HJ 829-2017 English PDFUS$489.00 · In stock
Delivery: <= 5 days. True-PDF full-copy in English will be manually translated and delivered via email. HJ 829-2017: Ambient air -- Determination of inorganic elements in ambient particle matter -- Energy dispersive X-ray fluorescence spectroscopy (ED-XRF) method Status: Valid
Basic dataStandard ID: HJ 829-2017 (HJ829-2017)Description (Translated English): Ambient air -- Determination of inorganic elements in ambient particle matter -- Energy dispersive X-ray fluorescence spectroscopy (ED-XRF) method Sector / Industry: Environmental Protection Industry Standard Classification of Chinese Standard: Z15 Word Count Estimation: 21,293 Date of Issue: 5/2/2017 Date of Implementation: 7/1/2017 Regulation (derived from): Ministry of Environment Protection Announcement 2017 [16] Issuing agency(ies): Ministry of Ecology and Environment HJ 829-2017: Ambient air -- Determination of inorganic elements in ambient particle matter -- Energy dispersive X-ray fluorescence spectroscopy (ED-XRF) method---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. Ambient air -Determination of inorganic elements in ambient Particle matter - Energy dispersive X-ray fluorescence spectroscopy (ED-XRF) method National Environmental Protection Standard of the People 's Republic of China Determination of inorganic elements in ambient air particulate matter Energy dispersive X - ray fluorescence spectroscopy 2017-05-02 release 2017-07-01 implementation Ministry of Environmental Protection released Directory Preface .ii 1 Scope of application2 normative reference documents3 Principle of the method4 interference and elimination5 reagents and materials6 instruments and equipment7 samples .28 Analysis steps9 results are calculated and expressed10 precision and accuracy 11 Quality assurance and quality control 12 Precautions Appendix A (Normative Appendix) Method Detection limit and lower limit of determination Appendix B (informative) ED-XRF Example of measurement conditions Appendix C (informative) Methodological precision and method accuracyForewordIn order to implement the Environmental Protection Law of the People's Republic of China and the Law of the People's Republic of China on the Prevention and Control of Atmospheric Pollution, Environment, the protection of human health, regulate the ambient air and unorganized emissions of particulate matter in the determination of inorganic elements, the development of this standard. This standard specifies the energy dispersive X-ray fluorescence of inorganic elements in the determination of ambient air and unorganized emissions of particulate matter (ED-XRF) analysis method. This standard is the first release. Appendix A to this standard is a normative appendix, both Appendix B and Appendix C are informative. This standard is formulated by the Environmental Monitoring Division of the Ministry of Environmental Protection and the Standards Division of Science and Technology. The main drafting unit of this standard. Sino-Japanese Friendship Environmental Protection Center (National Environmental Analysis and Testing Center). Participate in this standard method to verify the units are. Institute of Earth Environment, Chinese Academy of Sciences, Shanghai Environmental Science Research Institute, Jiangsu Tianrui Instrument Co., Ltd., Shanghai Si Baiji Instrument System Co., Ltd. (Panax business unit), Shimadzu enterprise management (China) Co., Ltd., Hunan Province Environmental Monitoring Center Station, Beijing Environmental Protection Monitoring Center, Tianjin Environmental Monitoring Center, Brooke (Beijing) Technology Co., Ltd. and the Ministry of Environmental Protection Standard Samples Institute. The environmental protection department of this standard approved on May 2,.2017. This standard has been implemented since July 1,.2017. This standard is explained by the Ministry of Environmental Protection. Determination of inorganic elements in ambient airborne particles - Energy dispersive X - ray fluorescence spectrometric method1 Scope of applicationThis standard specifies the energy dispersive X-ray fluorescence spectroscopy for the determination of inorganic elements in ambient air and unorganized particulate matter. This standard applies to the use of filter-collected ambient air and non-organized emissions of sodium (Na), magnesium (Mg), Aluminum (Al), silicon (Si), phosphorus (P), sulfur (S), chlorine (Cl), potassium (K), calcium (Ca), scandium (Sc), titanium (Ti), vanadium (V), chromium (Cr), manganese (Mn), iron (Fe), cobalt (Co), nickel (Ni) (Zn), arsenic (As), selenium (Se), strontium (Sr), bromine (Br), cadmium (Cd), barium (Ba) Tin (Sn), antimony (Sb) and other elements of the determination. This standard also applies to method validation to achieve accuracy and precision Requires other inorganic elements. The limit of detection and the limit of determination are shown in Appendix A under the characteristic line conditions recommended by this standard.2 normative reference documentsThis standard refers to the terms of the following documents. For undated references, the valid version applies to this standard. Technical Requirements and Test Methods for HJ 93 Environmental Air Particulate (PM10 and PM2.5) Sampler HJ 664 ambient air quality monitoring point layout technical specifications (Trial) Technical Guidelines for Unorganized Emissions Monitoring of Air Pollutants Technical specification for manual monitoring of ambient air quality Technical requirements and testing methods for HJ/T 374 total suspended particulate matter sampler3 Principle of the methodX-ray tube produced by the primary X-ray irradiation to the formation of flat, uniform particles on the surface of the sample, the measured elements released The characteristic X-ray fluorescence enters the detector directly. X-ray fluorescence of different energy (element) is obtained by the electronic system Light spectrum. The characteristic X-ray fluorescence intensity is obtained by full spectrum fitting or specific peak area integral. Particle load In a certain range, the use of thin sample analysis technology, the measured element characteristics peak intensity and its content is proportional to.4 interference and eliminationUsually using full spectrum fitting or specific peak area integral in two ways to obtain strength. Element content is low and no interference, Optional area of a specific peak area to obtain the intensity of the area. In the presence of interference, the full spectrum fitting method should be used to overlap the peaks And the influence of the interference peak is deduced to obtain the characteristic peak intensity of the target element. Examples of interference element fitting analysis Table B.4.5 reagents and materials5.1 Load on a polyester film (Mylar film) or a polycarbonate core membrane (Nuclepolar polycarbonate membranes) Of the single element or compound standard sample, (0.5 ~ 50) g/cm2, in terms of single element content. Note. The element surface of the film is supported under the support ring for the A mode, in the support ring above the B mode. It is recommended to use B mode (see 12). 5.2 pure metal or inorganic compounds samples, the purity is greater than 99.9%. 5.3 Standard sample of mixed elements supported on polycarbonate core membrane or simulated PM2.5 standard sample, certified reference material. 5.4 quartz filter, Teflon, polypropylene and other organic filter. Note. When using XRF to measure inorganic elements in ambient air particulates, Teflon filters are more suitable than quartz filters.6 instruments and equipment6.1 Particulate Sampler. Its performance and technical specifications shall comply with the requirements of HJ/T 374 and HJ 93. 6.2 Energy Dispersive X - ray Fluorescence Spectrometer. According to the determination of light elements, can be equipped with helium replacement or vacuum function. 6.3 particle filter cut round knife, diameter 47mm. Or ceramic scissors. 6.4 tweezers (tweezers head for non-metallic material). 6.5 with a lid sample box, PVC material, diameter 47mm, 90mm. 6.6 Packaging with foil. 6.7 XRF special polypropylene film (Prolene thin film 4.0 m).7 samples7.1 Sample collection 7.1.1 Sample load The amount of particulate matter collected on the filter should not exceed 100 g/cm2 in principle, and the particulate matter of the load should be evenly distributed A diameter of at least 30 mm. The amount of particulate matter on the filter can be controlled by controlling the sampling time. Note. Excessive particulate loading can lead to sample matrix effects, deviating from the thin sample hypothesis, affecting the accuracy of the analytical results. 7.1.2 Environmental airborne particulate samples The setting of ambient air sampling points shall comply with the relevant requirements of HJ 664. The sampling process was sampled according to the particulate matter in HJ/T 194 Request execution. When the target element content is low or PM10 (PM2.5) samples are collected, the sample volume can be increased as appropriate. sampling Sampling environmental conditions should be recorded in detail. 7.1.3 Unorganized Emissions of particulate samples Unorganized Emissions Particulate Sample Collection Sets the monitoring point according to the relevant requirements of HJ/T 55, other with ambient air Product collection requirements. 7.2 Sample storage After sampling, remove the filter with tweezers, place in a dry, clean sample box (6.5), with a large flow rate The sample of the quartz filter collected by the sampler can be folded and wrapped with the foil (6.6) for packaging and recorded according to the sampling requirements. The samples were stored in a dry, clean, room temperature environment in a silica gel dryer. 7.3 Sample handling Particle samples collected by the small flow sampler can be placed directly into the sample cup. Large, medium flow sampler collected by quartz filter Particulate samples need a diameter of 47 mm round knife (6.3) cut into a diameter of 47 mm filter disc, to be tested. The above operation Avoid contamination of the sample surface.8 Analysis steps8.1 Instrument measurement conditions According to the instrument operation manual, select the appropriate measurement condition establishment method. The main measurement parameters that need to be optimized are. to be tested Elements of the grouping; characteristic lines and measurement time; filter (or secondary target); X-ray tube voltage and current; interference elements And its interference coefficient determination. See Appendix B for an example of instrument measurement parameters. 8.2 Standard sample and pure element sample measurement According to the instrument operation manual, in the instrument software related interface to establish a standard sample data table. Enter the blank film and Standard values for each element in the standard sample (5.1) of the film. The series of standard samples were measured according to the optimized measurement conditions (8.1). The number of standard samples of the film can be selected according to the laboratory conditions between 2 and 4 (excluding the blank filter), the standard sample content is large The range is as follows. 0.5 to 2 μg/cm2, 3 to 8 μg/cm2, 15 to 25 μg/cm 2, and 40 to 60 μg/cm 2. The characteristic spectral scanning spectra of the pure element (5.2) were measured under the same measurement conditions. All the relevant elements in the standard sample Strength and pure element spectra should be completed in the same batch test. According to the linear regression model and procedure provided by the instrument, the content of the standard blank filter, the series of film standards and Strength regression analysis, the establishment of calibration curve, find the regression equation slope and stored in the computer. 8.3 Sample measurement The blank filter and the sample filter were measured under the same conditions as the standard sample (8.2). Usually using full spectrum fitting or Specific peak area integral in two ways to obtain strength. When the element content is low and there is no interference, the available area spectral net area is obtained Take strength. When the target element is interfering, the full spectrum fitting method should be used to analyze the overlapping peaks and subtract the interference peak Influence, get the target element characteristic spectral peak intensity. According to the sample filter and blank filter in the target element strength and calibration curve To calculate the target element content in the membrane sample.9 Results calculation and representation9.1 Results calculation Particulate matter content in the sample by (1). Where. A - the area (cm2) of particulate matter loaded on the filter; I - the target element X - ray fluorescence intensity (cps or cps/mA) in the sample filter; I 0 - the target element X-ray fluorescence intensity (cps or cps/mA) in the blank filter; B - calibration curve slope [cps/(g/cm2) or (cps/mA)/(g/cm2)]; V - standard volume (273 K, 101.325 Pa) sampling volume (m3); - Target element content in particle samples (g/m3). 9.2 The result is shown The number of digits retained after the decimal point of each element is consistent with the detection limit of the method. Bit effective number. Particulate sample test results can also be expressed in μg/cm2. 10 precision and accuracy 10 laboratories on the unified provision of atmospheric particulate samples, filter quality control samples, with different particle loading 3 TSP samples (quartz filter), 3 PM2.5 samples (polypropylene filter) and 2 unorganized particulate matter samples (quartz Filter), measured by X-ray fluorescence spectroscopy. The mathematical results of the measurement result are obtained, and the precision of the method is obtained The relative standard deviation range, the inter-laboratory relative standard deviation, the repeatability limit, and the reproducibility limit) in the laboratory The accuracy of the method (the relative error range and the relative error of the measured values of each element) are given in Appendix C. 11 quality assurance and quality control 11.1 filter blank Each batch of samples shall be analyzed for at least two blank filter samples purchased in the same batch as the sampling filters. Used to collect unorganized rows The determination of the target element in the blank sample of the particulate matter shall not be greater than one tenth of the target element emission standard limit. no Then, should be appropriate to increase the sampling volume, so that the target element of particulate matter measured value was significantly higher than the filter blank value. Used to collect the environment empty The determination of the target element in the blank filter of the particulate matter should be less than the lower limit of the method. 11.2 Calibration curve The calibration curve can be used for long periods of time when the analytical method is established. The calibration curve should be checked before each batch. To close the calibration The middle of the curve of the laboratory quality control samples (or different sources of membrane samples) to confirm the analysis, the relative error should meet the table 1 request. Otherwise, the calibration curve or calibration offset should be reestablished. Table 1 quality control samples of the various elements of laboratory testing accuracy requirements Element relative error range (%) Al, Si, K, Ca, Cr, Mn, Cu, Se, Sr, Ti, Fe, Ni, Zn, Co, Ba, Pb, Cl -10 to 10 Na, Mg, As, Cd, Sn, Sb, S, P, V, Sc, Br -20 to 20 11.3 precision If the particulate filter sample can be repeatedly measured (such as quartz membrane samples, polypropylene filter samples), each batch of samples should be drawn Take 10% of the sample for repeated determination. If the number of samples is less than 10, it should be at least one. When the element content is higher than the measured When the limit is set, the relative deviation of the parallel samples shall meet the requirements of Table 2. Table 2 of the elements parallel to the determination of precision requirements 11.4 Accuracy The method of this method should be verified by analyzing the standard sample of the film. If the measurement error exceeds the allowable range , Stop the analysis of the sample, find the cause. When available, validated samples of atmospheric particulate matter can be used. Test After the results meet the requirements, in order to continue the analysis. After the analysis of each batch of actual samples can be analyzed at the same time the laboratory Quality control samples (or different source filter standard), when the element content is higher than the lower limit of determination, the laboratory quality control sample indoor test Accuracy should meet the requirements of Table 1. Determination of mixed elements film (including Al, Si, Fe, Pb, Cu, Zn, Ni, Mn, Cr and other elements) It can be done before or after all samples are measured. The relative value of the measured value and the standard indication should be less than 10%. This standard and laboratory quality control series of measured values can be used to draw quality control charts and calculate the precision during the period. Period precision The multiplication value multiplied by 2 can be used to evaluate the measurement results for extended uncertainty. If the laboratory conditions are limited, you can consider the use of standard equipment provided by the manufacturer to verify. 12 Precautions ED-XRF determination process, for the next instrument, in order to prevent the particles falling into the instrument, and sometimes in its The filter sample surface is covered with a layer of XRF-specific polypropylene film (6.7) protective instrument. If the above considerations are made in the determination of the sample, Establish the calibration curve to determine the standard sample strength to take the same measures, the two measurement conditions should be consistent. The film standard can be selected according to the position of the support ring. The recommended selection is consistent with the actual sample measurement surface Mode, ie B mode (5.1 note). If the film sample is in the A mode, it should be placed on the surface of the actual filter sample Thin film standard support ring with the same thickness of the ring. If the instrument is under the control, put the ring in the sample cup and then into the filter sample Product, measured face down; for the photo, the sample cup in the first sample into the filter, the measurement side up, and then into the ring Fixed, so that the actual sample and film samples subject to X-ray irradiation distance consistent.Appendix A(Normative appendix) Method detection limit and lower limit of determination Table A.1 Characteristic lines of each element, method detection limit and lower limit of determination Note. 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