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HJ 1042-2019 English PDF

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HJ 1042-2019: Ambient air and waste gas - Determination of trimethylamine - Solvent absorption-Headspace/gas chromatography
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HJ 1042-2019	English	299	Add to Cart	3 days [Need to translate]	Ambient air and waste gas - Determination of trimethylamine - Solvent absorption-Headspace/gas chromatography	Valid	HJ 1042-2019

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Basic data

Standard ID	HJ 1042-2019 (HJ1042-2019)
Description (Translated English)	Ambient air and waste gas - Determination of trimethylamine - Solvent absorption-Headspace/gas chromatography
Sector / Industry	Environmental Protection Industry Standard
Classification of Chinese Standard	Z15
Classification of International Standard	13.040.20
Word Count Estimation	13,187
Date of Issue	2019
Date of Implementation	2020-04-29
Issuing agency(ies)	Ministry of Ecology and Environment

HJ 1042-2019: Ambient air and waste gas - Determination of trimethylamine - Solvent absorption-Headspace/gas chromatography

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(Ambient air and exhaust gas Determination of trimethylamine Solution absorption-headspace/gas chromatography) National Environmental Protection Standard of the People's Republic of China Determination of trimethylamine in ambient air and exhaust gas Solution absorption-headspace/gas chromatography Ambient air and waste gas-Determination of trimethylamine -Solvent absorption-Headspace/gas chromatography 2019-10-24 released 2020-04-24 Implementation Released by the Ministry of Ecology and Environment

Foreword ... ii 1 Scope ... 1 2 Normative references ... 1 3 Methodology ... 1 4 Interference and cancellation ... 1 5 Reagents and materials ... 2 6 Instruments and equipment ... 2 7 Sample ... 3 8 Analysis steps ... 5 9 Calculation and Representation of Results ... 7 10 Precision and accuracy ... 8 11 Quality Assurance and Quality Control ... 8 12 Notes ... 9 13 Waste disposal ... 9

Foreword

In order to implement the Law of the People's Republic of China on Environmental Protection and the Law of the People's Republic of China on the Prevention and Control of Atmospheric Pollution, Environment, protect human health, standardize the determination method of trimethylamine in ambient air and exhaust gas from fixed pollution sources, and develop this standard. This standard specifies the gas chromatography method for the determination of trimethylamine in ambient air and exhaust gas from stationary sources. This standard is issued for the first time. This standard is formulated by the Department of Eco-Environmental Monitoring, Laws and Standards Department of the Ministry of Ecology and Environment. This standard was drafted. Shandong Ecological Environment Monitoring Center. Verification units of this standard. Tianjin Ecological Environment Monitoring Center, Shandong Jinan Ecological Environment Monitoring Center, Shandong Province Fang Ecological Environment Monitoring Center, Shandong Provincial Product Quality Inspection Research Institute, Shandong Ante Testing Co., Ltd. and Shandong Yiwei Testing Ltd. This standard was approved by the Ministry of Ecology and Environment on October 24,.2019. This standard will be implemented from April 24, 2020. This standard is explained by the Ministry of Ecology and Environment. Determination of ambient air and exhaust gas trimethylamine. Solution absorption-headspace/gas chromatography Warning. The hydrochloric acid and ammonia used in the experiment are strongly irritating and corrosive. The reagent preparation process should be in a fume hood Protective equipment should be worn during operation to avoid breathing into the respiratory tract and contact with skin and clothing.

1 Scope

This standard specifies the solution absorption-headspace/gas chromatography method for the determination of trimethylamine in ambient air and exhaust gas from stationary sources. This standard applies to trimethylamine in ambient air, air from fugitive emission monitoring points of fixed pollution sources, and organized exhaust emissions. Determination. When using a hydrogen flame ionization detector, when the air sampling volume is 20 L (reference state), the absorption liquid volume is 10 ml The detection limit of the method is 0.004 mg/m3, and the lower detection limit is 0.016 mg/m3. When the exhaust gas sampling volume is 20 L (standard When the volume of the absorption solution is 50 ml, the detection limit of the method is 0.04 mg/m3, and the lower limit of determination is 0.16 mg/m3. When using a nitrogen and phosphorus detector, when the air sampling volume is 20 L (reference state) and the absorption liquid volume is 10 ml, the square The detection limit of the method is 0.0007 mg/m3, and the lower detection limit is 0.0028 mg/m3. When the exhaust gas sampling volume is 20 L (standard state), When the volume of the absorption solution is 50 ml, the detection limit of the method is 0.006 mg/m3, and the lower limit of determination is 0.024 mg/m3.

2 Normative references

This standard refers to the following documents or clauses therein. For undated references, the valid version applies to this standard. GB 14554 Emission Standard for Odor Pollutants GB/T 16157 Determination of particulate matter and sampling of gaseous pollutants in exhaust from stationary sources HJ 194 Technical Specifications for Manual Monitoring of Ambient Air Quality HJ 905 Technical Specification for Odor Pollution Environmental Monitoring HJ/T 55 Technical guidelines for fugitive emissions monitoring of air pollutants HJ/T 397 Fixed source exhaust gas monitoring technical specifications

3 Method principle

After the trimethylamine in the ambient air and the exhaust gas is absorbed by the dilute acid, the absorption liquid is transferred to the headspace bottle and treated with alkali. In a At a fixed temperature, trimethylamine in the sample volatilizes into the liquid space. After the two phases of gas and liquid reach thermodynamic equilibrium, the Methylamine concentration is directly proportional to the concentration in the liquid phase. Separated by gas chromatography with hydrogen flame ionization detector/nitrogen phosphorus detector Detection. Qualitatively based on retention time of chromatographic peaks and quantified by external standard method.

4 Interference and cancellation

Under the analytical conditions recommended by this method, ammonia, methylamine, dimethylamine, ethylamine, diethylamine, and triethylamine can all be combined with trimethylamine Achieve effective separation without disturbing the determination.

5 Reagents and materials

Unless otherwise specified, analytical reagents that meet national standards are used. Experimental deionized water Water or distilled water. 5.1 Sulfuric acid. ρ (H2SO4) = 1.84 g/ml, excellent purity. 5.2 Hydrochloric acid. ρ (HCl) = 1.189 g/ml, excellent grade pure. 5.3 Sodium hydroxide (NaOH). super pure. 5.4 Sodium chloride (NaCl). Burn in a muffle furnace at 400 ° C for 4 h before use, cool in a desiccator to room temperature, and transfer Store in ground glass bottle. 5.5 Potassium sulfate (K2SO4). Burn at 450 ° C for 4 h in a muffle furnace before use, cool in a desiccator to room temperature, and turn Move to a ground glass bottle for storage. 5.6 Ammonia water. ρ (NH3 · H2O) = 0.91 g/ml. 5.7 Trimethylamine hydrochloride. w (CH3) 3N · HCl) ≥98%. 5.8 Absorption liquid. One of the following two absorption liquids can be used. 5.8.1 Sulfuric acid absorption solution. c (H2SO4) = 0.06 mol/L. Transfer 3.2 ml of sulfuric acid (5.1), slowly add an appropriate amount of water, cool and dilute to a 1000 ml volumetric flask. uniform. Provisional use. 5.8.2 Hydrochloric acid absorption solution. c (HCl) = 0.12 mol/L. Take 10.0 ml of hydrochloric acid (5.2), slowly add an appropriate amount of water, cool and dilute to a 1000 ml volumetric flask. Mix well. Provisional use. 5.9 Sodium hydroxide solution. w (NaOH) = 50%. Weigh 50 g of sodium hydroxide (5.3) and dissolve in 50 ml of water. 5.10 Trimethylamine standard stock solution. ρ (TMA) = 100 mg/L. Accurately weigh 0.1620 g of trimethylamine hydrochloride (5.7), dissolve by taking 10.00 ml of absorbent solution (5.8), and determine the volume to 1000 ml. Refrigerated below 4 ° C can be stored for one month. 5.11 Trimethylamine standard solution. ρ (TMA) = 1.00 mg/L. Accurately transfer 1.00 ml of trimethylamine standard stock solution (5.10) into a 100 ml volumetric flask. Dilute with absorbing solution (5.8). Release to scale. Refrigerated below 4 ° C can be stored for one month. 5.12 Nitrogen. Purity ≥99.999%. 5.13 Hydrogen. purity ≥99.99%. 5.14 Air. air degassed by silica gel dehumidification and dehydrocarbonation tube or oil-free compressed air purified by 5A molecular sieve 5.15 Polytetrafluoroethylene or quartz filter membrane. The retention efficiency of particles with a particle size larger than 0.3 μm is not less than 99.9%.

6 Instruments and equipment

6.1 Flue gas sampler. The flow range is 0.1 L/min ～ 2.0 L/min. The sampling tube is made of hard glass or fluororesin. It is equipped with heating and heat preservation function. The heating temperature is ≥120 ℃. Other performance and technical indicators should meet the requirements of HJ/T 397. 6.2 Air sampler. flow range 0.1 L/min ～ 1.0 L/min, other performance and technical indicators should comply with HJ/T 194 Regulations. 6.3 Filter clip. PTFE and other materials, the size matches the filter (5.15). 6.4 Bubble absorption bottles. 25 ml, 75 ml. 6.5 Gas chromatograph. with split/splitless inlet, equipped with hydrogen flame ionization detector (FID) and/or nitrogen and phosphorus detection Tester (NPD). 6.6 Quartz capillary column. 30 m × 0.32 mm × 5.0 μm, 100% dimethylpolysiloxane (requires alkaline deactivation) Or other equivalent columns. 6.7 Headspace sampler. The heating temperature control range is from room temperature to.200 ° C; the temperature control accuracy is ± 1 ° C. 6.8 Headspace bottle. 22 ml, glass material, Teflon-coated gasket, sealing cap. 6.9 Instruments and equipment commonly used in general laboratories.

7 samples

7.1 Sample collection 7.1.1 Air samples Arrangement, sampling frequency and sampling of air sampling points for ambient air samples and fugitive emission monitoring points of fixed pollution sources The operation is performed in accordance with the relevant regulations of HJ 194, HJ 905 and HJ/T 55. After the sampling device, two 25 ml bubble absorption bottles (6.4) each containing 10.0 ml of absorption liquid (5.8) were connected in series, and samples were taken with air. The device (6.2) continuously samples for at least 20 minutes at a flow rate of 0.5 L/min to 1.0 L/min. 7.1.2 Exhaust gas samples Determination of sampling locations and sampling points for exhaust gas monitoring of fixed pollution sources, determination of exhaust parameters and sampling operations The relevant regulations of GB 14554, GB/T 16157, HJ 905 and HJ/T 397 are implemented. The sampling device is shown in Figure 1. After the sampling device, two 75 ml bubble absorption bottles (6.4) each containing 50.0 ml of absorption liquid (5.8) are connected in series, and the pipeline is connected It should be as short as possible. According to the gaseous pollutant collection method, use a flue gas sampler (6.1) at a flow rate of 0.5 L/min ～ 1.0 L/min Continuous sampling for at least 20 min. When sampling, heat and keep the sampling tube at 120 ° C to avoid condensation of water vapor before the absorption bottle. Flow measurement and control device Sampling tube with heating device Absorption fluid Exhaust pipe Three-way valve Bypass absorption bottle Three-way valve Figure 1 Sampling diagram of exhaust gas sample 7.1.3 Full Program Blank Bring the absorption bottle with the same batch of absorption liquid (5.8) to the sampling site, not connected to the sampler, and take it Back to the laboratory for testing. 7.2 Sample preservation The analysis should be completed as soon as possible after the sample is collected, otherwise it should be sealed and refrigerated and stored below 4 ° C, and the analysis should be completed within 7 days. 7.3 Sample preparation 7.3.1 Air sample Transfer the sample solution (7.1.1) in two absorption bottles into two 10 ml colorimetric tubes, and use the appropriate amount of absorption solution (5.8) The inner wall of the absorption bottle was washed, and the rinse solution was transferred into the colorimetric tube, and the volume was adjusted to the scale, and each of them was transferred into the headspace bottle (6.8). Weigh 3.2 g of sodium chloride (5.4) and 1.0 g of potassium sulfate (5.5) into the headspace bottle (6.8). 10.00 ml of solution was transferred into a headspace bottle. Add 500 μl sodium hydroxide solution (5.9) and 100 μl ammonia water (5.6), immediately Seal the headspace bottle and shake gently until the salt is dissolved. When adding ammonia and sodium hydroxide solution, it should be placed on the bottom of the headspace bottle to avoid the target Loss of compounds. 7.3.2 Exhaust gas sample Transfer the sample solution (7.1.2) in two absorption bottles into two 50 ml colorimetric tubes, and use the appropriate amount of absorption solution (5.8) Wash the inner wall of the absorption bottle, transfer the rinse solution into the colorimetric tube, make up to the mark, and transfer 10.00 ml of the absorption solution to the top. Empty bottle (6.8). The remaining steps are the same as 7.3.1. 7.3.3 Full Procedure Blank Sample The entire program blank (7.1.3) is prepared according to the same steps as the air sample (7.3.1) and the exhaust gas sample (7.3.2). 7.4 Preparation of laboratory blank samples Take 10.00 ml of the same batch of absorbent solution (5.8) instead of the sample and prepare according to the same steps as the sample preparation (7.3).

8 Analysis steps

8.1 Instrument Reference Conditions 8.1.1 Headspace Sampler Reference Conditions Heating equilibration temperature. 80 ℃; heating equilibration time. 30 min; sampling needle temperature. 110 ℃; transmission line temperature. 115 ℃; Injection volume. 1 ml. 8.1.2 Reference conditions of gas chromatography hydrogen flame ionization detector Inlet temperature..200 ° C; Injection method. split injection, split ratio 10. 1; column flow rate. 1.0 ml/min; program liter Temperature. 65 ° C for 5 min, rise to.200 ° C at a rate of 10 ° C/min; detector temperature. 250 ° C, hydrogen flow. 30 ml/min, Air flow. 300 ml/min, makeup air flow. 30 ml/min. 8.1.3 Reference conditions for gas chromatography nitrogen and phosphorus detectors Inlet temperature..200 ° C; Injection method. split injection, split ratio 10. 1; column flow rate. 1.0 ml/min; program liter Temperature. 65 ° C for 5 min, rise to.200 ° C at a rate of 10 ° C/min; detector temperature. 300 ° C, hydrogen flow. 3 ml/min, Air flow. 60 ml/min, makeup air flow. 30 ml/min. 8.2 Establishment of working curve 8.2.1 Hydrogen flame ionization detector Take an appropriate amount of trimethylamine standard solution (5.11) and dilute with an appropriate amount of absorbent solution (5.8) to prepare at least 5 concentrations. Point standard series, the mass concentrations of trimethylamine are 0.020 mg/L, 0.050 mg/L, 0.200 mg/L, 0.500 mg/L, 1.00 mg/L (this concentration is the reference concentration), and analyzed on the machine after treatment according to 7.3. According to the instrument reference conditions (8.1) Determination. Inject the samples in descending order of concentration, with the concentration of the standard series (mg/L) as the abscissa and the corresponding The peak area of the chromatographic peak is the ordinate, and a working curve is established. 8.2.2 Nitrogen and phosphorus detector Take an appropriate amount of trimethylamine standard solution (5.11), dilute with an appropriate amount of absorbent solution (5.8), and prepare at least 5 concentrated For the standard series of degree points, the mass concentrations of trimethylamine are 0.005 mg/L, 0.020 mg/L, 0.050 mg/L, 0.500 mg/L, 1.00 mg/L (this concentration is the reference concentration), and analyzed on the machine after treatment according to 7.3. According to the instrument reference conditions (8.1) Determination. Inject the samples in descending order of concentration, with the concentration of the standard series (mg/L) as the abscissa and the corresponding The peak area of the chromatographic peak is the ordinate, and a working curve is established. 8.2.3 Standard reference chromatogram Under the instrument reference conditions (8.1) given in this standard, reference chromatograms containing trimethylamine are shown in Figures 3 and 4. 1-air peak; 2-ammonia; 3-methylamine (25 mg/L); 4-dimethylamine (10 mg/L); 5-ethylamine (20 mg/L); 6-trimethylamine (0.80 mg/L); 7 -Diethylamine (0.80 mg/L); 8-triethylamine (0.80 mg/L). Figure 3 Reference chromatogram with trimethylamine (hydrogen flame ionization detector) 1-air peak; 2-methylamine (25 mg/L); 3-dimethylamine (10 mg/L); 4-ethylamine (8.0 mg/L); 5-trimethylamine (0.50 mg/L); 6-Diethyl Amine (0.25 mg/L); 7-triethylamine (0.25 mg/L). Figure 4 Reference chromatogram with trimethylamine (nitrogen and phosphorus detector) 8.3 Sample determination Make the measurement according to the same instrument reference conditions (8.1) as the working curve. 8.4 Blank test Perform the measurement in accordance with the same procedures as the sample measurement (8.3) and the instrument reference conditions.

9 Calculation and representation of results

9.1 Qualitative analysis Characterize by the retention time of the target compound. 9.2 Result calculation 9.2.1 Air samples Calculate the concentration of trimethylamine in the air sample according to formula (1). (1) Where. ρ-the concentration of trimethylamine in the air sample, mg/m 3; ρ1- the concentration of the sample solution in the first absorption bottle, mg/L; ρ2-the concentration of the sample solution in the second absorption bottle, mg/L; Vt-volume of sample to be tested, ml; D-sample dilution factor; Vs-Sampling volume in standard or reference state (298.15 K, 101.325 kPa), L. 9.2.2 Exhaust gas samples Calculate the concentration of trimethylamine in the exhaust gas sample according to formula (2). (2) Where. ρ-the concentration of trimethylamine in the exhaust gas sample, mg/m 3; ρ1- the concentration of the sample solution in the first absorption bottle, mg/L; ρ2-the concentration of the sample solution in the second absorption bottle, mg/L; Vt-volume of sample to be tested, ml; D-sample dilution factor; Vnd-Sampling volume of dry flue gas under standard conditions, L. 9.3 Representation of results The number of digits after the decimal point of the measurement result is consistent with the method detection limit, but a maximum of 3 significant digits is retained. 10 Precision and accuracy 10.1 Precision Six laboratories performed 6 parallel determinations of 3 different concentrations of spiked samples. When using a FID detector, The spiked concentrations were 0.025 mg/m3, 0.100 mg/m3, and 1.50 mg/m3, respectively. The standard deviations are 2.9% to 8.0%, 1.1% to 7.2%, 1.3% to 6.9%, and the relative standard deviations between laboratories are 8.2%, 4.6%, 5.1%, with repeatability limits of 0.040 mg/m3, 0.014 mg/m3, and 0.13 mg/m3, respectively. Others are 0.0071 mg/m3, 0.019 mg/m3, and 0.26 mg/m3; when the NPD detector is used, the spiked concentrations are. 0.010 mg/m 3. 0.025 mg/m3 and 1.50 mg/m3, measured after simulated sampling, the relative standard deviations in the laboratory are respectively It is 4.2% to 18%, 2.0% to 7.6%, 1.2% to 7.0%, and the relative standard deviations between laboratories are 7.9%, 7.9%, and 5.4%. Repeatability limits are 0.0030 mg/m3, 0.0044 mg/m3, and 0.13 mg/m3, respectively. Reproducibility limits are 0.0035 mg/m3, 0.0072 mg/m 3. 0.26 mg/m3. Six laboratories prepared standard gas samples with concentrations of 0.538 mg/m3 and 5.38 mg/m3 in six groups, respectively. Determined after sampling. When using FID detectors, the relative standard deviations in the laboratory are 1.4% ～ 7.4% and 2.8% ～ 7.3%, the relative standard deviations between laboratories were 3.5% and 4.2%, and the repeatability limits were 0.0069 mg/m3 and 0.071 mg/m 3, the reproducibility limits are 0.0079 mg/m3 and 0.088 mg/m3 respectively; when using NPD detector, the experiment The indoor relative standard deviations were 1.7% to 11% and 2.2% to 8.8%, and the relative standard deviations between laboratories were 7.3% and 5.9%, repeatability limits are 0.0093 mg/m3 and 0.071 mg/m3, and reproducibility limits are 0.014 mg/m3 and 0.12 mg/m 3. 10.2 Accuracy Six laboratories performed 6 parallel determinations of 3 different concentrations of spiked samples. When the FID detector is used, the spiked concentrations are 0.025 mg/m3, 0.100 mg/m3, and 2.00 mg/m3, respectively. After the intended sampling, the recovery of trimethylamine ranges from 96.7% to 100%, 97.3% to 105%, and 97.0% to 102%; The final recoveries were 98.6 ± 2.8%, 101 ± 5.4%, and 98.7 ± 3.6%. When an NPD detector is used, the spiked concentrations are 0.010 mg/m3, 0.050 mg/m3, and 2.00 mg/m3, respectively. The range of recovery of trimethylamine after simulated sampling was 98.3% ～ 118%, 97.2% ～ 108% and 97.7% ～ 102%; the final recoveries were 104 ± 15%, 101 ± 8.0%, and 99.4 ± 3.2%. 11 Quality Assurance and Quality Control 11.1 At least one laboratory blank and full procedure blank should be made for every 20 samples or batches (≤20 samples) The concentration of the target compound in the blank sample should be lower than the detection limit of the method. 11.2 A working curve shall be established for each batch of samples. Correlation coefficient of working curve ≥ 0.995, otherwise you should find the cause or re-establish Working curve. 11.3 Analyze the standard solution at the middle concentration point of the working curve every 20 samples or each batch (≤20 samples). The relative error between the measured result and the initial curve at this point should be within ± 20%. 11.4 The trimethylamine content in the second absorption bottle should be less than 10% of the total trimethylamine sample, otherwise the sample should be collected again. 12 Notes 12.1 The results shall be calculated according to the conditions required by the corresponding quality standards or emission standards. 12.2 The connection lines between the headspace sampler and the gas chromatograph should be all heated and insulated to ensure that there is no cold point. 12.3 Pure water samples should be added at the end of each batch of sample analysis sequence for headspace and connection pipeline cleaning to avoid headspace Blocked needle and six-way valve. 13 Waste treatment The waste liquid generated in the experiment should be collected separately, and processed safely according to the requirements or entrusted to a qualified unit for processing.

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