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Basic dataStandard ID: HJ 1040-2019 (HJ1040-2019)Description (Translated English): Stationary source emission - Determination of hydrogen bromide - Ion chromatography Sector / Industry: Environmental Protection Industry Standard Classification of Chinese Standard: Z25 Classification of International Standard: 13.040.40 Word Count Estimation: 12,168 Date of Issue: 2019 Date of Implementation: 2020-04-24 Issuing agency(ies): Ministry of Ecology and Environment HJ 1040-2019: Stationary source emission - Determination of hydrogen bromide - Ion chromatography---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. (Exhaust gas from stationary sources Determination of hydrogen bromide Ion chromatography) National Environmental Protection Standard of the People's Republic of China Determination of hydrogen bromide from stationary sources Ion chromatography Stationary source emission-Determination of hydrogen bromide -Ion chromatography 2019-10-24 released 2020-04-24 Implementation Released by the Ministry of Ecology and Environment ContentsForeword ... ii 1 Scope ... 1 2 Normative references ... 1 3 Terms and definitions ... 1 4 Methodology ... 1 5 Interference and cancellation ... 1 6 Reagents and materials ... 2 7 Instruments and equipment ... 2 8 Sample ... 3 9 Analysis steps ... 5 10 Calculation and Representation of Results ... 6 11 Precision and accuracy ... 7 12 Quality Assurance and Quality Control ... 8 13 Waste disposal ... 8 14 Notes ... 8ForewordIn order to implement the "Environmental Protection Law of the People's Republic of China" Environment, protect human health, standardize the determination method of hydrogen bromide in exhaust gas from fixed pollution sources, and formulate this standard. This standard specifies ion chromatography for the determination of hydrogen bromide in exhaust gas from stationary pollution 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 Island Ecological Environment Monitoring Center, Shandong Province Tai'an Ecological Environment Monitoring Center, Shandong Binzhou Ecological Environment Monitoring Center, Shandong Provincial Institute of Product Quality Inspection. 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 hydrogen bromide from exhaust gas from stationary sources. Ion chromatography WARNING. Hydrogen bromide is harmful to the human body. Samplers should pay attention to wearing protective equipment to avoid inhalation or contact with skin.1 ScopeThis standard specifies the determination of hydrogen bromide in the air from fixed sources of pollution, organized emissions and fugitive emissions monitoring points. Subchromatography. This standard is applicable to the determination of hydrogen bromide in the air of fixed pollution sources, organic emissions and fugitive emissions monitoring points. For organized exhaust, when the sample volume is 20 L (standard state) and the fixed volume is 50.0 ml, the method The detection limit was 0.05 mg/m3, and the lower detection limit was 0.20 mg/m3. For fugitive emission monitoring point air, when the sampling volume is 30 L (standard state) and the constant volume is 10.0 ml, The detection limit of the method was 0.008 mg/m3, and the lower detection limit was 0.032 mg/m3.2 Normative referencesThis standard refers to the following documents or clauses therein. For undated references, the valid version applies to this standard. GB/T 16157 Determination of particulate matter and sampling of gaseous pollutants in exhaust from stationary sources HJ/T 55 Technical guidelines for fugitive emissions monitoring of air pollutants HJ/T 397 Fixed source exhaust gas monitoring technical specifications3 terms and definitionsThe following terms and definitions apply to this standard. 3.1 Hydrogen bromide Hydrogen bromide determined by this standard refers to hydrogen bromide in the form of gaseous and mist droplets.4 Method principleFixed sources of pollution include organized emission of exhaust gas and fugitive emission of hydrogen bromide in the air at monitoring points, which are absorbed to form bromine Ions are separated by ion chromatography and detected by a conductivity detector. Qualitative based on retention time, quantitative peak height or area.5 Interference and cancellationParticulate bromide interferes with the measurement. Use PTFE or quartz filter to eliminate the interference. Gaseous bromine test There must be interference. The use of acidic absorption solution to absorb hydrogen bromide can eliminate the interference. Organic pollutants interfere with ion chromatography, Eliminate interference with activated solid phase extraction columns such as C18.6 Reagents and materialsUnless otherwise specified, analytical reagents that meet national standards are used. Experimental water is resistivity ≥18 MΩ · cm of fresh deionized water. 6.1 Sodium hydroxide (NaOH). excellent grade pure. 6.2 Potassium hydroxide (KOH). excellent grade pure. 6.3 Sulfuric acid. ρ (H2SO4) = 1.84 g/ml, excellent grade pure. 6.4 Potassium bromide (KBr). Excellent purity. Before use, it should be dried at 105 ° C ± 5 ° C for 2 hours, and placed in a desiccator for cooling. 6.5 Bromide stock solution. ρ (Br-) = 1000 mg/L. Weigh 1.4875 g of potassium bromide (6.4) and dissolve it in an appropriate amount of water. Transfer it to a 1000 ml volumetric flask. Move to a polyethylene bottle. It can be stored for 1 month in refrigerated, protected from light and sealed below 4 ° C. Commercially available certified standard solutions are also available. 6.6 Standard bromide solution. ρ (Br-) = 100 mg/L. Take 10.00 ml bromide stock solution (6.5), put it in a 100 ml volumetric flask, make up to volume with water, mix well, and use immediately Match. 6.7 Alkaline absorption solution. c (NaOH) = 35 mmol/L or c (KOH) = 35 mmol/L. Weigh 1.40 g of sodium hydroxide (6.1) or 1.96 g of potassium hydroxide (6.2), dissolve in an appropriate amount of water and transfer to a 1000 ml volume In a measuring flask, make up to volume with water, mix well, and transfer to a polyethylene bottle. Provisional use. 6.8 Sulfuric acid absorption solution. c (H2SO4) = 50 mmol/L. Take 2.7 ml of sulfuric acid (6.3), slowly add an appropriate amount of water, and after cooling, transfer it to a 1000 ml volumetric flask, and set it with water. Content, mix well and transfer to a polyethylene bottle. Refrigerated and sealed below 4 ℃ can be stored for 3 months. 6.9 Eluent stock solution. Prepare according to the model of the instrument and the operating conditions of the column. Refrigerated and sealed below 4 ℃ Save for 3 months. 6.10 Eluent. Dilute the eluent stock solution (6.9) to obtain the eluent. 6.11 Sodium hydroxide solution. c (NaOH) = 5.0 mol/L. Weigh 20.0 g of sodium hydroxide (6.1), dissolve in an appropriate amount of water, transfer to a 100 ml volumetric flask, make up to volume with water, mix well, Transfer to a polyethylene bottle. Refrigerated and sealed below 4 ℃ can be stored for 3 months. 6.12 Disposable microporous membrane syringe filter. pore size ≤0.45 μm. 6.13 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%.7 instruments and equipment7.1 Flue gas sampler. The sampling flow rate is 0.1 L/min ～ 1.0 L/min. The sampling tube is made of hard glass or fluororesin. Equipped with heating and heat preservation function, heating temperature ≥120 ℃. 7.2 Air sampler. The sampling flow is 0.1 L/min ～ 1.0 L/min. 7.3 Particle sampler. The sampling flow rate is 5 L/min ～ 50 L/min. The sampling tube is made of hard glass or fluororesin. Equipped with heating and heat preservation function, heating temperature ≥120 ℃. 7.4 Brown bubble absorption bottle. 25 ml, 75 ml. 7.5 Connection pipe. PTFE pipe or silicone rubber pipe lined with PTFE film. 7.6 Ion chromatograph. An analysis system consisting of an ion chromatograph host, operating software and required accessories. 7.7 Chromatographic column. anion separation column, particle size 5.5 μm, inner diameter 5 mm, column length 250 mm, polydivinylbenzene/ethyl Vinylbenzene/polyvinyl alcohol matrix (with alkyl quaternary ammonium or alkanol quaternary ammonium functional groups), or other equivalent high-capacity columns. 7.8 Syringe. 10 ml. 7.9 Pretreatment column. Silica matrix bonded C18 and other solid phase extraction columns. 7.10 Instruments and equipment commonly used in general laboratories.8 samples8.1 Sample collection 8.1.1 Organized emission sample Layout and sampling according to the relevant regulations of GB/T 16157 and HJ/T 397. The sampling device is shown in Figure 1. Two in series 75 ml brown bubble absorption bottle (7.4) containing 50.0 ml of alkaline absorption solution (6.7), connected to the flue gas sampler (7.1), According to the gaseous pollutant collection method, at a flow rate of 0.5 L/min ～ 1.0 L/min, sampling for 1 hour continuously, or within 1 hour, etc. Collect 3 to 4 samples at time intervals. Flow measurement and Control device Absorption fluid Full heating, temperature ≥120 ℃ Filter Exhaust pipe Fig. 1 Sampling schematic diagram of hydrogen bromide in organized exhaust gas Note 1. When the exhaust gas from a fixed pollution source contains bromine, four 75 ml brown bubble absorption bottles (7.4) are connected in series, and the first two are filled with 50 ml sulfuric acid absorption solution. (6.8), the last two are filled with 50 ml of alkaline absorption solution (6.7), and the first and second groups of absorption bottles absorb hydrogen bromide and bromine respectively. Note 2. When the moisture content in the exhaust gas from the fixed pollution source is relatively large, and the moisture absorption of hydrogen bromide exists in the form of mist droplets, the layout and sampling should comply with GB/T 16157 HJ/T 397 on the collection of particulate matter. The sampling device is shown in Figure 2. Two 50 ml alkaline absorbent solutions (6.7) in series 75 ml brown bubble absorption bottle (7.4), connected to the particulate sampler (7.3), and sampled according to the particulate collection method. Shunt Set the sampling flow rate of hydrogen bromide gas at 0.5 L/min ～ 1.0 L/min, and take samples continuously for 1 hour, or take samples at regular intervals within 1 hour. Set of 3 to 4 samples. When the exhaust gas from the fixed pollution source contains bromine interference, the absorption bottle is connected in series according to Note 1. Filter Particle sampling tube Absorption fluid Shunt device Full heating, temperature ≥120 ℃ Pitot tube Temperature, pressure and Humidity Sensor Flow measurement and Control device Exhaust pipe Fig. 2 Sampling diagram of hydrogen bromide in organized exhaust gas (with droplets) 8.1.2 Air samples at fugitive emission monitoring points Layout and sampling according to relevant regulations in HJ/T 55. When sampling, two 10 ml alkaline absorbents are connected in series. (6.7) 25 ml brown bubble absorption bottle (7.4), connected to the air sampler (7.2). 0.5 L/min ～ 1.0 L/min Flow rate, take 1 hour of continuous sampling, or collect 4 samples at equal time intervals within 1 hour. 8.1.3 Full program blank Bring the absorption bottle filled with the same batch of absorption liquid to the sampling site, not connected to the sampler, and bring it back to the laboratory after sampling To be tested. 8.2 Sample storage After the sample is collected, the absorption bottle is sealed with a connecting tube (7.5), refrigerated at 4 ° C, protected from light and stored in a sealed container for 24 hours. Analytical measurement is completed within. If the analysis cannot be performed in a timely manner, the sample should be transferred to a polyethylene bottle, refrigerated below 4 ° C, protected from light and Sealed for 14 days. 8.3 Preparation of test specimens 8.3.1 Organized emission sample Transfer the sample solution (8.1.1) from the two absorption bottles into two 50 ml stoppered colorimetric tubes and wash them with a small amount of water The inner wall of the absorption bottle is incorporated into the colorimetric tube, and the volume is adjusted and shaken. Note. For bromine-containing waste gas samples, transfer the sulfuric acid absorption solution in the first two bubble absorption bottles into two 50 ml colorimetric tubes, and wash them with a small amount of water The inner wall of the polyester absorption bottle was merged into a colorimetric tube, diluted to a constant volume, and shaken. Adjust the sample pH to the column with an appropriate amount of sodium hydroxide solution (6.11) Within the allowed range. 8.3.2 Air samples at fugitive emission monitoring points Transfer the sample solution (8.1.2) from the two absorption bottles to two 10 ml stoppered colorimetric tubes and wash them with a small amount of water The inner wall of the absorption bottle is incorporated into the colorimetric tube, and the volume is adjusted and shaken. 8.3.3 Full Procedure Blank Sample The entire program blank (8.1.3) is synchronized according to the organic exhaust gas sample and the air sample at the fugitive emission monitoring point. 预 制备。 Prepared. 8.3.4 Laboratory blank sample Take the same batch of absorbent, and synchronize them according to the samples of the organic exhaust gas emission and the air samples at the fugitive emission monitoring point. 预 制备。 Prepared.9 Analysis steps9.1 Chromatographic Reference Conditions Reference condition 1. Eluent is 35 mmol/L potassium hydroxide solution, isocratic eluent, flow rate is 1.00 ml/min, injection The volume was 25 µl, the column temperature was 30 ° C, and the suppressor current was 104 mA. Reference condition 2. The eluent is a mixed solution of 1.8 mmol/L sodium carbonate and 1.7 mmol/L sodium bicarbonate. The flow rate was 1.00 ml/min, the injection volume was 20 µl, the column temperature was 30 ° C, and the suppressor current was 40 mA. 9.2 Establishment of standard curve Take 0.00 ml, 0.10 ml, 0.50 ml, 1.00 ml, 2.50 ml, 5.00 ml bromide standard solution (6.6) respectively In 6 50 ml volumetric flasks, dilute with water and mix. The mass concentration of bromide ion in this standard series (as Br-) It is 0.00 mg/L, 0.20 mg/L, 1.00 mg/L, 2.00 mg/L, 5.00 mg/L, 10.0 mg/L (reference concentration). According to the chromatographic reference condition (9.1), the measurement is performed in order from low concentration to high concentration, and the peak area or peak height is recorded. Taking the mass concentration of bromide ion (calculated as Br-, mg/L) as the abscissa, and its corresponding peak height or peak area as the ordinate, establish Establish a standard curve. The bromine ion chromatogram in the hydroxide eluent system is shown in Figure 3. The reference color of the bromide ion in the carbonate eluent system The spectrum is shown in Figure 4. Figure 3 Reference chromatogram of bromide ion in hydroxide eluent system μS min Figure 4 Reference chromatogram of bromide ion in carbonate eluent system 9.3 Sample measurement Filter the prepared samples (8.3.1 and 8.3.2) with disposable microporous membrane syringe filters (6.12), and then use The injector (7.8) is injected into the ion chromatograph, and the measurement of the sample is performed according to the same chromatographic conditions as the standard curve establishment (9.2). set. 9.4 Blank test Prepare the prepared blank samples (8.3.3 and 8.3.4) according to the same operation and chromatographic conditions as the sample measurement (9.2). Line determination. 10 Calculation and representation of results 10.1 Calculation of results 10.1.1 Organized emission sample Calculate the concentration of hydrogen bromide in the organic exhaust gas according to formula (1). Vnd HBr 9.79 9.800.50) (21 ) ( (1) In the formula. ρ (HBr)-the concentration of HBr in the organic exhaust, mg/m 3; ρ1--Br in the first cuvette sample with stopper -Concentration, mg/L; ρ2--Br in second cuvette sample with stopper -Concentration, mg/L; Vnd--sampling volume of dry flue gas under standard conditions, L; 80.9--HBr molar mass, g/mol; 79.9--Br -The molar mass, g/mol; 50.0--constant volume, ml; D--sample dilution. μS min 10.1.2 Air samples at fugitive emission monitoring points Calculate the concentration of hydrogen bromide in the air at the fugitive emission monitoring point according to formula (2). Vn HB r 9.79 9.800.10) (21 ) ( (2) Where. ρ (HBr)-the concentration of HBr in the air at the fugitive emission monitoring point, mg/m 3; ρ1--Br in the first cuvette sample with stopper -Concentration, mg/L; ρ2--Br in second cuvette sample with stopper -Concentration, mg/L; Vn--sampling volume under standard conditions, L; 80.9--HBr molar mass, g/mol; 79.9--Br -The molar mass, g/mol; 10.0--constant volume, ml; D--sample dilution. 10.2 Results representation The number of reserved digits after the decimal point of the measurement result is consistent with the detection limit, and a maximum of three significant digits are retained. 11 Precision and accuracy 11.1 Precision Six verification laboratories have spiked bromine ions at concentrations of 0.400 mg/L, 1.00 mg/L and 4.00 mg/L Perform 6 parallel determinations after the simulated sampling process. Relative standard deviations in the laboratory are. 2.2% to 7.0%, 2.2% to 4.0%, 1.1% to 5.9%; The relative standard deviations between laboratories are. 6.3%, 5.0%, 2.7%; Repeatability limits are. 0.03 mg/m3, 0.23 mg/m3, 1.0 mg/m3; Reproducibility limits were 0.04 mg/m3, 0.42 mg/m3, and 1.2 mg/m3, respectively. Six verification laboratories simulated actual samples of hydrogen bromide standard gases at concentrations of 0.250 mg/m3 and 12.5 mg/m3, respectively Perform 6 parallel determinations after sampling. The relative standard deviations in the laboratory are. 3.7% to 6.3% and 1.2% to 6.5%; The relative standard deviations between laboratories are 4.2% and 3.5%; Repeatability limits are. 0.04 mg/m3 and 1.2 mg/m3; The reproducibility limits are. 0.03 mg/m3 and 1.5 mg/m3. 11.2 Accuracy Six verification laboratories have tested the uniform standard samples containing bromide (Br-) (standard value is 2.03 mg/L ± 0.08 mg/L) Perform 6 parallel determinations. The relative errors are. -0.5% to 3.0%; The final relative error is 0.6% ± 4.0%. Six verification laboratories simulate the sampling process of solutions with bromine ions spiked at 4.00 μg, 40.0 μg, and 100 μg, respectively After recovery measurement. Spike recovery rates were. 88.6% to 102%, 98.0% to 103%, 96.1% to 101%; The final recoveries were 95.5% ± 6.4%, 101% ± 2.0%, and 99.9% ± 2.0%. 12 Quality Assurance and Quality Control 12.1 Blank test Determine at least 1 full program blank and 1 laboratory blank for every 20 samples or batch (≤20 samples). The blank measurement value should be lower than the detection limit of the method, otherwise the cause should be found or the sample should be collected again. 12.2 Calibration curve The linear correlation coefficient of the standard curve should be ≥0.999. Every 20 samples or each batch (less than 20 samples) shall be measured. Check the middle concentration point of the standard curve, and the relative error should be within ± 10%. 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