HJ 1219-2021 English PDF

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HJ 1219-2021: Ambient air and waste gas - Determination of pyridine - Gas chromatography method
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Basic data

Standard ID: HJ 1219-2021 (HJ1219-2021)
Description (Translated English): Ambient air and waste gas - Determination of pyridine - Gas chromatography method
Sector / Industry: Environmental Protection Industry Standard
Word Count Estimation: 10,158
Issuing agency(ies): Ministry of Ecology and Environment

HJ 1219-2021: Ambient air and waste gas - Determination of pyridine - Gas chromatography method

---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 and waste gas Determination of pyridine Gas chromatography) National Ecological Environment Standard of the People's Republic of China Determination of pyridine in ambient air and waste gas gas chromatography Ambient air and waste gas-Determination of pyridine -Gas chromatography method 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 2022-06-01 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 Interference and cancellation...1 5 Reagents and materials...1 6 Instruments and equipment...2 7 Samples...2 8 Analysis steps...4 9 Result calculation and representation...5 10 Accuracy...6 11 Quality Assurance and Quality Control...6 12 Waste Disposal...7 Determination of pyridine in ambient air and waste gas by gas chromatography Warning. The solvents and reagents used in the experiment have certain toxicity. The preparation of standard solutions and sample pretreatment should be carried out in a fume hood. When operating, wear protective equipment as required to avoid direct contact with skin and clothing.

1 Scope of application

This standard specifies a gas chromatography method for the determination of pyridine in ambient air and exhaust gas. This standard is applicable to the determination of pyridine in ambient air, the air of fugitive emission monitoring points and the organic emission of fixed pollution sources. When collecting ambient air and fugitive emission monitoring point air, the sampling volume is 30 L, and the constant volume of absorption liquid is 10 ml, the method is checked. The output limit is 0.02 mg/m3, and the lower limit of determination is 0.08 mg/m3; when collecting the organized waste gas from fixed pollution sources, the sampling volume is 30 L. The detection limit of the method was 0.09 mg/m3 and the lower limit of determination was 0.36 mg/m3 when the volume of the collected liquid was 50 ml.

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 16157 Sampling method for particulate matter and gaseous pollutants in exhaust gas from stationary pollution sources HJ/T 55 Technical guidelines for monitoring fugitive emissions of air pollutants HJ 194 Technical Specification for Manual Monitoring of Ambient Air Quality HJ/T 397 Technical Specification for Stationary Source Waste Gas Monitoring

3 Principles of the method

The pyridine in ambient air and waste gas is absorbed by the acid absorption liquid, and the absorption liquid is placed in a sealed headspace bottle. Under alkaline conditions, the headspace The pyridine in the sample in the bottle volatilizes into the head space to generate vapor pressure, and the thermodynamic dynamic equilibrium is achieved in the gas-liquid two-phase. Quantitative extraction of gas phase fraction Separation by gas chromatography, hydrogen flame ionization detector detection. Qualitatively based on retention time, quantified by external standard method of working curve.

4 Interference and cancellation

Under the experimental conditions specified in this method, some of the volatile organic compounds in the sample absorbed by the sulfuric acid absorption solution may interfere with the determination. Interferences were removed by separation using columns of different polarities.

5 Reagents and Materials

Unless otherwise stated, analytical reagents that meet national standards are used in the analysis, and the experimental water is newly prepared water without organic matter. 5.1 Pyridine (C5H5N). The purity should be ≥99.5%, and it should be stored in a refrigerator away from light. 5.2 Sulfuric acid. ρ=1.84 g/ml, excellent grade. 5.3 Sodium hydroxide (NaOH). flake, excellent grade pure. 5.4 Sodium chloride (NaCl). heated at 400 ℃ for 4 h, and then transferred to a ground glass bottle after being slightly cooled, and stored in a desiccator. 5.5 Sulfuric acid absorption solution. c(H2SO4)=0.1 mol/L. Pipette 5.4 ml of sulfuric acid (5.2) into 1 L of water and mix well. Ready to use. 5.6 Standard stock solution of pyridine. ρ(C5H5N)=10.0 mg/ml. Accurately weigh 0.250 g (accurate to ± 0.1 mg) of pyridine (5.1), transfer it to a 25 ml brown volumetric flask with a small amount of water, and determine with water. Make up to mark, shake well. Refrigerated below 4 ℃, sealed and protected from light, it can be stored for 2 months. You can also directly purchase certified standard solutions, refer to the standard certificate to save. 5.7 Pyridine standard solution. ρ(C5H5N)=1.00 mg/ml. Accurately pipette 1.00 ml of pyridine standard stock solution (5.6) into a 10 ml brown volumetric flask, dilute with water to the mark, and prepare as pyridine pyridine standard solution, refrigerated below 4 ℃, sealed and protected from light, it can be stored for 7 d. 5.8 Carrier gas. nitrogen, purity ≥99.999%. 5.9 Combustion gas. hydrogen, purity ≥99.99%. 5.10 Supporting gas. air, dehydrated by silica gel, dehydrated by activated carbon.

6 Instruments and equipment

6.1 Air sampler. the sampling flow range is 0.1 L/min ~ 1.0 L/min, other performance and technical indicators should comply with the provisions of HJ 194. 6.2 Flue gas sampler. the sampling flow range is 0.1 L/min ~ 1.0 L/min, the sampling tube is made of hard glass or fluororesin, and it should have heating and heat preservation function, the heating temperature of the sampling tube is not lower than 120 ℃, and other performance and technical indicators should comply with the provisions of HJ/T 397. 6.3 Connecting pipe. Teflon hose or silicone rubber pipe lined with Teflon film. 6.4 Cooling device. ice water bath. 6.5 Small multi-well glass plate brown absorption bottle. 25 ml. The absorption bottle should be tight and airtight, the foaming of the porous glass plate absorption bottle should be uniform, and other properties And technical indicators should comply with the provisions of HJ 194. 6.6 Large multiwell glass plate brown absorption bottle. 75 ml or larger volume multiwell glass plate brown absorption bottle. The absorption bottle should be tight and airtight, porous The foaming of the glass plate absorption bottle should be uniform, and other performance and technical indicators should comply with the provisions of HJ/T 397. 6.7 Gas chromatograph. with capillary column split/splitless injection port, with constant flow or constant pressure function, programmable temperature, with hydrogen flame ionization Chemical Detector (FID) and Workstation. 6.8 Chromatographic column. quartz capillary column, the stationary phase is cross-linked polyethylene glycol, 30 m × 0.25 mm × 0.5 m; or other equivalent capillary column. 6.9 Automatic headspace sampler. temperature control accuracy is ±1 °C, with headspace vial, sealing gasket (teflon/siloxane or teflon) /butyl rubber), caps (screw caps or disposable glands). 6.10 Analytical balance. the actual division value is 0.1 mg. 6.11 General laboratory instruments and equipment.

7 samples

7.1 Sample Collection 7.1.1 Ambient air and fugitive emission monitoring point air samples The air sampling of ambient air and fugitive emission monitoring points shall be carried out in accordance with the relevant regulations in HJ 194 and HJ/T 55.Air sampler (6.1) Airtightness check and flow calibration should be performed prior to use. Connect a 9 ml sulphuric acid absorbent (5.5) to the air sampler (6.1) 25 ml small multi-well glass plate brown absorption bottle (6.5), sample at a flow rate of about 0.5 L/min, and the sampling volume should be at least 30 L. 7.1.2 Samples of organic emissions from stationary pollution sources The sampling of waste gas from fixed pollution sources and organized emissions shall be carried out in accordance with the relevant regulations in GB/T 16157 and HJ/T 397.The sampling device is shown in Figure 1. Show. The flue gas sampler (6.2) shall be checked for air tightness and flow calibrated before use. Connect a built-in to the flue gas sampler (6.2) 75 ml brown absorption bottle (6.6) with 45 ml sulfuric acid absorption solution (5.5), sampling at a flow rate of about 0.5 L/min, sampling body The volume is at least 30 L. During the sampling process, the temperature of the insulation jacket of the sampling tube should be kept at 120 °C to avoid condensation of water vapor before the absorption bottle. At the same time use the cooling device (6.4) to cool the large multi-well glass plate brown absorption bottle (6.6). When collecting the same batch of samples, at least one absorption bottle should be connected in series to confirm whether there is penetration. The volume of the absorbing liquid should be appropriately increased according to the actual situation and the sampling time should be shortened when penetration occurs. 7.1.3 Full program blank At least one full-program blank should be included for each sample collection. Put the same batch of absorbing bottles (6.5 or 6.6) containing sulfuric acid absorbing solution (5.5) Take it to the sampling site, open its two ends, do not connect it with the sampler, and close it after 1 min. Under the same conditions as for sample transport and storage (7.2) Take it back to the lab. 7.2 Sample Shipping and Storage After sample collection, use connecting tube (6.3) to close the inlet and outlet of the brown absorption bottle (6.5 or 6.6) of the multi-well glass plate, and place it upright. Transport and storage in a refrigerated box. If it cannot be determined in time, the samples should be refrigerated, protected from light and sealed under 4 °C, and the analysis and measurement should be completed within 7 days. Certainly. 7.3 Preparation of test specimens 7.3.1 Ambient air and fugitive emission monitoring point air samples Transfer the whole volume of the ambient air and the air sample absorption solution of the fugitive emission monitoring point (the absorption solution collected in 7.1.1) into a 10 ml colorimetric tube , wash the small multi-well glass plate brown absorption bottle (6.5) with a small amount of sulfuric acid absorption solution (5.5), and transfer it to a 10 ml colorimetric tube. Dilute the acid absorption solution (5.5) to the 10 ml mark and shake well. In the headspace vial (6.9) add 3 g sodium chloride (5.4), 0.2 g sodium hydroxide (5.3), pour 10 ml of absorbing solution into the headspace bottle, seal and shake well until all the added salt is dissolved, and inject it into the automatic headspace sampler (6.9). sample, to be tested. 7.3.2 Samples of organic emissions from stationary pollution sources Transfer the entire amount of the absorbing liquid (the absorbing liquid collected in 7.1.2) of the waste gas sample discharged from the fixed pollution source into a 50 ml colorimetric tube, and use less Sulfuric acid absorption solution (5.5) to wash the large multi-well glass plate brown absorption bottle (6.6), and transfer it into a 50 ml colorimetric tube, use sulfuric acid absorption solution (5.5) Dilute to the 50 ml mark and shake well. Add 3 g of sodium chloride (5.4), 0.2 g of sodium hydroxide (5.3) to the headspace vial (6.9), Accurately measure 10 ml of the absorption solution and pour it into the headspace bottle, seal it and shake it well until all the added salt is dissolved, and inject the sample into the automatic headspace sampler (6.9). To be tested. 7.3.3 Full procedure blank sample Combine the full procedure blank sample (7.1.3) in accordance with the preparation (7.3.1) or solid state of the air sample sample for ambient air and fugitive emission monitoring points. The preparation of the sample of the waste gas from the organic emission of the fixed pollution source (7.3.2) is the same as the preparation of the blank sample of the whole procedure. 7.3.4 Laboratory blank sample Take 10 ml of the same batch of sulfuric acid absorption solution (5.5) instead of the sample, according to the air sample sample at the monitoring point of ambient air and fugitive emission The same procedure as the preparation (7.3.1) was used to prepare a laboratory blank.

8 Analysis steps

8.1 Instrument Reference Conditions 8.1.1 Headspace injection reference conditions Heating equilibrium temperature. 80 °C; heating equilibrium time. 30 min; injection valve temperature. 100 °C; transfer line temperature. 120 °C. other The parameters are set according to the instructions of the headspace sampler, and the gas circulation time is set according to the analysis time of the gas chromatography. 8.1.2 Reference conditions for chromatographic analysis Injection port temperature..200 °C; detector temperature. 250 °C; column temperature program. 40 °C (hold for 1 min), at 10 °C/min Warm up to 120 °C (hold for 1 min); flow rate of carrier gas (5.8). 1.0 ml/min; flow rate of combustion gas (5.9). 40 ml/min; (5.10) Flow rate. 450 ml/min; makeup gas flow rate. 30 ml/min; split ratio of 10.1. 8.2 Establishment of working curve 8.2.1 Air working curve of ambient air and fugitive emission monitoring points Measure an appropriate amount of the pyridine standard solution (5.7) and dilute it with an appropriate amount of sulfuric acid absorption solution (5.5) to prepare at least 5 concentration points of the standard solution. Standard series in a 25 ml volumetric flask. The mass concentrations of pyridine were 0.20 µg/ml, 0.50 µg/ml, 1.00 µg/ml, 2.00 µg/ml, 5.00 µg/ml. Add 3 g of sodium chloride (5.4), 0.2 g of sodium hydroxide (5.3) to the headspace vial (6.9), and accurately measure 10 ml of the standard solution To the headspace vial, seal and shake until all the added salt is dissolved. According to the instrument reference conditions (8.1), analyze and measure from low concentration to high concentration. Taking the pyridine concentration as the abscissa and the peak height or peak area as the ordinate, draw the working curve. 8.2.2 Working curve of organized emission of waste gas from fixed pollution sources Measure an appropriate amount of the pyridine standard solution (5.7) and dilute it with an appropriate amount of sulfuric acid absorption solution (5.5) to prepare at least 5 concentration points of the standard solution. Standard series in a 25 ml volumetric flask. The mass concentrations of pyridine were 5.00 µg/ml, 10.0 µg/ml, 20.0 µg/ml, 50.0 µg/ml, 100 µg/ml. Add 3 g of sodium chloride (5.4), 0.2 g of sodium hydroxide (5.3) to the headspace vial (6.9), and accurately measure 10 ml of the standard solution To the headspace vial, seal and shake until all the added salt is dissolved. According to the instrument reference conditions (8.1), analyze and measure from low concentration to high concentration. Taking the pyridine concentration as the abscissa and the peak height or peak area as the ordinate, draw the working curve. Under the reference conditions of this standard instrument, the reference chromatogram of pyridine is shown in Figure 2. 8.3 Sample Determination The samples (7.3.1 or 7.3.2) are tested according to the instrument reference conditions (8.1). 8.4 Blank test The full procedure blank (7.3.3) and laboratory blank (7.3.4) are measured according to the instrument reference conditions (8.1).

9 Result calculation and presentation

9.1 Qualitative Analysis According to the retention time of the standard chromatogram of pyridine. When the sample matrix is complex, another chromatographic column with different polarities should be used for dual-column characterization or mass spectrometry characterization. 9.2 Result calculation 9.2.1 Ambient air and fugitive emission monitoring point air samples The concentration of pyridine in ambient air and the air of fugitive emission monitoring points is calculated according to formula (1). Vff  (1) In the formula. ρ - the concentration of pyridine in the sample, mg/m3; ρf -- the concentration of pyridine found according to the working curve, µg/ml; Vf - volume of absorption solution, ml; D--dilution factor; V--sampling volume in the corresponding state according to the relevant quality standard or emission standard, L. 9.2.2 Samples of organic emissions from stationary pollution sources The concentration of pyridine in the organically emitted exhaust gas from stationary pollution sources is calculated according to formula (2). 9.3 Result representation The retention of the number of digits after the decimal point of the determination result is consistent with the detection limit of the method, and the retention of three significant figures at most. 10 Accuracy 10.1 Precision 6 laboratories carried out 6 parallel measurements on ambient air and exhaust gas samples of 0.50 mg/m3, 2.00 mg/m3 and 30.0 mg/m3, respectively. Certainly. The intra-laboratory relative standard deviations were. 4.8%-9.2%, 2.0%-8.3%, 2.9%-6.2%; inter-laboratory relative standard deviation Respectively. 13.1%, 4.6%, 8.3%; repeatability limits are. 0.10 mg/m3, 0.28 mg/m3, 3.48 mg/m3; repeatability limits are respectively As. 0.21 mg/m3, 0.35 mg/m3, 7.63 mg/m3. 10.2 Correctness The 6 laboratories respectively spiked the ambient air and the air (15.0 µg, 60.0 µg) of the ambient air and the air at the monitoring point of fugitive emissions, and the fixed pollution sources were Tissue emissions (900 µg) spiked samples were measured in 6 replicates. After simulated sampling, the recovery rates of pyridine spiked in the range of are. 86.7% to 117%, 91.9% to 104%, 87.6% to 112%; the final values of the spiked recoveries are. 106%±27.4%, 99.3% ±9.0%, 100% ±16.6%. 11 Quality Assurance and Quality Control 11.1 Blank For every 20 samples or batches (less than 20/batch), at least 1 laboratory blank and 1 full procedure blank should be analyzed For samples, it is required that the blank determination result should be lower than the detection limit of the method. If the measured value of pyridine in the blank sample analysis is higher than the detection limit of the method, the original due to, or resampling. 11.2 Calibration The correlation coefficient of the working curve should be ≥ 0.995. For every 20 samples or batches of samples (less than 20/batch), an intermediate concentration point of the working curve should be determined. The measurement result and the point The relative error of the concentration should be within ±20%, otherwise, redraw the working curve. 11.3 Blank Spike Recovery For every 20 samples or batches of samples (less than 20/batch), 1 blank spike should be determined, and the recovery rate of the blank spike should be in the range of 80%～ between 120%. 12 Waste Disposal All wastes generated in the experiment (including residual liquid after testing) should be classified and collected in airtight containers. It is required to entrust a qualified unit to handle it according to the law. ......

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