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HJ 1077-2019 English PDF

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HJ 1077-2019: Stationary source emission--Determination of oil fume and oil mist--Infrared spectrophotometric method
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HJ 1077-2019	English	259	Add to Cart	3 days [Need to translate]	Stationary source emission--Determination of oil fume and oil mist--Infrared spectrophotometric method	Valid	HJ 1077-2019

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Basic data

Standard ID	HJ 1077-2019 (HJ1077-2019)
Description (Translated English)	Stationary source emission--Determination of oil fume and oil mist--Infrared spectrophotometric method
Sector / Industry	Environmental Protection Industry Standard
Classification of Chinese Standard	Z25
Classification of International Standard	13.040.40
Word Count Estimation	11,198
Date of Issue	2019
Date of Implementation	2020-06-30
Issuing agency(ies)	Ministry of Ecology and Environment

HJ 1077-2019: Stationary source emission--Determination of oil fume and oil mist--Infrared spectrophotometric method

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Stationary source emission--Determination of oil fume and oil mist--Infrared spectrophotometric method National Environmental Protection Standard of the People's Republic of China Determination of exhaust fumes and oil mist from stationary pollution sources Infrared spectrophotometry Stationary source emission-Determination of oil fume and oil mist -Infrared spectrophotometric method 2019-12-31 release 2020-06-30 Implementation Published by the Ministry of Ecology and Environment

Foreword ... ii 1 Scope ... 1 2 Normative references ... 1 3 Terms and definitions ... 1 4 Method principle ... 1 5 Reagents and materials ... 2 6 Instruments and equipment ... 3 7 Sample ... 3 8 Analysis steps ... 4 9 Calculation and presentation of results ... 6 10 Precision and accuracy ... 6 11 Quality Assurance and Quality Control ... 7 12 Waste disposal ... 7 13 Precautions ... 7

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 measurement methods of oil smoke and oil mist in the exhaust gas from stationary sources. This standard specifies the infrared spectrophotometric method for the determination of oil smoke and oil mist in the exhaust gas from stationary sources. 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. Dalian Ecological Environment Monitoring Center of Liaoning Province. Verification unit of this standard. Liaoning Ecological Environment Monitoring Center, Changchun City Environmental Monitoring Center Station, Jilin City Environmental Monitoring Station, Anshan Ecological Environment Monitoring Center of Liaoning Province, Heilongjiang Environmental Monitoring Center Station and Yingkou Environmental Monitoring Center. 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. Determination of exhaust fumes and oil mist from stationary pollution sources Infrared spectrophotometry Warning. The extraction solvent used in the experiment is harmful to human health, and the sample preparation process should be carried out in a fume hood. Wear protective equipment as required to avoid contact with skin and clothing.

1 Scope of application

This standard specifies the infrared spectrophotometric method for the determination of oil smoke and oil mist in the exhaust gas from stationary sources. This standard is applicable to the determination of oil smoke and oil mist in the exhaust gas of stationary pollution sources. When the sampling volume is 250 L (standard state), the extraction volume is 25 ml, when using a 4 cm quartz cuvette, the Methods The detection limits of oil fume and oil mist were both 0.1 mg/m3, and the lower detection limits were 0.4 mg/m3.

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 18483 Catering industry smoke emission standards (for trial implementation) GB/T 16157 Determination of particulate matter in exhaust gas from stationary sources and sampling method of gaseous pollutants Technical condition of HJ/T 48 soot sampler HJ/T 397 Fixed source exhaust gas monitoring technical specification

3 Terms and definitions

The following terms and definitions apply to this standard. 3.1 Oil fume Refers to the volatile oils and fats, organic matter, and their thermal decomposition or cracking products during food cooking and processing. 3.2 Oil mist Refers to the mineral oil and its heating generated in the industrial production process (such as mechanical processing, heat treatment of metal materials, etc.) and its heating Decomposition or cracking products.

4 Method principle

The oil fume and oil mist in the waste gas from the fixed pollution source are adsorbed by the filter cartridge, and then ultrasonically extracted with tetrachloroethylene, and the extract is separated by infrared Photometric determination. The content of oil fume and oil mist is 2930 cm-1 by wave number (the stretching vibration of CH bond in CH2 group), 2960 cm -1 (the stretching vibration of CH bond in CH3 group) and 3030 cm -1 (extension vibration of CH bond in aromatic ring) The absorbances A2930, A2960 and A3030 at the band are calculated.

5 Reagents and materials

Unless otherwise stated, analytical reagents that meet national standards are used for analysis. 5.1 n-hexadecane (C16H34). 5.2 Isooctane (C8H18). 5.3 Benzene (C6H6). 5.4 Tetrachloroethylene (C2Cl4). Using a 4 cm cuvette and air cell as reference, the absorbance at wavenumbers of 2930 cm-1, 2960 cm-1 and 3030 cm-1 should be Do not exceed 0.34, 0.07, and 0, respectively. 5.5 Anhydrous sodium sulfate (Na2SO4). It was heated at 500 ℃ for 4 h, and after cooling, it was put into a ground glass bottle and placed in a desiccator. 5.6 Standard stock solution of n-hexadecane. ρ≈1 × 104 mg/L. Weigh a 100 ml empty volumetric flask (accurate to 1 mg), then add about 1 g of n-hexadecane (5.1), and weigh it again (quasi Make sure to 1 mg), add tetrachloroethylene (5.4) to volume, mix well, and calculate the exact concentration of n-hexadecane standard stock solution. 5.7 Standard use liquid of n-hexadecane. ρ = 1.00 × 103 mg/L. Pipette an appropriate amount of n-hexadecane standard stock solution (5.6) into a 100 ml volumetric flask and make up to volume with tetrachloroethylene (5.4). Mix well. 5.8 Standard stock solution of isooctane. ρ≈1 × 104 mg/L. Weigh a 100 ml empty volumetric flask (accurate to 1 mg), then add about 1 g of isooctane (5.2), and weigh again (precise Make sure to 1 mg), add tetrachloroethylene (5.4) to the volume, mix well, and calculate the exact concentration of the standard stock solution of isooctane. 5.9 Standard use solution of isooctane. ρ = 1.00 × 103 mg/L. Pipette an appropriate amount of the standard stock solution of isooctane (5.8) into a 100 ml volumetric flask, make a volume with tetrachloroethylene (5.4) uniform. 5.10 Standard stock solution of benzene. ρ≈1 × 104 mg/L. Weigh a 100 ml empty volumetric flask (accurate to 1 mg), then add about 1 g of benzene (5.3), weigh again (accurate to 1 mg), add tetrachloroethylene (5.4) to the volume, mix well, and calculate the exact concentration of benzene standard stock solution. 5.11 Standard use solution of benzene. ρ = 1.00 × 103 mg/L. Pipette an appropriate amount of benzene standard stock solution (5.10) into a 100 ml volumetric flask, make up to volume with tetrachloroethylene (5.4), and mix. Note. The commercially available certified standard solution can be purchased directly. 5.12 Standard fume oil. Add 300 ml of peanut oil to a 500 ml double-necked decanter, insert a thermometer with a range of 500 ° C at the side port, at 120 ° C Heat at an open temperature for 30 min, then install an air condensing tube at the upper mouth, raise the temperature to 300 ° C, and reflux for 2 h, then the standard After cooling, take an appropriate amount and place it in a 500 ml sample vial with a Teflon lined screw cap. 5.13 Standard oil stock solution of fume. ρ≈1 × 104 mg/L. Weigh a 100 ml empty volumetric flask (accurate to 1 mg), then add about 1 g of fume standard oil (5.12), and weigh again (Accurate to 1 mg), add tetrachloroethylene (5.4) to the mark, mix well, and calculate the exact concentration of the stock oil of standard oil fume. 5.14 Use liquid for standard oil of fume. ρ = 100 mg/L. Pipette a proper amount of stock oil standard oil stock solution (5.13) into a 250 ml volumetric flask and dilute with tetrachloroethylene (5.4) to Marking. 5.15 Oil mist standard oil. Pipette 6.5 ml n-hexadecane (5.1), 2.5 ml isooctane (5.2) and 1.0 ml benzene (5.3) with a graduated pipette Transfer to a 10 ml volumetric flask and stop tightly and mix immediately. 5.16 Standard oil stock solution of oil mist. ρ≈1 × 104 mg/L. Weigh a 100 ml empty volumetric flask (accurate to 1 mg), then add about 1 g of oil mist standard oil (5.15), and weigh again (Accurate to 1 mg), add tetrachloroethylene (5.4) to the mark, mix well, and calculate the exact concentration of the stock oil standard oil mist. 5.17 Oil mist standard oil use solution. ρ = 100 mg/L. Pipette an appropriate amount of oil mist standard oil stock solution (5.16) into a 250 ml volumetric flask and make up to volume with tetrachloroethylene (5.4). Note. You can directly buy commercially available standard solutions for oil fume and oil mist. 5.18 Metal sampling filter cartridge and PTFE sleeve. Metal filter cartridge material. 316 stainless steel, filled with matte glass beads or 316 stainless steel fiber Dry oil-free clean air and store in the sleeve. When the concentration of oil fume or oil mist is above 10 mg/m3, the oil fume and oil mist The collection efficiency should be ≥95%. 5.19 Glass fiber filter cartridge. Φ28 × 70 mm, the particle collection efficiency for particle size 0.5 μm is not less than 99.9%, and the weight loss is ≤0.2%. After burning at 400 ℃ for 1 h, Check after cooling, and the undeformed or broken glass fiber filter cartridge is put into a Teflon cylindrical sleeve with a cover and sealed for use.

6 Instruments and equipment

6.1 Infrared oil gauge. Equipped with a 4 cm quartz cuvette with lid, the instrument scanning range. 3400 cm-1 to 2400 cm-1. 6.2 Smoke tester. Meet the requirements of HJ/T 48. 6.3 Glass fiber filter cartridge sampling tube. Meet the requirements of HJ/T 48. 6.4 Metal filter cartridge sampling tube and matching filter cartridge. 6.5 Commonly used instruments and equipment in general laboratories.

7 samples

7.1 Sample collection Sampling location, frequency and sampling conditions are in accordance with GB 18483, GB/T 16157, HJ/T 397 and other relevant standards Seeking to proceed. Choose a suitable sampler, install the sampling nozzle and filter cartridge. Choose glass fiber filter cartridge sampling tube (6.3) when collecting oil mist Or metal filter cartridge sampling tube (6.4), select metal filter cartridge sampling tube (6.4) when collecting fume. Check the air tightness of the system before sampling Sex. Continuous sampling for 10 min, put the filter cartridge into the sleeve after sampling. 7.2 Storage of samples The samples should be measured as soon as possible after collection. If the sample cannot be measured within 24 hours, it can be stored in a refrigerator (≤4 ℃) for 7 days. 7.3 Preparation of samples 7.3.1-Sample preparation of oil fume Add 12 ml of tetrachloroethylene (5.4) solvent to the sleeve after sampling, tighten the sleeve cap, and place the sleeve on ultrasonic cleaning Washing device, ultrasonic cleaning for 10 min, the extract is transferred to a 25 ml colorimetric tube, then add 6 ml of tetrachloroethylene (5.4) ultrasonic cleaning Wash for 5 min and transfer the extract to the 25 ml colorimetric tube described above. Clean the filter cartridge and PTFE with a little tetrachloroethylene (5.4) Ethylene sleeve twice, the cleaning solution is transferred to the above 25 ml colorimetric tube, add tetrachloroethylene (5.4) to the scale mark, seal To be tested. 7.3.2 Sample preparation of oil mist 7.3.2.1 If a fiber filter cartridge is used for sampling, the sampled filter cartridge is shredded and placed in a 50 ml beaker, using 25 ml of tetrachloromethane Ethylene (5.4) was ultrasonically extracted in an ultrasonic cleaner for 10 min. The extract was transferred to a 25 ml colorimetric tube and sealed for testing. 7.3.2.2 Sampling with metal filter cartridge, refer to 7.3.1 Sample preparation method of cooking fume in catering industry. 7.4 Preparation of blank samples Using a blank filter cartridge, prepare a blank sample according to the sample preparation step (7.3).

8 Analysis steps

8.1 Calibration 8.1.1 Determination of correction coefficient Measure 2.00 ml of n-hexadecane standard solution (5.7), 2.00 ml of isooctane standard solution (5.9) and 10.00ml Benzene standard use solution (5.11) was placed in three 100 ml volumetric flasks, made up to the mark with tetrachloroethylene (5.4), and mixed. positive The concentrations of cetane, isooctane and benzene standard solutions were 20.0 mg/L, 20.0 mg/L and 100 mg/L, respectively. With tetrachloroethylene (5.4) As a reference solution, use a 4 cm cuvette to measure the standard solution of n-hexadecane, isooctane and benzene at 2930 cm-1, 2960 cm The absorbances A2930, A2960 and A3030 at -1 and 3030 cm-1. After substituting into formula (1) and solving, we can obtain Corresponding correction factors X, Y, Z and F are entered into the instrument for calibration. ) (2930303029602930 F AZAYAX  (1) In the formula. ρ-- the content of the target substance in tetrachloroethylene (mg/L); A2930, A2960 and A3030--the absorbance measured at each corresponding wave number; X, Y, Z-coefficients corresponding to the absorbance of various CH bonds; F--the correction factor for the effect of aliphatic hydrocarbons on aromatic hydrocarbons, namely the absorption of n-hexadecane at 2930 cm-1 and 3030 cm-1 Photometric ratio. For n-hexadecane and isooctane, since their aromatic hydrocarbon content is zero, that is 029303030  , There are. ) H (A ) H (A 2930 (2) 2930 2960 () () () HXAHYAH     (3) 2930 2960 () () () IXAIYAI     (4) The F value can be obtained from formula (2), and the X and Y values can be obtained from formulas (3) and (4). For benzene, there are. 2930 2960 3030 () () () () [()] AB BXABYABZAB        (5) The value of Z can be obtained from formula (5). In the formula. ρ (H)-the concentration of n-hexadecane standard solution, mg/L; ρ (I)-the concentration of isooctane standard solution, mg/L; ρ (B)-the concentration of benzene standard solution, mg/L; A2930 (H), A2960 (H), A3030 (H)-the absorbance of n-hexadecane standard solution measured at each corresponding wavenumber; A2930 (I), A2960 (I), A3030 (I)-the absorbance of the isooctane standard solution measured at each corresponding wavenumber; A2930 (B), A2960 (B), A3030 (B)-The absorbance of the benzene standard solution was measured at each corresponding wavenumber. 8.1.2 Inspection of correction coefficient Each batch of samples should be tested for the correction factor, and according to the required concentration, an appropriate amount of standard oil use liquid (5.14) Or oil mist standard oil use solution (5.17), use tetrachloroethylene (5.4) to configure the standard solution of appropriate concentration, and measure according to the sample Steps are measured, and the measured concentration is calculated according to formula (1). If the relative error between the measured value and the standard value is within ± 10%, Then the correction factor can be used. Otherwise, you need to find the reason, re-determine the correction factor and calibrate the instrument, or re-prepare the inspection and calibration Standard solution for positive coefficients. Note. If the correction coefficient is set when the infrared spectrophotometer is shipped from the factory, it is not necessary to measure the correction coefficient every time. When the correction coefficient test fails, Need to re-determine the correction factor. 8.2 Determination of samples Place the prepared sample (7.3) in a 4 cm quartz cuvette, cover the cuvette cover, and use tetrachloroethylene (5.4) as For reference, the absorbances A2930, A2960 and A3030 are measured at 2930 cm-1, 2960 cm-1 and 3030 cm-1 according to the formula (1) Calculate the concentration of oil smoke or oil mist. Note. When the sample concentration exceeds the measurement range, it can be measured after dilution.

9 Calculation and presentation of results

9.1 Concentration of oil smoke and oil mist Read the absorbance at 2930 cm-1, 2960 cm-1 and 3030 cm-1, and calibrate according to X, Y, Z and F as determined in 8.1.1 The positive coefficient calculates the mass concentration ρ1 of the sample cartridge extract according to formula (1). 9.2 Calculation of emission concentration The emission concentration ρ emission (mg/m3) of the oil fume or oil mist in the exhaust gas of the stationary pollution source is calculated according to formula (6). ndV V11  Row (6) In the formula. ρ row-the emission concentration of oil fume or oil mist, mg/m3; ρ1--mass concentration of sample cartridge extract, mg/L; V1--extract volume, ml; Vnd--Dry flue gas sampling volume under standard conditions, L; for its calculation method, refer to GB/T 16157. 9.3 Results The number of digits after the decimal point of the measurement result remains the same as the detection limit of the method, and at most three significant digits are retained. 10 Precision and accuracy 10.1 Precision The six laboratories conducted three unified actual fume samples with concentrations of 0.4 mg/m3, 2.0 mg/m3 and 18.0 mg/m3. Line measurement, the relative standard deviations in the laboratory were 3.8% to 11%, 1.6% to 2.6% and 0.9% to 1.6%; The relative standard deviations are 11%, 5.8% and 3.1% respectively; the repeatability limits are 0.1 mg/m3, 0.2 mg/m3 and 0.7 mg/m3, respectively; The reproducibility limits were 0.2 mg/m3, 0.4 mg/m3 and 1.0 mg/m3, respectively. The six laboratories conducted three unified actual oil mist samples with concentrations of 0.4 mg/m3, 2.0 mg/m3 and 18.0 mg/m3, respectively. Determination, the relative standard deviations in the laboratory are 3.8% to 7.7%, 1.7% to 2.9% and 2.6% to 4.6%; The relative standard deviations are 1.0%, 3.4% and 2.4%; the repeatability limits are 0.1 mg/m3, 0.2 mg/m3 and 1.7 mg/m3, respectively; The reproducibility limits were 0.4 mg/m3, 0.2 mg/m3 and 1.9 mg/m3, respectively. 10.2 Accuracy The six laboratories have unified the actual conditions of oil fume and oil mist with concentrations of about 1.0 mg/m3, 4.0 mg/m3 and 10.0 mg/m3, respectively. The samples were subjected to standard addition determination, and the recovery rates of oil fume addition were. 88.2% to 119%, 96.7% to 105%, 83.2% to 93.6%, The final values of the recovery rate of standard addition are. 103% ± 20.4%, 102% ± 5.8%, 86.9% ± 7.6%; the recovery rate of oil mist standard addition The difference is. 85.2% ～ 90.1%, 87.3% ～ 95.1%, 82.9% ～ 91.2%; the final value of the recovery rate of the standard addition is. 87.9% ± 4.0%, 90.2% ± 5.6%, 86.4% ± 5.6%. 11 Quality assurance and quality control 11.1 The quality control of the sampling process shall be carried out in accordance with the requirements of GB/T 16157 and HJ/T 397. 11.2 The measured value of the blank test should be less than the detection limit of the method. 11.3 The standard solutions with at least 3 concentration points shall be measured every quarter to carry out the linear test of the correction coefficient. 12 Waste disposal The waste generated in the experiment should be kept in a sealed container and entrusted to a qualified unit for treatment/disposal. 13 Notes 13.1 The same batch of tetrachloroethylene should be used for the preparation of standard solutions, samples and blank tetrachloroethylene. Use different batches of tetrachloroethane If the relative error between the measured value and the standard value exceeds 10%, the standard stock solution and the With liquid. 13.2 Newly purchased metal filter cartridges or filter cartridges that collect high-concentration fume (oil mist) need to be washed with solvent or detergent. When washing When washing with detergent, rinse the detergent with pure water and dry it. In addition to using solvents or detergents, the filter cartridge can also be Burn at 400 ℃ for 1 h to remove oil pollution. The measured value of the filter cartridge after treatment is lower than the detection limit of the method before use. 13.3 Before sampling, make sure that the sampler is not contaminated by oil fumes or oil mist.

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