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HJ 1041-2019 English PDF

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HJ 1041-2019: Stationary source emission - Determination of trimethylamine - Suppressed ion chromatography
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Standard ID	Contents [version]	USD	STEP2	[PDF] delivered in	Standard Title (Description)	Status	PDF
HJ 1041-2019	English	229	Add to Cart	3 days [Need to translate]	Stationary source emission - Determination of trimethylamine - Suppressed ion chromatography	Valid	HJ 1041-2019

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Basic data

Standard ID	HJ 1041-2019 (HJ1041-2019)
Description (Translated English)	Stationary source emission - Determination of trimethylamine - Suppressed ion chromatography
Sector / Industry	Environmental Protection Industry Standard
Classification of Chinese Standard	Z25
Classification of International Standard	13.040.40
Word Count Estimation	10,114
Date of Issue	2019
Date of Implementation	2020-04-24
Issuing agency(ies)	Ministry of Ecology and Environment

HJ 1041-2019: Stationary source emission - Determination of trimethylamine - Suppressed ion chromatography

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(Determination of trimethylamine in exhaust gas from stationary sources Suppressed ion chromatography) National Environmental Protection Standard of the People's Republic of China Determination of trimethylamine in exhaust gas from stationary sources Suppressed ion chromatography Stationary source emission-Determination of trimethylamine -Suppressed ion 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 ... 1 6 Instruments and equipment ... 2 7 Sample ... 3 8 Analysis steps ... 4 9 Results calculation and representation ... 4 10 Precision and accuracy ... 5 11 Quality Assurance and Quality Control ... 5 12 Waste disposal ... 6

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 exhaust gas from fixed pollution sources, and formulate this standard. This standard specifies ion chromatography for the determination of trimethylamine in 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 Eco-environment Monitoring Center, Shandong Product Quality Inspection Research Institute, Shandong Ante Testing Co., Ltd. and Chinese Academy of Sciences Island Bioenergy and Process Institute. 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 trimethylamine in exhaust gas from stationary sources. Suppressed ion chromatography Warning. The hydrochloric acid used in the experiment is strongly irritating and corrosive. The reagent preparation process should be performed in a fume hood; Wear protective equipment as required during operation to avoid breathing into the respiratory tract and contact with skin and clothing.

1 Scope

This standard specifies an inhibitory ion chromatography method for the determination of trimethylamine in exhaust gas from stationary sources. This standard applies to the determination of trimethylamine in exhaust gas from stationary sources. When the sampling volume is 20 L (standard state) and the absorption volume is 50 ml, the method detection limit is 0.03 mg/m3. The lower limit of determination was 0.12 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 905 Technical Specification for Odor Pollution Environmental Monitoring HJ/T 397 Fixed source exhaust gas monitoring technical specifications

3 Method principle

After the trimethylamine in the exhaust gas from the fixed pollution source is absorbed by the acidic solution, it is separated by ion chromatography and detected by a suppressed conductivity detector. Measurement. Qualitative according to retention time, quantified by external standard method.

4 Interference and cancellation

4.1 Under the analysis conditions recommended by this method, Li, Na, NH4 , K, Mg2, Ca2 6 common cations, Both methylamine and dimethylamine can be effectively separated from trimethylamine without disturbing the determination. 4.2 Some hydrophobic compounds in the sample may affect the chromatographic separation effect and the service life of the column. Activated pre-treatment columns eliminate or reduce effects.

5 Reagents and materials

Unless otherwise specified, analytical reagents that meet national standards are used. Experimental water is resistivity ≥ 18 MΩ · cm of fresh deionized 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 Methanesulfonic acid. w (CH3SO3H) ≥99%. 5.4 Trimethylamine hydrochloride standard. w (CH3) 3N · HCl) ≥98%. 5.5 Absorption liquid. One of the following two absorption liquids can be used. 5.5.1 Sulfuric acid absorption solution. c (H2SO4) = 0.03 mol/L. Pipet 1.60 ml of sulfuric acid (5.1), slowly add an appropriate amount of water, cool and dilute to a 1000 ml volumetric flask. Mix well. Provisional use. 5.5.2 Hydrochloric acid absorption solution. c (HCl) = 0.06 mol/L. Pipette 5.00 ml of hydrochloric acid (5.2), slowly add an appropriate amount of water, and dilute to a 1000 ml volumetric flask after cooling. Mix well. Provisional use. 5.6 Trimethylamine (TMA) standard stock solution. ρ ((CH3) 3N) = 1000 mg/L. Accurately weigh 0.1620 g of trimethylamine hydrochloride standard (5.4), dissolve it in absorbent solution (5.5), and determine the volume to 100 ml. It can be stored stably for 1 month if refrigerated below 4 ° C. 5.7 Trimethylamine standard solution. ρ ((CH3) 3N) = 10.00 mg/L. Accurately transfer 1.00 ml of trimethylamine standard stock solution (5.6) into a 100 ml volumetric flask and dilute with absorbent solution (5.5) To the mark, it can be stored for 1 month under 4 ℃. 5.8 Methanesulfonic acid eluent. Prepare according to the instrument model and the operating conditions of the column manual. Leaching given below Liquid conditions for reference. 5.8.1 Methanesulfonic acid eluent stock solution. c (CH3SO3H) = 0.92 mol/L. Accurately weigh 88.42 g of methanesulfonic acid (5.3) and slowly add it into a volumetric flask containing an appropriate amount of deionized water. After cooling, dilute Reconstitute to 1000 ml and mix. 5.8.2 Methanesulfonic acid eluent. c (CH3SO3H) = 0.023 mol/L. Accurately pipette 25.00 ml of methanesulfonic acid eluent stock solution (5.8.1) into a 1000 ml volumetric flask and dilute to volume with water. 5.9 Filter membrane. glass fiber, PTFE or equivalent material. 5.10 Water phase needle filter. 0.45 μm, polyethersulfone or equivalent.

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 Filter clip. PTFE and other materials, the size matches the filter (5.9). 6.3 Bubble absorption bottle. 75 ml. 6.4 Ion chromatograph. equipped with cation suppression conductivity detector. 6.5 Chromatographic column. cation separation column, particle size 5.5 μm, inner diameter 5 mm, column length 250 mm, polydivinylbenzene/ethyl Vinyl phenylene (with carboxylic or phosphoric acid functional groups) and cation-protected columns, or other equivalent high-capacity columns. 6.6 Pretreatment column. Silica matrix bonded C18 column and other solid phase extraction columns. 6.7 General laboratory instruments and equipment.

7 samples

7.1 Sample collection 7.1.1 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 (6.3) each containing 50.0 ml of absorption liquid (5.5) 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 7.1.2 Full Program Blank Bring the absorption bottle filled with the absorption liquid (5.5) in the same batch to the sampling site, not connected to the sampler. 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 Transfer the sample solution (7.1.1) from two absorption bottles into two 50 ml colorimetric tubes, and use a small amount of absorption solution (5.5) Wash the inner wall of the absorption bottle, and transfer the lotion into the colorimetric tube, and make up to the mark. Filter with water phase needle filter (5.10), Discard 2 ml of the initial solution and collect the filtrate into a 5 ml stoppered vial for testing. The entire program is blank (7.1.2) Follow the steps above 预制备。 Prepared. 7.4 Preparation of laboratory blank samples Replace the sample with the same batch of absorbent solution (5.5) and prepare the blank sample according to the sample preparation (7.3) step.

8 Analysis steps

8.1 Chromatographic Reference Conditions Optimize the measurement conditions or parameters according to the instrument's instruction manual. Reference conditions. Methanesulfonic acid eluent (5.8.2) 0.023 mol/L, isocratic eluent; flow rate 1.0 ml/min. Sample volume was 25 µl; column temperature was 30 ° C ± 0.5 ° C; suppressor current was 68 mA. 8.2 Establishment of calibration curve Take an appropriate amount of trimethylamine standard solution (5.7), dilute with an appropriate amount of absorbent solution (5.5), and prepare at least 5 concentrations Point standard series, the mass concentration of trimethylamine is 0.00 mg/L, 0.05 mg/L, 0.25 mg/L, 1.00 mg/L, 5.00 mg/L, 10.00 mg/L (this concentration is the reference concentration). Inject the samples in descending order of concentration and record the peak surface Product (or peak height). A calibration curve was established with the mass concentration of trimethylamine as the abscissa and the peak area (or height) as the ordinate. The reference chromatogram of trimethylamine standard sample is shown in Figure 2. Figure 2 Reference chromatogram of trimethylamine standard sample 8.3 Sample determination The determination of the sample was performed in accordance with the same chromatographic reference conditions (8.1) as the calibration curve was established. 8.4 Blank test The measurement was performed according to the same procedure as the sample measurement (8.3) and the chromatographic 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 Calculate the concentration of trimethylamine in the sample according to formula (1). (1) Where. ρ-the concentration of trimethylamine in the exhaust gas sample, mg/m3; 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 retained after the decimal point of the measurement result is consistent with the method detection limit, and a maximum of three significant digits are retained. 10 Precision and accuracy 10.1 Precision Six laboratories have separately spiked 6 groups of 0.500 mg/m3, 10.0 mg/m3 and 20.0 mg/m3 spiked samples. Determined after simulated sampling. The relative standard deviations in the laboratory were 1.4% to 7.1%, 1.1% to 7.3%, and 1.2% to 7.9%. The relative standard deviations between laboratories were 2.1%, 2.9%, and 2.0%; the repeatability limits were 0.07 mg/m3, 1.1 mg/m3, 2.6 mg/m 3, the reproducibility limits are 0.07 mg/m3, 1.3 mg/m3, and 2.7 mg/m3, respectively; 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. Relative standard deviations within the laboratory are 1.8% to 7.6% and 1.5% to 8.0%, respectively. The deviations were 2.0% and 1.9%, respectively; the repeatability limits were 0.05 mg/m3 and 0.56 mg/m3, respectively, and the reproducibility limits were 0.06 mg/m 3 and 0.58 mg/m3. 10.2 Accuracy Six laboratories have separately spiked 6 groups of 0.500 mg/m3, 10.0 mg/m3 and 20.0 mg/m3 spiked samples. Determined after simulated sampling. Spike recovery rates were 86.5% -99.8%, 90.2% -99.7%, and 90.0% -101%, respectively. The final recoveries were 92.6% ± 5.2%, 96.5% ± 3.9%, and 96.7% ± 4.4%. 11 Quality Assurance and Quality Control 11.1 Make at least one laboratory blank and full procedure blank sample for every 20 samples or each batch (≤20 samples), The trimethylamine concentration in the blank sample should be below the method detection limit. 11.2 A calibration curve shall be established for each batch of samples. Correlation coefficient of calibration curve ≥ 0.995, otherwise you should find the cause or re-establish Calibration curve. 11.3 Analyze the standard solution at the middle concentration point of the calibration curve every 20 samples or each batch (≤20 samples). The relative error between the measurement result and the initial curve at this point should be within ± 10%. 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 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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