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HJ 1223-2021 English PDF

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HJ 1223-2021: Ambient air Emergency determination of volatile organic compounds - Portable gas chromatography-mass spectrometry
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HJ 1223-2021English629 Add to Cart 5 days [Need to translate] Ambient air Emergency determination of volatile organic compounds - Portable gas chromatography-mass spectrometry Valid HJ 1223-2021

Standard similar to HJ 1223-2021

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Basic data

Standard ID HJ 1223-2021 (HJ1223-2021)
Description (Translated English) Ambient air Emergency determination of volatile organic compounds - Portable gas chromatography-mass spectrometry
Sector / Industry Environmental Protection Industry Standard
Word Count Estimation 27,224
Issuing agency(ies) Ministry of Ecology and Environment

HJ 1223-2021: Ambient air Emergency determination of volatile organic compounds - Portable gas chromatography-mass spectrometry


---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.
(Ambient air - Emergency determination of volatile organic compounds - Portable gas chromatography-mass spectrometry) National Ecological Environment Standard of the People's Republic of China Emergency Determination of Volatile Organic Compounds in Ambient Air Portable Gas Chromatography-Mass Spectrometry Ambient air-Emergency determination of volatile organic compounds- Portable gas chromatography-mass spectrometry This electronic version is the official standard text, which is reviewed and typeset by the Environmental Standards Institute of the Ministry of Ecology and Environment. Published on 2021-12-16 2022-03-01 Implementation Released by the Ministry of Ecology and Environment directory Foreword...ii 1 Scope...1 2 Normative references...1 3 Principles of the method...1 4 Reagents and materials...1 5 Instruments and equipment...2 6 Preparation before monitoring...2 7 Samples...2 8 Analysis steps...2 9 Result calculation and representation...5 10 Accuracy...6 11 Quality Assurance and Quality Control...7 12 Waste Disposal...7 13 Notes...7 Appendix A (Normative Appendix) Method Detection Limit and Determination Limit of Target Compounds...8 Appendix B (Informative Appendix) Preparation of Standard Gas by Static Dilution...10 Appendix C (informative) Total ion chromatograms of target compounds...11 Appendix D (informative) Quantitative ions and auxiliary ions of target compounds...13 Appendix E (Informative) Method Accuracy...15 Portable gas chromatography-mass spectrometry for emergency determination of volatile organic compounds in ambient air Warning. When using this method, pay attention to the dangers of the accident site and the surrounding environment, and do a good job of personal protection.

1 Scope of application

This standard specifies a portable gas chromatography-mass spectrometry method for the determination of volatile organic compounds in ambient air. This standard is applicable to the on-site emergency determination of 52 volatile organic compounds such as toluene in the ambient air around the site of an environmental emergency. This method can also be used for qualitative analysis and concentration estimation of volatile organic compounds. In full scan mode, when the injection volume is 600 ml, the split ratio is 50.1, or the injection volume is 100 ml, splitless, the method detection limit is It is 3 μg/m3～9 μg/m3, and the lower limit of determination is 12 μg/m3～36 μg/m3, see Appendix A for details.

2 Normative references

This standard refers to the following documents or clauses thereof. For dated references, only the dated version applies to this standard. For undated references, the latest edition (including all amendments) applies to this standard. GB/T 32210 Portable gas chromatography-mass spectrometer technical requirements and test methods HJ 589 Technical specification for emergency monitoring of environmental emergencies HJ 732 Sampling air bag method for volatile organic compounds in waste gas from stationary pollution sources

3 Principles of the method

The sample is directly introduced or adsorbed by an adsorption tube and thermally desorbed, and then enters into the gas chromatography for separation, and is detected by a mass spectrometer. for 52 species Standard compound, qualitative by comparing with standard substance mass spectrum and retention time, internal standard method quantification; for substances other than 52 target compounds By comparing with the mass spectrum of the standard substance qualitatively, according to the ratio of its response value to the response value of the internal standard, its concentration is estimated.

4 Reagents and Materials

4.1 Standard gas. the concentration is not less than 1 μmol/mol, the pressure is not less than 1.0 MPa, stored in a steel cylinder, it can be stored for 1 year, or refer to the standard Instructions for the gas certificate. According to the actual work needs, you can purchase a higher concentration of certified standard gas or customize a suitable mixture in a qualified unit. standard gas. 4.2 Field standard gas. use the gas diluter (5.7) in the laboratory to dilute the standard gas (4.1) with nitrogen gas (4.4) to 10 nmol/mol. Field standard gas can be stored in stainless steel tank (5.6) for 20 days and in air bag (5.2) for 8 hours. Note. The static dilution method (see Appendix B) can also be used to prepare liquid standard substances. 4.3 Internal standard gas. 1,3,5-tris(trifluoromethyl)benzene (100 μmol/mol), bromopentafluorobenzene (50 μmol/mol) or 4-bromo Fluorobenzene (20 μmol/mol), stored in a steel cylinder, can be kept for 1 year, or refer to the relevant instructions of the standard gas certificate. meeting the method requirements and Under the premise of not interfering with the target compound, other substances can also be used as internal standards. 4.4 Diluent gas. nitrogen, purity ≥99.999%. 4.5 Carrier gas. nitrogen or helium, purity ≥99.999%.

5 Instruments and equipment

5.1 Vacuum gas sampling box. It is composed of air inlet pipe, vacuum box, valve and air pump. The components to be tested react. 5.2 Air bag. The material should meet the relevant requirements of HJ 732. 5.3 Portable gas chromatography-mass spectrometer. gas sampling module with temperature control function, adsorption thermal desorption module, gas chromatography module (with temperature programmed function), and quadrupole or ion trap mass spectrometry modules. The mass spectrometry module features a 70 eV electron impact (EI) ion source with full scan Scanning/selected ion scanning, automatic/manual tuning, spectral library search and quantitative analysis, etc. The performance indicators should meet the requirements of GB/T 32210.Place Pipes and fittings through which the sample passes should be inert. 5.4 Capillary column. 15 m×0.25 mm×1.0 m or 10 m×0.1 mm×0.4 m, the stationary phase is 100% dimethylpolysiloxane alkane, other equivalent capillary columns can also be used. 5.5 Built-in adsorption tube. Fill with adsorbents such as Tenax, Carbopack, silica gel, or other equivalent adsorbents. 5.6 Stainless steel tank. The inner wall is inertized, and the pressure resistance value is greater than 241 kPa. 5.7 Gas diluting instrument. the maximum dilution ratio is at least 1000 times, and the pipelines should be inertized. 5.8 Commonly used instruments and equipment.

6 Preparation before monitoring

Check the working status of the portable gas chromatograph-mass spectrometer, and confirm that the on-site standard gas (4.2) and internal standard standard that meet the work requirements are carried. gas (4.3) and carrier gas (4.5); confirm carrying batteries, vacuum gas sampling box (5.1), gas bag (5.2), gas sampling module and personal Protective equipment and other necessary spare parts.

7 samples

7.1 Sample Collection 7.1.1 The requirements for point layout and on-site monitoring shall be implemented in accordance with the relevant regulations of HJ 589. 7.1.2 Select an appropriate method according to the on-site situation, and use the gas sampling module of the portable gas chromatograph-mass spectrometer (5.3) for direct sampling; When the field conditions are limited or the actual work requires, the vacuum gas sampling box (5.1) can also be used to collect air bag samples. 7.1.3 After sampling, air bag samples should be transported and stored in dark and normal temperature conditions, and should be analyzed as soon as possible. 7.2 Preparation of blank samples Fill the pre-cleaned air bag (5.2) with nitrogen gas (4.4).

8 Analysis steps

8.1 Instrument Reference Conditions 8.1.1 Adsorption thermal desorption reference conditions Condition 1.Sampling probe temperature. 40 ℃; heating line temperature. 70 ℃; injection flow rate. 100 ml/min; adsorption tube desorption temperature. 300 ℃; pre-desorption time of adsorption tube. 0.1 min; desorption time of adsorption tube. 0.5 min; splitless; injection volume. 5 ml to 100 ml. Condition 2.Sampling probe temperature. 40 °C; heating line temperature. 70 °C; injection flow rate. 100 ml/min; adsorption tube desorption temperature. 300 ℃; pre-desorption time of adsorption tube. 0.1 min; desorption time of adsorption tube. 0.5 min; split ratio of 50.1; injection volume. 6 ml to 600 ml. Or set according to the instrument instruction manual. 8.1.2 Gas chromatography reference conditions Condition 1.Column pressure. 80 kPa; splitless; temperature program. 60 °C for 3 min, 18 °C/min to 130 °C, and then 30 °C/min The temperature was raised to.200 °C and held for 1 min. Condition 2.column flow rate. 0.2 ml/min; split ratio 50.1; temperature program. 60 °C for 1 min, 10 °C/min to 80 °C, and then Raised to 220 °C at 40 °C/min and held for 1 min. Or set according to the instrument instruction manual. 8.1.3 Reference conditions for mass spectrometry Ion source. EI; ionization energy. 70 eV; scanning mode. full scan; scanning range. 41 u～300 u. or use according to the instrument manual to set. See Appendix C for the total ion chromatogram obtained from the determination of the target compound standard substance under the reference conditions. Note. When the detection limit of the target compound does not meet the standard limit requirements, the ion scanning mode can be selected. 8.2 Calibration 8.2.1 Tuning After starting up, firstly check the performance of the portable gas chromatograph-mass spectrometer (5.3) according to the instrument manual. to guarantee For the accuracy of the test results, after the startup, the mass spectrometer function should be tuned. use request. Every 12 hours, the mass spectrometer function should be retuned. If the tuning substances are 1,3,5-tris(trifluoromethyl)benzene and bromopentafluorobenzene, then The abundance of key ions should meet the requirements of Table 1; if the tuning substance is perfluorotributylamine, the abundance of key ions should meet the requirements of Table 2, otherwise The parameters of the mass spectrometer should be adjusted; if other substances are used for tuning, the relevant requirements of the instrument manual should be met. 8.2.2 Plotting the calibration curve 8.2.2.1 Prefabricated calibration curve In the laboratory, dilute the standard gas (4.1) with nitrogen gas (4.4) by means of a gas diluter (5.7), or use the static dilution method (see appendix). Record B) Preparation of standard gas, prepared into low and high concentration series. Low concentration series are 2.0 nmol/mol, 5.0 nmol/mol, 10.0 nmol/mol, 25.0 nmol/mol, 50.0 nmol/mol (100 ml injection volume, splitless; or 600 ml injection volume, split ratio 50.1); high concentration series are 50.0 nmol/mol, 100 nmol/mol,.200 nmol/mol, 400 nmol/mol, 600 nmol/mol (in The sample volume is 5 ml, splitless; or the injection volume is 25 ml, the split ratio is 50.1), and the concentration series can be adjusted according to the actual sample conditions. According to the meter The instrument reference conditions (8.1) are measured sequentially from low concentration to high concentration, and the calibration curve is drawn and stored in the instrument. At the emergency monitoring site, If the calibration complies with the relevant requirements in 11.3, use a pre-made calibration curve for quantification. 8.2.2.2 Field calibration At the emergency monitoring site, if the calibration does not meet the relevant requirements in 11.3, the site standard gas (4.2) should be used for single-point calibration. At this time, the zero crossing should be forced. Note. When 1,3,5-tris(trifluoromethyl)benzene and bromopentafluorobenzene (4.3) were used as internal standard compounds, the added amount of internal standard compounds was 20 μl, and 1,3,5-tris(4.3) was used as the internal standard compound. three When fluoromethyl)benzene and 4-bromofluorobenzene (4.3) were used as internal standard compounds, the added amount of internal standard compounds was 600 μl. 8.2.3 Average relative response factor method The relative response factor (RRFi) of a target compound at point i in the standard series is calculated according to formula (1). 8.2.4 Calibration curve method Taking the concentration of the target compound as the abscissa, taking the ratio of the quantitative ion response value of the target compound to the quantitative ion response value of the internal standard compound The product of the value and the concentration of the internal standard compound is the ordinate, and a calibration curve is established. 8.3 Sample concentration prediction Before the sample measurement, the quick-check method, sample dilution or other methods specified in the instrument manual, combined with the on-site investigation situation, should be used to predict. sample concentration. 8.4 Determination of samples Collect the sample directly with the gas sampling module or connect the gas bag (5.2) to the gas sampling module, in accordance with the reference conditions of 8.1 and the sample in 8.3 According to the result of the pre-judgment of the concentration of the product, select the appropriate injection volume for the determination. 8.5 Blank test Carry out the determination of the blank sample (7.2) according to the same conditions and steps as the sample determination.

9 Result calculation and presentation

9.1 Target compounds 9.1.1 Qualitative Analysis By comparing the retention time, fragment ion mass-to-charge ratio and its abundance ratio of the target in the sample and the target in the standard series, the target The target is qualitative. The retention time of the target compound in the sample should be controlled within t±3S, where t is the target of each concentration level during the initial calibration. The mean value of the retention time of the target compound, S is the standard deviation of the retention time of the target compound at each concentration level during the initial calibration. target compound All ions with relative abundance higher than 30% in the quasi-mass spectrum should be present in the sample mass spectrum, and qualitative judgment should be made in combination with the on-site situation. Such as If the actual sample has obvious background interference, the background influence should be deducted when comparing. 9.1.2 Quantitative analysis Quantitative calculations were performed using the calibration curve method or the average relative response factor method. When the quantitative ion of the target compound in the sample interferes, Auxiliary ions can be used for quantification. See Appendix D for quantitative ions and auxiliary ions. 9.1.3 Result calculation 9.1.3.1 Average Relative Response Factor Method When calculated by the average relative response factor method, the mass concentration 𝜌𝑥 of the target compound in the sample is calculated according to formula (3). 9.1.3.2 Calibration curve method When the target compound is calibrated using a linear calibration curve, the mass concentration 𝜌𝑥 of the target compound in the sample is calculated according to formula (4). 9.2 Off-target compounds 9.2.1 Qualitative Analysis Perform the determination in full scan mode, compare the mass spectrum of the sample with the mass spectrum of the standard material in the library, and the relative abundance in the mass spectrum of the standard material in the library All ions above 30% should be present in the sample mass spectrum, the signal-to-noise ratio of qualifier ions should be greater than 3.1, primary qualifier ions and secondary qualifiers The ion peak apex of the ion should be maximally co-elute in the same scan segment. According to information such as mass spectrum and spectral library matching degree, combined with the actual situation on site The qualitative results of the samples were obtained by judging the condition. 9.2.2 Concentration estimation Integrate the chromatographic peaks of the total ion chromatogram of the qualitative target external compound and internal standard in the sample, and the mass of the target external compound is concentrated. The degree ρx is estimated according to formula (5). 9.3 Result representation The number of decimal places in the determination result is consistent with the detection limit of the method, and a maximum of 3 significant figures are reserved. For non-target compounds, original information such as mass spectrum and search results should be attached to the qualitative results. 10 Accuracy 10.1 Precision Actual samples spiked at 5.0 nmol/mol, 25.0 nmol/mol, 45.0 nmol/mol, and.200 nmol/mol by six laboratories The precision of the products was measured, and the relative standard deviations in the laboratory ranged from 2.2% to 25%, 1.1% to 24%, 0.6% to 14% and 1.0% to 1.0%. 13%; interlaboratory relative standard deviations were 4.1%-32%, 3.5%-20%, 2.9%-24%, 2.5%-28%; repeatability limit 3.3 μg/m3～20 μg/m3, 17 μg/m3～70 μg/m3, 19 μg/m3～1.3×102 μg/m3, 34 μg/m3～4.3×102 μg/m3; The current limit is 4.7 μg/m3～36 μg/m3, 21 μg/m3～1.5×102 μg/m3, 26 μg/m3～1.4×102 μg/m3, 1.4×102 μg/m3～ 7.8×102 μg/m3.See Table E.1 in Appendix E. 10.2 Correctness 6 labs replicated 6 actual samples for samples spiked at 5.0 nmol/mol, 45.0 nmol/mol,.200 nmol/mol The recovery rate of standard addition was determined, and the recovery rate of standard addition ranged from 86.5% to 107%, 92.7% to 105%, and 94.3% to 106%; The final values were 98.6%±36.2%, 100%±27.0%, 99.0%±33.0%, respectively. See Table E.2 in Appendix E. 11 Quality Assurance and Quality Control 11.1 One blank sample (7.2) should be analyzed for every 20 samples or batches (≤20 samples), and the target compound in the blank sample should be analyzed. The concentration of the substance should be less than the lower limit of method determination. Note. If the above conditions are not met, the concentration of the target compound in the blank sample should be less than 10% of the standard limit, otherwise measures should be taken to eliminate contamination and re-sample Analyze the same batch of samples. 11.2 During calibration curve verification and sample testing, the retention time of the internal standard and the internal standard at the midpoint of the calibration curve should not change by more than 10 s, and the quantitative ion The peak area variation was between 60% and 140%. 11.3 Before quantitative analysis, use the sample at the midpoint of the calibration curve for calibration check, and the relative error of the target component determination results should be Within ±30%; in continuous measurement, analyze the intermediate concentration point of the calibration curve every 12 h, and the relative error between the measurement result and the standard value Should be within ±30%. Otherwise, a single point calibration shall be carried out in accordance with 8.2.2.2. 12 Waste Disposal Expired standard gas should be entrusted to a qualified unit for recycling and disposal according to law. 13 Notes 13.1 During emergency monitoring of environmental emergencies, on-site personnel shall take necessary protective measures to ensure personal safety. 13.2 Portable gas chromatograph-mass spectrometers should not be used in explosive atmospheres. 13.3 After analyzing a high-level sample, at least one blank sample should be analyzed to check for system residues. If system residues occur, bake out Appropriate measures such as instrument pipelines should be taken to confirm that there is no system residue before continuing the test.

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