release draft) Issued on.2014-11-27 2015-01-01 implementation Ministry of Environmental Protection issued i Table of Contents Preface .ii 1. Scope ..1 2 Normative references ..1 3 principle of the method ..1 4 and eliminate interference .1 5 Reagents and materials .1 6 .2 instruments and equipment 7 .3 Samples 8 analysis step ..4 9 Results Calculation and representation ..5 10 precision and accuracy 7 11 Quality Assurance and Quality Control .7 12 waste disposal 8 Appendix A (normative) Determination of the detection limit and a lower limit .9 Determination of Annex B (informative) object reference parameters 10 Annex C (informative) method precision and accuracy .11

Foreword

To implement the "People's Republic of China Environmental Protection Law" and "People's Republic of China Water Pollution Prevention Law," protecting the environment, safeguarding human Healthy, standardized measurement method nitrobenzene compounds in water, the development of this standard. This standard specifies the determination of surface water, groundwater, industrial wastewater, sewage and seawater nitrobenzene compounds by GC - 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. Drafting of this standard. Tianjin Environmental Monitoring Center. The standard verification unit. State Key Lab of odor pollution control environmental protection, scientific research and monitoring by the Ministry of Agriculture, Environmental Protection, Tianjin Hexi District Environmental Monitoring Station, Tianjin Tanggu District Environmental Monitoring Station, Tianjin Dongli District Environmental Monitoring Station and Tianjin Dagang District Environmental Monitoring Station. This standard is approved by the Ministry of Environmental Protection November 27, 2014. This standard since January 1, 2015 implementation. The standard explanation by the Ministry of Environmental Protection. Water quality measurement 1 nitrobenzene compounds Gas chromatography - mass spectrometry Warning. Reagents and standard solutions used in this method has some toxicity, potentially harmful to health, and this should be avoided Direct contact with these chemicals. Operation should be required to required to wear protective equipment, sample pre-treatment process should be carried out in a fume hood.

1 Scope

This standard specifies the liquid-liquid extraction Determination of nitrobenzene compounds and solid phase extraction/gas chromatography - mass spectrometry. This standard applies to surface water, groundwater, measurement of industrial wastewater, sewage and seawater 15 kinds of nitrobenzene compounds. When the sample volume is 1L, the method detection limit of the target compound 0.04 μg/L ~ 0.05 μg/L, detection limit of 0.16 μg/L ~ 0.20 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 applies to this standard quasi. GB 17378 specification for marine monitoring Part 3 sample collection, storage and transport HJ/T 91 surface water and wastewater monitoring technical specifications HJ/T 164 groundwater environmental monitoring technical specifications

3 PRINCIPLE OF THE METHOD

Liquid-liquid extraction or solid phase extraction methods nitrobenzene compounds in the sample, extract was dehydrated, concentrated, purified and constant volume Separation by gas chromatography, mass spectroscopy. Based on retention time and mass spectra qualitative, quantitative internal standard.

4 and elimination of interference

High concentration samples with low concentration samples alternans cause interference when analyzing a high concentration samples should be analyzed after a blank sample or Reagent blank in order to prevent cross-contamination. If a target compound contained in the sample before the next sample also appeared, the analyst must Shall not be proved because the remaining result.

5 Reagents and materials

Unless otherwise indicated, the use of line with national standards for analytical chemistry reagents and distilled water analysis. 5.1 acetone (C3H6O). pesticide grade. 5.2 methanol (CH3OH). pesticide grade. 5.3 toluene (C7H8). pesticide grade. 5.4 dichloromethane (CH2Cl2). pesticide grade. 5.5 n-hexane (C6H14). pesticide grade. 5.6 sodium thiosulfate (Na2S2O3 • 5H2O). 25.7 anhydrous sodium sulfate (Na2SO4). Calcined at 400 ℃ for 4h, cooled charged grinding mouth glass bottles, placed in a desiccator save. 5.8 hydrochloric acid (HCl).  (HCl) = 1.19 g/ml. 5.9 Sodium hydroxide (NaOH). 5.10 nitrobenzene stock solution.  = 10 mg/ml, the solvent is methanol, commercially available. 5.11 internal standard stock solution.  = 10 mg/ml, the solvent is methanol, commercially. 5.12 alternatives stock solution.  = 10 mg/ml, the solvent is methanol, commercially. 5.13 tuning stock standard solution.  = 2.5 mg/ml, the solvent is methanol, commercially available. 5.14 nitrobenzene using standard solution.  = 200 μg/ml. Take 0.50 ml nitrobenzene stock solution (5.10) added to a solution containing an appropriate amount of methylene chloride (5.4) of 10.0 ml brown volumetric flask, Diluted with dichloromethane (5.4) to the mark, frozen. 5.15 internal standard solution is used.  = 200 μg/ml. Take 0.50 ml of internal standard stock solution (5.11), containing an appropriate amount was added to methylene chloride (5.4) in 10.0 ml brown flask, with Dichloromethane (5.4) diluted to the mark, frozen. 5.16 alternatives using standard solution.  = 200 μg/ml. Take 0.50 ml substitute stock solution (5.12) added to a solution containing an appropriate amount of methylene chloride (5.4) of 10.0 ml brown volumetric flask, Diluted with dichloromethane (5.4) to the mark, frozen. 5.17 tuning using standard solution.  = 50 μg/ml. Take 0.20 ml tuning stock standard solution (5.13) added to a solution containing an appropriate amount of methylene chloride (5.4) of 10.0 ml brown volumetric flask Dichloromethane (5.4) diluted to the mark, frozen. 5.18 hydrochloric acid solution. 11. Sodium hydroxide solution 5.19. C (NaOH) = 0.1 mol/L. 5.20 dichloromethane - n-hexane. 91. 5.21 SPE column. C18 or equivalent type of filler or combination of fillers type filler, 1000 mg/6.0 ml, commercially available, or solid phase extraction disk, etc. Extraction performance with equivalent items. 5.22 Florisil Column. 1000 mg/6.0 ml, particle size of 40 μm, commercially available. 5.23 Carrier gas. helium, purity ≥99.999%. 5.24 nitrogen purity ≥99.999%. For drying the concentrated sample remaining.

6 instruments and equipment

6.1 GC/MS. a capillary split/splitless inlet, a constant current or constant voltage function, programmable up, with EI source And ChemStation. 6.2 Solid phase extraction device. 6.3 concentration device. nitrogen blowing instrument, a rotary evaporator or the like KD concentrator considerable performance devices. 6.4 Precision Balances. a sense of the amount of 0.1 mg. 6.5 Capillary Column. capillary column, length 30 m, an inner diameter of 0.25 mm, a thickness of 0.25 μm, the stationary phase is 100% dimethylpolysiloxane Silicone or other equivalent capillary column. 36.6 Sampling bottle. 1 ~ 4 L brown with teflon liner screw cap bottles. 6.7 micro syringe. 100 l, 50 l and 10 l. 6.8 funnel. 0.5 L, 1 L or 2 L. 6.9 General Commonly used laboratory instruments and equipment.

7 Sample

Sample collection and preservation 7.1 According to GB 17378, HJ/T 91 and HJ/T relevant provisions of the 164 water samples were collected and preserved. When collecting samples, do not use Sample pre-wash water sampling bottles. Samples should be filled sampling bottle (6.6) and affix the seal. Flow in the presence of residual chlorine to be added per liter of water at 80 g sodium thiosulfate (5.6) dechlorination. After sample collection should be dark at 4 ℃ refrigerator, complete extraction within the 7 d, 40 d complete analysis within. 7.2 Preparation of the sample 7.2.1 liquid-liquid extraction 7.2.1.1 Extraction The exact amount of 1000 ml water sample (sample extraction of the water volume may be appropriately adjusted according to the water quality), with a hydrochloric acid solution (5.18) or hydrogen Sodium hydroxide solution (5.19) adjusting the pH in the neutral water sample, placed in a separatory funnel, was added 5.0 μl substitute standard solution (5.16), Mix, plus 50 ml of methylene chloride and extracted 3 ~ 5 min, allowed to stand for 5 ~ 10 min stratification, the organic phase was separated, then 30 ml of methylene chloride was added Extraction was repeated once, and the combined extracts were dried over anhydrous sodium sulfate, and concentrated to about 0.5 ml, add 5 ml of n-hexane, concentrated to continue Approximately 0.5 ml. Note 1. Emulsion phenomenon extraction process, we can use salting, stirring, centrifugation, freezing and breaking glass wool filtration method. Note 2. The concentration of the extract process should pay attention to the speed of the water bath temperature and concentration, otherwise nitrobenzene prone to large losses. 7.2.1.2 Purification Flush with 8 ml of n-hexane Florisil before the liquid disappears, and the extract was concentrated liquid was transferred to a cleaning column with 4 ml n Washed with hexane and concentrated pipe, washing liquid also transferred onto florisil (Note. You should always maintain a level above the filler left), discard the effluent Washed with 10 ml of dichloromethane - n-hexane (5.20) eluting samples, collected in a receiving tube. 7.2.1.3 concentrate volume The eluate was concentrated to about 0.5 ml, to which was added 10.0 μl using internal standard solution (5.15), with dichloromethane and dilute to 1.0 ml, Mix tested. 7.2.2 Solid Phase Extraction 7.2.2.1 Activation. successively with 5 ml of dichloromethane, 5 ml of methanol and 10 ml of water, activated solid phase extraction column, flow rate of about 5 ml/min. Note 3. The activation process should be avoided SPE packing above the liquid level is drained, or need to re-activation. 7.2.2.2 Extraction. The exact amount of 1000 ml water sample (sample enrichment of the water volume may be appropriately adjusted according to the actual situation of water samples), acid-soluble salt Solution (5.18) or sodium hydroxide solution (5.19) in water samples neutral pH adjusted to each water sample was added methanol (5.2), methanol concentration Of about 5 ‰, then add 5.0 μl alternative to the standard solution (5.16) and mix. The water sample to 5 ~ 10 ml/min flow rate of enriched sample After completion, rinse with 10 ml of water on the inner wall of the vial, and enriched in the solid phase extraction column, drained cartridge. If using automated solid phase extraction sample extraction device, in accordance with the rules of each model of the instrument extracted. 7.2.2.3 elution. with 10 ml of methylene chloride to 2 ml/min sample rate of elution, the eluent dried column eluate to collect concentrated Shrink tube. 47.2.2.4 concentrated volume. eluent shrink shrink to 0.5 ml, was added 10.0 μl using internal standard solution (5.15), with dichloromethane to volume To 1.0 ml, mix, prepare analysis. Note 4. high suspended solids content of the water sample, not for solid phase extraction. 7.3 Preparation of blank samples Samples were analyzed at the same time, taking the same volume of water, according to the sample preparation method of (7.2), prepare a blank sample. Analysis Step 8 8.1 GC reference conditions Inlet temperature. 250 ℃. Injection mode. split injection, split ratio of 5. 1. Oven temperature. 60 ℃ → 10 ℃/min → 200 ℃ → 15 ℃/min → 250 ℃. Column flow rate. 1.0 ml/min. Injection volume. 1.0 μl. 8.2 Mass Reference Conditions Scan mode. Full scan or selected ion monitoring (SCAN/SIM). Scan range. 40 ~ 500 amu. Ion source temperature. 230 ℃. Transfer line temperature. 280 ℃. Ionization energy. 70 eV. The remaining parameters are set with reference to the instrument instruction manual. 8.3 Instrument performance checks Before using the instrument, sample and analyze each running 24 h, gas chromatography mass spectrometer system must be carried out to check the performance of the instrument. Take 1.0 μl Tuning standard solution (5.21) directly into the chromatograph, DFTPP key ion abundance obtained shall meet the specified criteria in Table 1. Otherwise required Some parameters can be adjusted or cleaning the mass spectrometer ion source. Table 1 Decafluorotriphenylphosphine triphenylphosphine (DFTPP) ion and abundance of key criteria Mass to charge ratio (m/z) abundance of standard mass ion (m/z) abundance Standard 5% 9% 51 base peak 30% to 60% of the base peak 199 Less than 69 68 275 2% of the peak of the fundamental peak of 10% to 30% 70 less than 69 peaks higher than 2% 365 1% of the base peak 127 base peak of 40% to 60% and less than 441 exist peaks 443 197 is less than 1% of the base peak 442 is greater than 40% of the base peak 198 base peak, the abundance of 17% to 23% 100% 443 442 peak 8.4 Calibration 8.4.1 Calibration Series A certain amount of nitrobenzene compounds using standard solution (5.14) and the use of alternatives to the standard solution (5.16) in dichloromethane (5.4) To prepare a series of six standard concentration point, the mass concentration of nitrobenzene compounds were 0.1 μg/ml, 0.5 μg/ml, 1.0 μg/ml, 2.0 μg/ml, 5.0 μg/ml, 10.0 μg/ml, was added to the standard uses standard solution (5.15), so that the internal standard concentration was 2.0 μg/ml. 58.4.2 average relative response factor calibration curve Standard Series point i of the target (or substitutes) relative response factor (iRRF), according to (1) calculated as follows. i IS IS ii ARRF A   (1) Where. iRRF-- standard series point i object (or substitutes) relative response factor; ISiA - Standard series point i object (or substitute) corresponding to the response of the internal standard quantitation ion; iA - response standard series point i object (or substitute) quantitative ion; IS - standard series, the subject of concentration, g/ml; i - Standard series point i object (or substitute) mass concentration, g/ml. Average object (or substitutes) relative response factors iRFF, (2) calculated according to the formula. RRF RRF  1 (2) Wherein. the average iRRF-- object (or substitutes) relative response factors; iiRRF - Standard series point i object (or substitutes) relative response factor; n-- standard series points. RRF standard deviation (SD), in accordance with the formula (3) is calculated. . (3) RRF relative standard deviation (RSD), in accordance with the formula (4) is calculated. .. (4) 8.4.3 calibration curve using the method of least squares If a standard series of target compounds relative standard deviation of the relative response factor greater than 20%, then the required target Least Squares Method calibration curve calibration. That is relative to the target and within the target response value ratio of the vertical axis, the concentration ratio of the horizontal axis, a calibration curve. 8.5 Determination Take 1.0 l sample (7.2) into the gas chromatograph mass spectrometer, a calibration curve in accordance with the same instrumental conditions were determined. 8.6 blank test Take the prepared blank sample (7.3), according to a calibration curve with the same instrumental conditions were determined.

9 Results Calculation and representation

9.1 Qualitative Analysis The retention time of the sample in the target compound (RT), the fragment ions of different mass to charge ratio and ion abundance than qualitative. Nitrobenzene i = 1 n-1SD   2 (RRF RRF) 100% SDRSD  RRF Characteristics of ionic compounds 6, see Appendix B. Retention time in the sample with the desired retention time of the target compound (i.e., the average standard solution relative retention time) of the relative deviation Should be controlled within ± 3%; different fragment ion abundance ratios and the expected sample target compound (ie, the standard fragment ions in solution The average ion abundance ratio) relative deviation should be controlled within ± 30%. Under instrument conditions specified in this standard, total ion current target compound, shown in Figure 1. 1- nitrobenzene -d5 (SS); 2- nitrobenzene; 3-o - nitrotoluene; 4- Room - nitrotoluene; 5-p - nitrotoluene; 6-- Room - nitro chlorobenzene ; 7-p - nitro chlorobenzene; 8- o - nitro chlorobenzene; 9-1--bromo-2-nitrobenzene (IS); 10- to - dinitrobenzene; 11- Room - dinitrobenzene ; 12-2,6- Dinitrotoluene; 13-o - dinitrobenzene; 14-2,4- dinitrotoluene; 15-2,4- dinitrochlorobenzene; 16-3,4- dinitrotoluene; 17-2,4,6- trinitrotoluene; 18- PCNB (SS) Fig.1 Total ion nitrobenzene compounds 9.2 Quantitative Analysis In full-scan method to collect data, to select the ions, internal standard. 9.2.1 average relative response factor calculation When the object (or substitute) using the average relative response factor for calibration, sample quality target (or substitutes) concentrated Degree  according to formula (5) is calculated. x IS ex IS i AV DFVA RRF     (5) Where.  - mass concentration of the target compound or substitute a sample, g/L; xA - object (or substitute) response quantitation ion; ISA - and the target (or substitute) corresponding to the response of the internal standard quantitation ion; IS - mass concentration of the internal standard, g/L; exV - sample volume, ml; 0V - water sample volume, L; DF-- dilution factor. 79.2.2 calculated using linear or non-linear calibration curve When the object (or substitute) linear or non-linear calibration curve for calibration, sample target (or substitutes) mass  volume concentration is calculated by the corresponding calibration curve according to equation (6).  = 0V Vexi  DF (6) Where. i - concentration by the calibration curve to obtain the objective compound (or substitutes) of, g/ml; exV - sample volume, ml; 0V - water sample volume, L; DF-- dilution factor. 9.3 The results are shown When the measurement result is less than 1.00 g/L, data retention to the second decimal place; when the result is greater than equal to 1.00 g/L, data Three significant figures. 10 precision and accuracy 10.1 Precision Six laboratories 0.100 g/L, 2.50 g/L, 5.00 g standard samples/L nitrobenzene compounds at different concentrations were measured. Liquid-liquid extraction. the laboratory relative standard deviation of 1.1% ~ 9.2%, inter-laboratory relative standard deviation of 1.0% to 12.6%, the repeatability limit 0.01 g/L ~ 0.46 g/L, the reproducibility limit 0.03 g/L ~ 0.88 g/L. Solid Phase Extraction. Laboratory relative standard deviation of 1.3% ~ 8.8%, inter-laboratory relative standard deviation of 1.0% to 11.9%, the repeatability limit 0.01 g/L ~ 0.59 g/L, the reproducibility limit 0.03 g/L ~ 1.02 g/L. 10.2 Accuracy Liquid-liquid extraction. Six laboratories containing compounds nitrobenzene low, medium and high concentrations of the different samples were analyzed measured recovery was. 71.9% To 101%. Six laboratories containing compound concentration of nitrobenzene was 2.50 g/L were unified sample Determination recoveries range 78.4% to 101%. Solid Phase Extraction. Six laboratories containing compounds nitrobenzene low, medium and high concentrations of the different samples were analyzed measured recovery was. 71.4% ~ 100%. Six laboratories containing compound concentration of nitrobenzene was 2.50 g/L were unified sample Determination recoveries range 73.6% to 101%. Precision and accuracy of results in Appendix C. 11 Quality Assurance and Quality Control 11.1 Analysis of the internal standard Comparison Comparison internal standard internal standard and internal standard curve middle point of the calibration curve verification, samples with the same batch of the internal standard calibration curve verification, Paul Stay time is not more than 10 s, quantification ion peak area varied between 50% to 100%. Standard 811.2 allow initial calibration curve Standard Series object (or substitutes) relative response factor (RRF) relative standard deviation (RSD) should be less than or equal to 20%. If the object of a series of standards relative response factor relative standard deviation is greater than 20%, the target required this method of least squares calibration curve Line calibration, nonlinear curve fitting may also be used for calibration, the correlation coefficient should ≥0.990. 11.3 calibration curve verification A second intermediate point of the calibration curve of the standard solution is determined at least every working day, according to equation (7) Calculate measured value of the target compound (cRFF Or i) and last initial calibration curve relative deviation (iRFF or s) between (RD). Formula is as follows. 100 siRD  % (7) Where. s - the concentration of the calibrator calibration curve middle point, g/ml; i - The calibration concentration measurement, g/ml. If RD≤20%, the initial calibration curve can continue to use; if any one of the compounds RD > 20%, to reconfigure System curve or intermediate point to measure the...

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