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HJ 1133-2020 English PDF

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HJ 1133-2020: Ambient air and waste gas - Determination of arsenic, selenium, bismuth, antimony in ambient particle matter - Atomic fluorescence spectrometry
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Standard ID	Contents [version]	USD	STEP2	[PDF] delivered in	Standard Title (Description)	Status	PDF
HJ 1133-2020	English	349	Add to Cart	3 days [Need to translate]	Ambient air and waste gas - Determination of arsenic, selenium, bismuth, antimony in ambient particle matter - Atomic fluorescence spectrometry	Valid	HJ 1133-2020

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Basic data

Standard ID	HJ 1133-2020 (HJ1133-2020)
Description (Translated English)	Ambient air and waste gas - Determination of arsenic, selenium, bismuth, antimony in ambient particle matter - Atomic fluorescence spectrometry
Sector / Industry	Environmental Protection Industry Standard
Classification of Chinese Standard	Z15
Word Count Estimation	15,152
Date of Issue	2020-05-15
Date of Implementation	2020-08-15
Regulation (derived from)	Ministry of Ecology and Environment Announcement No. 29 of 2020
Issuing agency(ies)	Ministry of Ecology and Environment

HJ 1133-2020: Ambient air and waste gas - Determination of arsenic, selenium, bismuth, antimony in ambient particle matter - Atomic fluorescence spectrometry

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Ambient air and waste gas - Determination of arsenic, selenium, bismuth, antimony in ambient particle matter - Atomic fluorescence spectrometry National Environmental Protection Standards of the People's Republic of China Determination of arsenic, selenium, bismuth, and antimony in ambient air and waste gas particles. Atomic fluorescence method 2020-05-15 release 2020-08-15 Implementation Issued by the Ministry of Ecology and Environment

Foreword...ii 1 Scope of application...1 2 Normative references...1 3 Principles of the method...1 4 Interference and cancellation...2 5 Reagents and materials...2 6 Instruments and equipment...4 7 Sample...4 8 Analysis steps...6 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) method detection limit and lower limit of determination...10 Appendix B (Informative Appendix) Method Precision and Accuracy...11

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 To ensure human health, regulate the determination of arsenic, selenium, bismuth, and antimony in ambient air and waste gas particles, and formulate this standard. This standard specifies the atomic fluorescence method for the determination of arsenic, selenium, bismuth, and antimony in ambient air and exhaust particles. Appendix A of this standard is a normative appendix, and Appendix B is an informative appendix. This standard is issued for the first time. This standard was formulated by the Department of Ecological Environment Monitoring and the Department of Regulations and Standards of the Ministry of Ecology and Environment. Drafting organization of this standard. China Environmental Monitoring Center. The verification unit of this standard. Qinghai Province Ecological Environment Monitoring Center, Liaoning Province Ecological Environment Monitoring Center, Inner Mongolia Autonomous Region Environmental Monitoring Center Station, Taiyuan Ecological Environment Monitoring Center of Shanxi Province, Yangzhou Environmental Monitoring Center of Jiangsu Province, and Zhanjiang Environmental Protection Monitoring Station. This standard was approved by the Ministry of Ecology and Environment on May 15, 2020. This standard will be implemented on August 15, 2020. This standard is interpreted by the Ministry of Ecology and Environment. 1 Determination of arsenic, selenium, bismuth and antimony in ambient air and waste gas particles Atomic fluorescence Warning. Nitric acid and hydrochloric acid are highly corrosive and oxidizing. The sample digestion process should be carried out in a fume hood. The experimenters should pay attention to wearing protective equipment. Avoid breathing into the respiratory tract or contact with skin and clothing.

1 Scope of application

This standard specifies the atomic fluorescence method for the determination of arsenic, selenium, bismuth, and antimony in ambient air and exhaust particles. This standard applies to ambient air, unorganized emission monitoring point air and fixed pollution sources organized emission of exhaust particles Determination of arsenic (As), selenium (Se), bismuth (Bi), and antimony (Sb). When the ambient air sampling volume is 150 m3 (actual state) and the sample pretreatment constant volume is 50.0 ml, the method is The detection limit is 0.2 ng/m3～2 ng/m3, the lower limit of determination is 0.8 ng/m3～8 ng/m3; air sampling at monitoring points for fugitive emissions When the volume is 50 m3 (standard state) and the sample pretreatment constant volume is 50.0 ml, the method detection limit is 0.4 ng/m3 to 4 ng/m3, The lower limit of determination is 1.6 ng/m3～16 ng/m3; the sampling volume of organic emission from fixed pollution sources is 0.600 m3 (standard state Dry flue gas), when the sample pretreatment constant volume is 100.0 ml, the detection limit of the method is 0.1 g/m3～0.7 g/m3. The limit is 0.4 g/m3～2.8 g/m3.See Appendix A for details.

2 Normative references

This standard quotes the following documents or their clauses. For undated reference documents, their valid versions are applicable to this standard. GB/T 16157 Determination of particulate matter in exhaust from stationary sources and sampling method for gaseous pollutants GB/T 21191 Atomic Fluorescence Spectrometer HJ/T 48 Technical requirements for soot sampler HJ/T 55 Technical Guidelines for Monitoring Unorganized Emissions of Air Pollutants HJ 93 Ambient air particulate matter (PM10 and PM2.5) sampler technical requirements and detection methods HJ 194 Technical specification for manual monitoring of ambient air quality HJ/T 374 Technical requirements and testing methods for total suspended particulate matter sampler HJ/T 397 Fixed source exhaust gas monitoring technical specification HJ 664 Technical specification for the layout of ambient air quality monitoring points (for trial implementation)

3 Principles of the method

Use a filter membrane or a filter cartridge to collect particulate matter in the air or waste gas. After the sample is digested by a mixed acid of nitric acid and hydrochloric acid, it enters the atomic fluorescence Optical spectrometer, the arsenic, selenium, bismuth, and antimony in the sample undergo oxidation-reduction with potassium borohydride (or sodium borohydride) under acidic conditions The reaction produces arsine, hydrogen selenide, hydrogen bismuth, and hydrogen antimonide gas. The hydride forms ground-state atoms in the argon-hydrogen flame. 2 element lamps (arsenic, selenium, bismuth, antimony) emit atomic fluorescence under excitation, and the intensity of atomic fluorescence within a certain concentration range It is proportional to the content of the elements in the test solution.

4 Interference and elimination

Transition metal elements such as copper may interfere with the determination. Adding thiourea-ascorbic acid mixed solution (5.17) can basically Eliminate interference. Under the experimental conditions of this standard, the sample contains Cu2 below 100 mg/L, Fe3 below 50 mg/L, Co2 below 1 mg/L, Pb2 below 10 mg/L and Mn2 below 150 mg/L do not affect the determination.

5 Reagents and materials

Unless otherwise specified, analytical reagents that meet national standards are used for analysis, and the experimental water is newly prepared deionized water or distilled water. 5.1 Hydrochloric acid. ρ(HCl)=1.19 g/ml, excellent grade pure. 5.2 Nitric acid. ρ(HNO3)=1.42 g/ml, excellent grade pure. 5.3 Potassium hydroxide (KOH). 5.4 Sodium hydroxide (NaOH). 5.5 Potassium borohydride (KBH4). 5.6 Thiourea (CH4N2S). 5.7 Ascorbic acid (C6H8O6). 5.8 Arsenic trioxide (As2O3). pure superior grade. 5.9 Selenium powder. high purity (mass fraction above 99.99%). 5.10 Bismuth. high purity (above 99.99% mass fraction). 5.11 Antimony trioxide (Sb2O3). pure superior grade. 5.12 Hydrochloric acid solution. 5 95 Measure 50 ml of hydrochloric acid (5.1) and dissolve in about 500 ml of water, then dilute with water and dilute to 1 L. 5.13 Hydrochloric acid solution. 1 1 Measure 500 ml of hydrochloric acid (5.1) and dissolve it in about 400 ml of water, then dilute with water and dilute to 1 L. 5.14 Hydrochloric acid solution. c(HCl)=1 mol/L Measure 41.6 ml of hydrochloric acid (5.1), dissolve it in a certain amount of water, and dilute with water to 500 ml. 5.15 Nitric acid-hydrochloric acid mixed solution Measure 55.5 ml of nitric acid (5.2) and 166.5 ml of hydrochloric acid (5.1) respectively, dissolve in about 500 ml of water, and dilute with water Relieve and dilute to 1 L. 5.16 Potassium borohydride solution. ρ(KBH4)=20 g/L Weigh 0.5 g of potassium hydroxide (5.3) dissolved in 100 ml of water, stir the glass rod until it is completely dissolved, then add 2.0 g Potassium borohydride (5.5), stir to dissolve, prepare when used. Note. Sodium hydroxide and sodium borohydride can also be used to prepare sodium borohydride solution. 5.17 Thiourea-Ascorbic Acid Mixed Solution Weigh 5 g each of thiourea (5.6) and ascorbic acid (5.7), dissolve in 100 ml of water, mix well, and prepare when used. 35.18 Sodium hydroxide solution. c (NaOH) = 1 mol/L Weigh 20.0 g of sodium hydroxide (5.4), dissolve in water, and dilute to 500 ml after cooling. 5.19 Arsenic standard solution 5.19.1 Arsenic standard stock solution. ρ(As)=100 mg/L Buy commercially available certified reference materials, or weigh 0.1320 g of premium grade pure arsenic trioxide (5.8) dried at 105°C for 2 hours Dissolve in 5 ml sodium hydroxide solution (5.18), neutralize with hydrochloric acid solution (5.14) until phenolphthalein red fades, and dilute to volume with water To 1000 ml, mix well. It can be stored for 2 years at 4°C. 5.19.2 Arsenic standard intermediate solution. ρ(As)=1.00 mg/L Pipette 5.00 ml arsenic standard stock solution (5.19.1), place it in a 500 ml volumetric flask, add 100 ml hydrochloric acid solution (5.13), dilute to the mark with water and mix well. It can be stored for 1 year at 4°C. 5.19.3 Arsenic standard liquid. ρ(As)=100 μg/L Pipette 10.00 ml arsenic standard intermediate solution (5.19.2), place it in a 100 ml volumetric flask, add 20 ml hydrochloric acid solution (5.13), Dilute to the mark with water and mix well. It can be stored for 30 days at 4°C. 5.20 Selenium standard solution 5.20.1 Selenium standard stock solution. ρ(Se)=100 mg/L Purchase a commercially available certified reference material, or weigh 0.1000 g selenium powder (5.9), place it in a 100 ml beaker, and add 20 ml Nitric acid (5.2) is heated and dissolved at low temperature and then cooled to the greenhouse, transferred to a 1000 ml volumetric flask, dilute to the mark with water, and mix well. It can be stored for 2 years at 4°C. 5.20.2 Selenium standard intermediate solution. ρ(Se)=1.00 mg/L Pipette 5.00 ml selenium standard stock solution (5.20.1), place it in a 500 ml volumetric flask, add.200 ml hydrochloric acid solution (5.13), dilute to the mark with water and mix well. It can be stored for 100 days at 4℃. 5.20.3 Selenium standard liquid. ρ(Se)=100 μg/L Pipette 10.00 ml selenium standard intermediate solution (5.20.2), place it in a 100 ml volumetric flask, add 40 ml hydrochloric acid solution (5.13), Dilute to the mark with water and mix well. Equipped when used. 5.21 Bismuth standard solution 5.21.1 Bismuth standard stock solution. ρ(Bi)=100 mg/L Purchase a commercially available certified reference material, or weigh 0.1000 g of bismuth (5.10), place it in a 100 ml beaker, and add 20 ml Nitric acid (5.2), heat at low temperature to dissolve completely, cool, transfer to a 1000 ml volumetric flask, dilute to the mark with water, and mix. It can be stored for 2 years at 4°C. 5.21.2 Bismuth standard intermediate solution. ρ(Bi)=1.00 mg/L Pipette 5.00 ml bismuth standard stock solution (5.21.1), place it in a 500 ml volumetric flask, add 100 ml hydrochloric acid solution (5.13), dilute to the mark with water and mix well. It can be stored for 1 year at 4°C. 5.21.3 Bismuth standard liquid. ρ(Bi)=100 μg/L Pipette 10.00 ml bismuth standard intermediate solution (5.21.2), place it in a 100 ml volumetric flask, add 20 ml hydrochloric acid solution (5.13), Dilute to the mark with water and mix well. Available when used. 5.22 Antimony standard solution 5.22.1 Antimony standard stock solution. ρ(Sb)=100 mg/L Purchase a commercially available certified reference material, or weigh out 0.1197 g of antimony trioxide (5.11) dried at 105°C for 2 hours, 4 Dissolve in 80 ml of hydrochloric acid (5.1), transfer to a 1000 ml volumetric flask, add 120 ml of hydrochloric acid (5.1), and dilute to volume with water To the mark, mix well. It can be stored for 2 years at 4°C. 5.22.2 Antimony standard intermediate solution. ρ(Sb)=1.00 mg/L Pipette 5.00 ml antimony standard stock solution (5.22.1), place it in a 500 ml volumetric flask, and add 100 ml hydrochloric acid solution (5.13), dilute to the mark with water and mix well. It can be stored for 1 year at 4°C. 5.22.3 Antimony standard liquid. ρ(Sb)=100 μg/L Pipette 10.00 ml antimony standard intermediate solution (5.22.2), place it in a 100 ml volumetric flask, add 20 ml hydrochloric acid solution (5.13), Dilute to the mark with water and mix well. Available when used. 5.23 Quartz or glass fiber filter membrane The retention efficiency of particles larger than 0.3 μm is not less than 99%. 5.24 Quartz or glass fiber filter cartridge The retention efficiency of particles larger than 0.3 μm is not less than 99.9%. 5.25 Argon gas. purity ≥99.99%.

6 Apparatus and equipment

6.1 Particulate matter sampler The performance and technical indicators of the ambient air particulate matter sampler used should comply with the requirements of HJ/T 374 and HJ 93.Pollution The sampling flow rate of the source exhaust particulate matter sampler is 5 L/min～80 L/min, and other performance and technical indicators should meet the requirements of HJ/T 48. 6.2 The atomic fluorescence spectrometer should meet the requirements of GB/T 21191, with elements lamps of arsenic, selenium, bismuth and antimony. 6.3 Microwave digestion device 6.3.1 Microwave digestion instrument. with temperature control and temperature program functions. 6.3.2 Microwave digestion container. PTFE or similar material. 6.3.3 Rotating disk. A rotating disk must be used in the microwave digestion process to ensure the uniformity of the sample receiving the microwave. 6.4 Electric heating plate. temperature control accuracy ±5℃. 6.5 Constant temperature water bath device. temperature control accuracy ±1℃. 6.6 Analytical balance. the accuracy is 0.0001 g. 6.7 Ceramic scissors. 6.8 Teflon beaker. 6.9 Commonly used instruments and equipment in general laboratories.

7 samples

7.1 Sample collection 7.1.1 Ambient air sample The layout and sampling process of ambient air sampling points shall be implemented in accordance with the requirements for particulate matter sampling in HJ 664 and HJ 194. 57.1.2 Air samples at monitoring points for fugitive emissions The air sample collection at the unorganized emission monitoring point shall be in accordance with the relevant requirements in HJ/T 55.The monitoring point shall be set up, and the rest shall be the same as the environmental air sample collection requirements. 7.1.3 Organized emissions samples from stationary sources The sampling process of stationary pollution source waste gas shall be implemented in accordance with the requirements of particulate matter sampling in GB/T 16157 and HJ/T 397. Use the dust sampler to collect particulate matter samples not less than 0.600 m3 (standard state dry flue gas), when the concentration of heavy metals is low The sampling volume can be increased appropriately. If the temperature of the flue gas in the pipeline is higher than the melting point of the relevant metal elements to be collected, cooling measures should be taken. Make the temperature of the flue gas before entering the filter cartridge lower than the melting point of the relevant metal elements. 7.2 Sample storage After the filter membrane sample is collected, put it in a sample box or sample bag for storage; after collecting the filter cartridge sample, fold the seal inward and place it vertically Return to the original sampling sleeve for airtight storage. The samples should be stored in a dry, ventilated, dark, and room temperature environment. 7.3 Preparation of samples 7.3.1 Microwave digestion Take the whole or part of the filter membrane sample, cut into small pieces with ceramic scissors (6.7) and place in the digestion tank, add 15.0 ml nitric acid -Hydrochloric acid mixed solution (5.15), so that the filter membrane is immersed, capped, placed in the digestion tank assembly and screwed tightly, and placed on the microwave turntable Shelf. Set the digestion temperature to.200°C and the digestion duration to 15 min, and start the digestion. After the digestion is over, remove the digestion Tank components, cool, rinse the inner wall with water, add about 10 ml of water, let stand for half an hour for extraction, filter, and dilute to 50.0 ml, to be tested. If the sample volume of the filter membrane is large, the volume of the nitric acid-hydrochloric acid mixed solution (5.15) can be appropriately increased. Submerge the filter membrane. Take the entire filter cartridge sample, cut into small pieces, add 40.0 ml nitric acid-hydrochloric acid mixed solution (5.15), so that the filter cartridge is immersed Among them, the other operations are the same as the filter sample, and the final volume is 100.0 ml. 7.3.2 Electric heating plate digestion Take the whole or part of the filter membrane sample, cut into small pieces with ceramic scissors (6.7) and place in a PTFE beaker (6.8), Add 15.0 ml of nitric acid-hydrochloric acid mixed solution (5.15) to immerse the filter membrane in it, cover with a watch glass, and heat to reflux at 100°C Cool down after 2.0 hours. Rinse the inner wall with water, add about 10 ml of water, let stand for half an hour for extraction, filter, and dilute with water To 50.0 ml, to be tested. If the sample volume of the filter membrane is large, the volume of the nitric acid-hydrochloric acid mixed solution (5.15) can be appropriately increased. Submerge the filter membrane. Take the entire filter cartridge sample, cut into small pieces, add 40.0 ml of nitric acid-hydrochloric acid mixed solution (5.15), so that the filter cartridge is immersed, The other operations are the same as the filter sample, and the final volume is adjusted to 100.0 ml. 7.3.3 Preparation of samples to be tested Pipette 5.0 ml of the digested sample into a 10 ml colorimetric tube, add hydrochloric acid solution (5.13), sulfur Urea-ascorbic acid mixed solution (5.17), mix well, and place at room temperature for 30 min. Dilute to the mark with water and mix well. 7.4 Laboratory blank Take the blank filter membrane (or filter cartridge) of the same batch as the sample, and carry out the experiment according to the same procedure of sample preparation (7.3) Preparation of blank samples in the chamber. 7.5 Blank in the whole program Take the blank filter membrane (or filter cartridge) of the same batch as the sample, store and transport it under the same conditions as the sample. Will be blank The filter membrane (or filter cartridge) is installed on the sampler without sampling. The exposure time of the blank filter membrane (or filter cartridge) at the sampling site is different from that of the sample. The product filter membrane (or filter cartridge) has the same time from being taken out until it is installed to the sampler, and then the blank filter membrane (or filter cartridge) is removed and sampled Ship the product back to the laboratory together, and prepare a blank sample for the whole procedure according to the same steps as the sample preparation (7.3).

8 Analysis steps

8.1 Measurement conditions The atomic fluorescence spectrometer is turned on and preheated, and the lamp current, negative high voltage, carrier gas flow, shielding are set according to the instrument manual For working parameters such as air flow, see Table 2 for reference conditions. 8.2 Establishment of calibration curve 8.2.1 Preparation of calibration series 8.2.1.1 Arsenic calibration series Pipette 0 ml, 0.50 ml, 1.00 ml, 2.00 ml, 4.00 ml and 5.00 ml arsenic standard use solution (5.19.3) In a 50 ml volumetric flask, add 10.0 ml hydrochloric acid solution (5.13), 10.0 ml thiourea-ascorbic acid mixed solution (5.17), Leave it at room temperature for 30 minutes (when the room temperature is lower than 15°C, keep it in a 30°C water bath for 30 minutes), dilute to the mark with water, and mix. 78.2.1.2 Selenium Calibration Series Pipette 0 ml, 1.00 ml, 2.00 ml, 3.00 ml, 4.00 ml and 5.00 ml selenium standard use solution (5.20.3) In a 50 ml volumetric flask, add 10.0 ml hydrochloric acid solution (5.13), dilute to the mark with water, and mix. 8.2.1.3 Bismuth calibration series Pipette 0 ml, 0.50 ml, 1.00 ml, 2.00 ml, 4.00 ml and 5.00 ml bismuth standard solution (5.21.3) In a 50 ml volumetric flask, add 10.0 ml hydrochloric acid solution (5.13), dilute to the mark with water, and mix. 8.2.1.4 Antimony calibration series Pipette 0 ml, 1.00 ml, 2.00 ml, 3.00 ml, 4.00 ml and 5.00 ml antimony standard solution (5.22.3) In a 50 ml volumetric flask, add 10.0 ml hydrochloric acid solution (5.13), 10.0 ml thiourea-ascorbic acid mixed solution (5.17), Leave it at room temperature for 30 minutes (when the room temperature is lower than 15°C, keep it in a 30°C water bath for 30 minutes), dilute to the mark with water, and mix. The concentration of arsenic, selenium, bismuth, and antimony calibration series solutions are shown in Table 3. 8.2.2 Establish calibration curve Use potassium borohydride solution (5.16) as the reducing agent and hydrochloric acid solution (5.12) as the carrier, from low concentration to high concentration in sequence Determine the atomic fluorescence intensity of arsenic, selenium, bismuth and antimony calibration series standard solutions. Take the mass concentration of the corresponding element as the abscissa, Use atomic fluorescence intensity as the ordinate to establish a calibration curve. 8.3 Sample measurement Import the prepared sample into the atomic fluorescence spectrometer, and perform the measurement under the same instrument working conditions as the calibration curve. set. If the concentration of the measured element exceeds the concentration range of the calibration curve, it should be diluted and re-measured. 8.4 Blank test Determine the laboratory blank and the full procedure blank according to the same procedure as the sample determination (8.3).

9 Calculation and presentation of results

9.1 Result calculation 9.1.1 Membrane sample The concentration of the target element in the filter membrane sample is calculated according to formula (1). 9.2 Presentation of results The number of digits retained after the decimal point of the determination result is consistent with the detection limit of the method, and up to three significant digits are retained. 10 Precision and accuracy 10.1 Precision 6 laboratories separately tested 3 simulated samples of air particulate matter standard materials with different contents of arsenic, selenium, bismuth, and antimony. Different content of exhaust particulate matter standard material simulation sample, 1 actual filter membrane sample and 1 exhaust particulate matter simulation sample (flying Ash samples) were measured. Four laboratories used microwave digestion method to process the samples, and two laboratories used electric heating. The sample is processed by the plate digestion method, see Appendix B for details. 10.2 Accuracy

6 laboratories respectively performed a simulated sample of air particulate matter reference material and a simulated sample of exhaust particulate matter reference material

The samples were measured, 4 laboratories used microwave digestion method to process samples, 2 laboratories used electric heating plate digestion For processing samples, see Appendix B for details. 911 Quality Assurance and Quality Control 11.1 At least 2 laboratory blanks and 1 full-procedure blank sample should be analyzed for each batch of samples. The target elements in the blank samples should be measured. The value should be lower than the lower limit of the method. 11.2 A calibration curve should be drawn for each sample analysis, and the correlation coefficient should be greater than or equal to 0.999. 11.3 Check the concentration of the midpoint of the calibration curve every 20 samples, and the relative error should be within ±20%. 11.4 Take 10% of the filter membrane samples for parallel sample determination. When the number of samples is less than 10, at least one parallel double sample should be determined. The relative deviation of the measurement results should be ≤20%. 12 Waste treatment The waste liquid generated during the experiment cannot be dumped at will, and a qualified unit should be entrusted for disposal in accordance with regulations. 13 matters needing attention 13.1 The results shall be calculated according to the state required by the corresponding quality standards or emission standards. 13.2 The flow rate calibration and air tightness check of the sampler shall be carried out before each sampling. 13.3 The glassware used in the experiment was first rinsed with tap water, then soa...

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