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HJ 1078-2019 English PDF

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HJ 1078-2019: Stationary source emission--Determination of 8 organosulfur compounds including methanethiol--Bag sampling and preconcentration/gas chromatography mass spectrometry
Status: Valid

Standard ID	USD	BUY PDF	Lead-Days	Standard Title (Description)	Status
HJ 1078-2019	399	Add to Cart	4 days	Stationary source emission--Determination of 8 organosulfur compounds including methanethiol--Bag sampling and preconcentration/gas chromatography mass spectrometry	Valid

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Basic data

Standard ID: HJ 1078-2019 (HJ1078-2019)
Description (Translated English): Stationary source emission--Determination of 8 organosulfur compounds including methanethiol--Bag sampling and preconcentration/gas chromatography mass spectrometry
Sector / Industry: Environmental Protection Industry Standard
Classification of Chinese Standard: Z25
Classification of International Standard: 13.040.40
Word Count Estimation: 17,152
Date of Issue: 2019
Date of Implementation: 2020-06-30
Issuing agency(ies): Ministry of Ecology and Environment

HJ 1078-2019: Stationary source emission--Determination of 8 organosulfur compounds including methanethiol--Bag sampling and preconcentration/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.
Stationary source emission--Determination of 8 organosulfur compounds including methanethiol--Bag sampling and preconcentration/gas chromatography mass spectrometry National Environmental Protection Standard of the People's Republic of China 8 kinds of sulfur containing methanethiol from stationary pollution sources Determination of organic compounds by air bag sampling-pre-concentration / Gas chromatography-mass spectrometry Stationary source emission-Determination of 8 organosulfur compounds including methanethiol-Bag sampling and preconcentration/gas chromatography mass spectrometry 2019-12-31 release 2020-06-30 Implementation Published by the Ministry of Ecology and Environment i directory Foreword ... ii 1 Scope ... 1 2 Normative references ... 1 3 Method principle ... 1 4 Interference and elimination ... 1 5 Reagents and materials ... 1 6 Instruments and equipment ... 2 7 Sample ... 3 8 Analysis steps ... 4 9 Calculation and presentation of results ... 7 10 Precision and accuracy ... 8 11 Quality Assurance and Quality Control ... 9 12 Waste disposal ... 9 13 Precautions ... 9 Appendix A (Normative Appendix) Limits of detection and determination of target compounds ... 10 Appendix B (informative appendix) Retention time and characteristic ions of the target compound ... 11 Appendix C (Informative Appendix) Precision and accuracy of the method ... 12

Foreword

To implement the Environmental Protection Law of the People ’s Republic of China and the Air Pollution Prevention and Control Law of the People ’s Republic of This standard is formulated to ensure human health, regulate the determination of sulfur-containing organic compounds in exhaust gas from stationary pollution sources. This standard stipulates the sampling and pre-concentration of airbags for the determination of 8 sulfur-containing organic compounds such as methyl mercaptan in waste gas from stationary sources. Gas chromatography-mass spectrometry. Appendix A of this standard is a normative appendix, and Appendix B and Appendix C are informative appendices. This standard is issued for the first time. This standard is organized and formulated by the Ecological Environment Monitoring Department and the Regulations and Standards Department of the Ministry of Ecology and Environment. This standard was drafted by. Shanghai Environmental Monitoring Center. Verification unit of this standard. Beijing Environmental Protection Monitoring Center, Quanzhou Environmental Monitoring Station, Shanghai Putuo District Environmental Monitoring Station, Shanghai Fengxian District Environmental Monitoring Station, Shanghai Jinshan District Environmental Monitoring Station and Shanghai Boyou Testing Technology Co., Ltd. This standard was approved by the Ministry of Ecology and Environment on December 31,.2019. This standard will be implemented from June 30, 2020. This standard is interpreted by the Ministry of Ecology and Environment. 1 Determination of 8 kinds of sulfur-containing organic compounds such as methyl mercaptan from stationary pollution sources Bag sampling-preconcentration/gas chromatography-mass spectrometry Warning. The standard products used in the experiment are all volatile and toxic chemicals. The reagent preparation and sample preparation process should be It should be carried out in a fume hood, and protective equipment should be worn according to regulations to avoid inhalation of the respiratory tract.

1 Scope of application

This standard stipulates the sampling and pre-concentration of airbags for the determination of 8 sulfur-containing organic compounds such as methyl mercaptan in waste gas from stationary sources. Gas chromatography-mass spectrometry. This standard applies to methyl mercaptan, ethyl mercaptan, methyl sulfide, methyl ethyl sulfide, carbon disulfide, ethyl sulfide in waste gas from stationary sources Determination of 8 sulfur-containing organic compounds including ether, dimethyl disulfide and thiophene. When the sampling volume is 50.0 ml, the detection limit of the method for sulfur-containing organic compounds determined by this standard is 0.01 ～ 0.02 mg/m3, The lower limit of determination is 0.04 to 0.08 mg/m3, see Appendix A for details.

2 Normative references

This standard refers to the following documents or their clauses. For the cited documents without date, the valid version applies to this standard. GB/T 16157 Sampling methods for particulate matter and gaseous pollutants in exhaust from stationary sources HJ 732 Sampling airbag method for volatile organic compounds in waste gas from stationary sources HJ/T 373 Technical Specifications for Quality Assurance and Quality Control of Fixed Pollution Source Monitoring (Trial) HJ/T 397 Fixed source exhaust gas monitoring technical specification

3 Method principle

Collect waste gas from stationary pollution sources with an air bag, after cold trap concentration and thermal analysis, enter gas chromatography separation and detect by mass spectrometry Device for detection. Qualitative comparison with the standard substance mass spectrum and retention time, internal standard method for quantification.

4 Interference and elimination

When the concentration of other types of volatile organic compounds affects the measurement of sulfur-containing organic compounds, you can reduce the Release the sample or use a highly selective detector for sulfur compounds for analysis.

5 Reagents and materials

5.1 Standard gas. methyl mercaptan, ethyl mercaptan, methyl sulfide, methyl ethyl sulfide, carbon disulfide, ethyl sulfide, dimethyl disulfide, thiophene The concentration of 2 is 2 μmol/mol. High-pressure steel cylinders are stored, the pressure of the steel cylinder is not less than 1.0 MPa, please refer to the standard gas certificate for the storage period Related instructions. Note. The concentration of standard gas is for reference only, and other concentration standard gas can be purchased on demand if the method performance parameters are met. 5.2 Standard gas. use a gas diluter (6.7) to dilute the standard gas (5.1) with nitrogen (5.8) to 20 nmol/mol, Stored in the tank (6.6), now ready for use. 5.3 Internal standard gas. the concentration is 1 μmol/mol. Internal standard is 1,4-difluorobenzene, stored in high-pressure steel cylinders, the pressure of the steel cylinders is not low At 1.0 MPa, the storage period refers to the relevant description of the standard gas certificate. Before meeting the method requirements without interfering with the target compound Mentioned, other substances can also be used as internal standards. 5.4 Internal standard gas. use gas diluter (6.7) to dilute internal standard gas (5.3) with nitrogen (5.8) to The concentration is 100 nmol/mol and it can be stored in the tank (6.6) for 20 days. 5.5 4-bromofluorobenzene standard gas. the concentration is 1 μmol/mol, stored in a high-pressure steel cylinder, the pressure of the cylinder is not less than 1.0 MPa, stored Please refer to the relevant description of the standard gas certificate. 5.6 4-bromofluorobenzene standard gas. use a gas diluter (6.7) to use 4-bromofluorobenzene standard gas (5.5) with nitrogen (5.8) Dilute to a concentration of 100 nmol/mol and store in a tank (6.6) for 20 days. 5.7 High purity helium. purity ≥99.999%. 5.8 High purity nitrogen. purity ≥99.999%. 5.9 Liquid nitrogen.

6 Instruments and equipment

6.1 Sampling device. The requirements of the air bag sampling device shall comply with the relevant regulations of HJ 732. 6.2 Gas Chromatography-Mass Spectrometer. The gas phase has an electronic flow controller, and the column temperature box has a program temperature rise function. Equipped with column thermostat cooling device. The mass spectrometer part has an electron bombardment (EI) ion source, full scan/selective ion scan, Dynamic/manual tuning, library search and other functions. 6.3 Capillary chromatography column. 60 m × 0.32 mm × 1.04 µm (100% dimethyl polysiloxane fixative), or other Effective capillary chromatography column. 6.4 Gas cold trap concentrator. It has the functions of automatic quantitative sampling and automatic addition of standard gas and internal standard. Should have three levels The cold trap can introduce liquid nitrogen to be cooled to a minimum of -180 ℃, complete three-stage trapping and remove interferences such as H2O and CO2. Concentrator The internal pipeline and the pipeline connected with the gas chromatography-mass spectrometer are all made of inert materials, and can be heated in the range of 50 to 150 ℃. 6.5 Automatic sampler of concentrator. It can carry out automatic sampling of air bag and canister. The internal pipelines are made of inert materials and have tubes. Road heating function. 6.6 Tank. stainless steel tank with inert treatment on the inner wall, 6 L or other large-volume tank for storing standard gas The 0.45 L or other small volume tank is used to store samples. The pressure resistance of the tank is > 241 kPa. 6.7 Gas diluting instrument. It has the function of pressurizing and diluting the tank, the dilution factor can reach 1000 times, and the internal pipeline uses inert materials quality. 6.8 Tank cleaning device. It can pump the tank to vacuum (< 10 Pa), and it has the functions of heating, humidifying and pressure cleaning. 6.9 Airbag. fluoropolymer or other equivalent material airbag with a volume of at least 1L, with a sealed valve or inert material of inert material Gland. 6.10 Vacuum pressure gauge. accuracy requirement ≤7 kPa, pressure range. -101 ～ 202 kPa. 36.11 Gas-tight injection needle. 10 ml, with removable side-hole needle and round-hole needle. 6.12 Pneumatic connector. used in series with tank (6.6) and air bag (6.9) short. 6.13 Plug. stainless steel nuts and septa can be used to assemble or purchase commercial products. 6.14 Liquid nitrogen tank. stainless steel material with a volume of 100-200 L. 6.15 Commonly used instruments and equipment in general laboratories.

7 samples

7.1 Sample collection and storage 7.1.1 Sample collection Determination of sampling location and sampling point, sampling frequency and sampling time of exhaust gas from fixed pollution sources, measurement and sampling of exhaust parameters Such operations implement the relevant provisions of HJ/T 397, GB/T 16157 and HJ 732. When sampling, heating sampling should be turned on as required For the power supply, the air bag must be cleaned with sample gas at least 3 times, and then use the sampling device (6.1) to collect the sample gas. 7.1.2 Sample storage Airbag samples should be stored away from light at room temperature, and should be analyzed within 12 hours after sampling. If methyl mercaptan and ethyl mercaptan are not analyzed At this time, the sample can be measured within 18 h. Otherwise, use the pneumatic connector (6.12) to introduce the sample into the pre-clean and draw to The analysis was completed within 7 days in the vacuum tank (6.6). 7.2 Preparation of samples 7.2.1 Heating of the sample Before the sample analysis, the inner wall of the sample air bag must be observed. If droplets condense, the air bag should be placed in an oven and heated Until the droplet condensation phenomenon is eliminated, then quickly analyze. If there is no droplet condensation, the air bag (6.9) or tank (6.6) Connect directly to the autosampler (6.5) for analysis. Note. When using an oven to heat the air bag, a suitable heating temperature (not more than 50 ° C) should be set to avoid heating deformation of the sampling bag. 7.2.2 Dilution of the sample When the concentration of sulfur-containing organic compounds in the gas sample exceeds the linear range of the standard curve, the sample needs to be diluted. Dilute When the release factor does not exceed 3, the tank (6.6) can be diluted with nitrogen (5.8). Must be measured with a vacuum pressure gauge (6.10) Set the pressure in the tank and calculate the dilution factor according to formula (1). When the dilution factor exceeds 3, a gas-tight syringe (6.11) can be used Use a plug (6.13) to inject a suitable amount of sample into a tank that has been pre-cleaned and evacuated, and then pressurize it to 101 kPa with nitrogen And calculate the dilution factor according to formula (2). % 00 = Ya Xa (1) In the formula.% 00-dilution multiple, dimensionless; Xa-tank pressure before dilution, kPa; 4Ya-diluted tank pressure, kPa. % 00 = % 00a % 00% 00 (2) In the formula.% 00--dilution multiple, dimensionless; Va-the volume of the tank, ml; V% 00-the amount of sample injected into the tank, ml. Note. The laboratory may adopt other equivalent dilution methods. 7.3 Preparation of blank samples 7.3.1 Blank sample of the whole program Take a sample and collect an air bag of the same batch, fill it with nitrogen in the laboratory and bring it to the sampling site without sample collection. Follow the same steps as sample storage (7.1.2) to save the blank sample of the whole procedure and return it to the laboratory. 7.3.2 Laboratory blank samples Take a sample and collect an air bag of the same batch, and fill it with nitrogen in the laboratory.

8 Analysis steps

8.1 Instrument reference conditions 8.1.1 Reference conditions of cold trap concentrator At room temperature, the sampling volume is 50.0 ml (can be adjusted according to actual conditions) Primary cold trap (empty tube). trapping temperature. -30 ℃; trapping flow rate. 80 ml/min; analytical temperature. 10 ℃; valve temperature. 120 ℃; baking temperature. 150 ℃; baking time. 10 min. Secondary cold trap (TENAX tube). trapping temperature. -80 ℃, transfer preheating temperature. -60 ℃; trapping flow rate. 10 ml/min; Resolution temperature. 10 ° C; valve temperature. 120 ° C; baking temperature. 190 ° C; baking time. 10 min. Three-stage cold trap (silanized stainless steel capillary). focusing temperature. -170 ℃; analysis time. 2 min; analysis temperature. 50 ～ 70 ℃; baking time. 3 min. Transmission line temperature. 100 ° C. Note. The above conditions are the introduction of liquid nitrogen (5.9) low temperature enrichment at the same time in the first-stage cold trap. If segmented low temperature enrichment is used, when the primary cold trap is glass For beads, the trapping temperature is recommended to be adjusted to -170 ℃, and the trapping temperature of the secondary cold trap can be adjusted to -30 ℃ or below. Different models of the best The working conditions are different, and the operation should be carried out according to the instruction manual of the instrument. 8.1.2 Reference analysis conditions of gas chromatography Program temperature rise. the initial temperature is -35 ℃, after holding for 3 minutes, the temperature was raised to 180 ℃ at a rate of 7.5 ℃/min and kept for 3 minutes Inlet temperature. 100 ° C. Solvent delay time. 2.7 min. Carrier gas flow rate. the initial flow rate is 2.5 ml/min, and it is maintained at 2 ml/min for 30 min after 4 min. 5 Split ratio. 20. 1. Note. Separation of sulfur-containing organic compounds can be accomplished by programming at an initial temperature of room temperature. 8.1.3 Reference analysis conditions for mass spectrometry Interface temperature. 250 ℃; Ion source temperature. 230 ° C; Ionization energy. 70eV; Scanning method. full scan (SCAN); Scanning range. 35 ～ 300 amu. Note. The best working conditions of different models of instruments are different, and they should be operated according to the instruction manual of the instrument. If you meet the qualitative requirements, you can also Use Select ion scan method (SIM). 8.1.4 Instrument performance check Before analyzing samples, you need to check the performance of the GC/MS instrument. Concentrate 4-bromofluorobenzene standard gas (5.6) through cold trap The instrument injects 50.0 ml. The BFB key ion abundance obtained must meet the criteria in Table 1. Table 1 Key ion abundance standards for 4-bromofluorobenzene (BFB) Mass ion abundance standard mass ion abundance standard 50 8% ～ 40% of mass 95 174 50% ～ 120% of mass 95 75 30% ～ 66% of mass 95 175 4% ～ 9% of mass 174 95 base peak, 100% relative abundance 176 mass 174 93% ～ 101% 96 5% to 9% of mass 95 177 5% to 9% of mass 176 173 is less than 2% of mass 174 8.2 Calibration 8.2.1 Standard gas preparation Dilute the standard gas (5.1) 100 times. the standard gas (5.1) steel cylinder and nitrogen (5.8) steel cylinder and the gas dilution instrument (6.7) Connect, set the dilution factor, open the cylinder valve, adjust the flow rate of the two gases, wait for the standard gas and nitrogen flow After the speed is stabilized, empty it for more than 10 minutes to saturate the active points in the pipeline, and then take the 6 L tank (6.6) that was pre-cleaned and evacuated to vacuum Connect to the gas diluting instrument (6.7), open the tank valve and start preparation. After the tank pressure reaches the preset value (generally 172 kPa), Close the tank valve and cylinder gas valve. 8.2.2 Internal standard is prepared with gas The internal standard uses a gas concentration of 100 nmol/mol. Prepare the internal standard gas (5.3) according to step 8.2.1. 8.2.3 Determination of calibration series Extract 50.0 ml, 100 ml, 300 ml, 500 ml, and 700 ml standard gas (5.2), each adding 50.0 ml 6 The internal standard uses gas (5.4), and the target compound concentrations are 20 nmol/mol, 40 nmol/mol, 120 nmol/mol, Standard gas series of.200 nmol/mol and 280 nmol/mol (this is the reference concentration). According to the reference conditions of the instrument, Measure from low to high concentration. 8.2.4 Calculation of average relative response factor The relative response factor (% 00% 00% 00% 00) of the target compound at point i of the standard series is calculated according to formula (3). % 00% 00% 00i = % 00% 00 % 00% 00t ×% 00% 00t % 00i (3) In the formula.% 00% 00% 00i--the relative response factor of the target compound at point i in the standard series, dimensionless; Ai--the quantitative ion peak area of the target compound at point i in the standard series; AIS--The i-point in the standard series corresponds to the target compound to quantify the ion peak area; % 00% 00t--the mole fraction of the internal standard compound, nmol/mol; % 00% 00--the mole fraction of the target compound at point i in the standard series, nmol/mol. The average relative response factor of the target is calculated according to formula (4). % 00% 00% 00% 00% 00% 00% 00% 00 =% 00 % 00% 00% 00% 00% 00% 00 (4) Where.% 00% 00% 00% 00% 00% 00% 00% 00-the average relative response factor of the target compound, dimensionless; % 00% 00% 00% 00--the relative response factor of the target compound at point i in the standard series, dimensionless; n--standard series points. When calculating with relative response factors, the relative standard deviation (RSD) of the relative response factors of the standard series of target compounds should be Less than or equal to 30%. 8.2.5 Establish the calibration curve by least square method Taking the response value ratio of the target compound and the corresponding internal standard as the ordinate, and the concentration ratio as the abscissa, the least square method is used to estab......

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Question 1: How long will the true-PDF of HJ 1078-2019_English be delivered?

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