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HJ 830-2017: Ambient air -Determination of inorganic elements in ambient particle matter- Wavelength dispersive X-ray fluorescence spectroscopy (WD-XRF) method
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Ambient air -Determination of inorganic elements in ambient particle matter- Wavelength dispersive X-ray fluorescence spectroscopy (WD-XRF) method
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HJ 830-2017
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Basic data | Standard ID | HJ 830-2017 (HJ830-2017) | | Description (Translated English) | Ambient air -Determination of inorganic elements in ambient particle matter- Wavelength dispersive X-ray fluorescence spectroscopy (WD-XRF) method | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z15 | | Word Count Estimation | 25,241 | | 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 830-2017: Ambient air -Determination of inorganic elements in ambient particle matter- Wavelength dispersive X-ray fluorescence spectroscopy (WD-XRF) method
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Ambient air -Determination of inorganic elements in ambient
Particle matter-Wavelength dispersive X-ray fluorescence
Spectroscopy (WD-XRF) method
National Environmental Protection Standard of the People 's Republic of China
Determination of inorganic elements in ambient air particulate matter
Wavelength Dispersive X - Ray Fluorescence Spectroscopy
2017-05-02 release
2017-07-01 implementation
Ministry of Environmental Protection released
Directory
Preface .ii
1 Scope of application
2 normative reference documents
3 Principle of the method
4 interference and elimination
5 reagents and materials
6 instruments and equipment
7 samples .2
8 Analysis steps
9 results are calculated and expressed
10 precision and accuracy
11 Quality assurance and quality control
12 Precautions
Appendix A (normative) method detection limit and lower limit of determination
Appendix B (informative) Examples of interference factor correction factor calculation
Appendix C (informative) WD-XRF Example of measurement conditions
Appendix D (informative) Methodological precision and method accuracy
Foreword
In 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 wavelength dispersion X-ray fluorescence of inorganic elements in the determination of ambient air and unorganized emissions of particulate matter
(WD-XRF) analysis method.
This standard is the first release.
Annex A to this standard is a normative appendix, Appendix B, Appendix C and Appendix D are informative appendices.
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 to verify the units are. Hunan Province Environmental Monitoring Center Station, Beijing Environmental Protection Monitoring Center, Tianjin
Environmental Monitoring Center, Ministry of Environmental Protection Standard Samples Institute, Brook (Beijing) Technology Co., Ltd., Shimadzu Enterprise Management
(China) Co., Ltd., Institute of Earth Environment, Chinese Academy of Sciences, Shanghai Environmental Science Research Institute, Jiangsu Tianrui Instrument Unit
Co., Ltd., Shanghai Si Baiji Instrument System Co., Ltd. (Panax business unit).
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 - Wavelength dispersive X - ray fluorescence spectrometric method
1 Scope of application
This standard specifies the wavelength dispersion X-ray fluorescence of inorganic elements in the determination of ambient air and unorganized emissions.
(WD-XRF).
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 documents
This 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 sampler
JJG 810 Wavelength Dispersive X - Ray Fluorescence Spectrometer
3 Principle of the method
When the primary X-ray produced by the X-ray tube is irradiated onto the surface of the flat and uniform particle sample, the element to be measured is released
The characteristic X-ray is crystallized by the crystal, and the detector measures the X-ray fluorescence intensity at a selected characteristic wavelength corresponding to 2 ° C.
Particulate matter load in a certain range, the use of thin sample analysis technology, X-ray fluorescence intensity is proportional to the measured element content.
4 interference and elimination
Lead LNP line has significant interference with arsenic Kui line. Can be used to eliminate the interference factor of the interference element. The correction factor is real
The calculation is shown in Appendix B.
5 reagents and materials
5.1 Commercially available argon-methane mixed gas (P10), referred to as argon gas, 90% argon 10% methane.
5.2 Load on a polyester film (Mylar film) or a polycarbonate core membrane (Nuclepore 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 the B mode (see 12.2).
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 equipment
6.1 Particulate Sampler. Its performance and technical specifications shall comply with the requirements of HJ/T 374 and HJ 93.
6.2 Wavelength Dispersive X - Ray Fluorescence Spectrometer. Equipped with a suitable sample cup. The main test items and measurement performance should be accurate
The requirements of the A or B level specified in the JJG 810.
Note. The sample cup should have a gas channel design to avoid the vacuum, the filter surface measurement pressure caused by uneven imbalance. Filter in the sample
The cup should be fixed in a suitable way.
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 samples
7.1 Sample collection
7.1.1 Sample load
The amount of particulate matter collected on the filter should not exceed 100 g/cm2 in principle. Load the particles to 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 (or PM2.5) samples are collected, the sample volume may be increased as appropriate. Mining
Samples should be recorded in detail when sampling environmental conditions.
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 and place in a dry, clean sample box (6.5). Large Flow
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 47mm round knife or ceramic scissors (6.3) cut into a diameter of 47 mm filter disc to be
Measurement. The above operation should avoid contamination of the sample measurement surface.
8 Analysis steps
8.1 Instrument measurement conditions
Refer to the instrument operation manual to establish the measurement method. Select the target element from the database to measure the line and correct it. Reference instrument
The database provided by the manufacturer selects the best working conditions, including the X-ray tube voltage and current, the elemental analysis line and
Background points, spectroscopic crystals, collimators, detectors, pulse height distribution (PHA or PHD), and filters. Analyze the line
And background measurement time can be adjusted according to actual needs. Refer to Appendix C for an example of instrument reference measurement conditions.
8.2 Calibrate the sample measurement
According to the instrument operation manual, in the instrument software related interface to establish the standard sample data table. Enter blank film and film
Standard values for each element in standard sample (5.2). The above series of standard samples were measured according to the optimized measurement conditions (8.1).
The number of standard samples of the film according to laboratory conditions, can be selected between 2 to 4 (not including blank filter), standard sample content
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.
According to the linear regression model and procedure provided by the instrument, the content and intensity of the series of film samples are regressed
Analysis, the establishment of calibration curve, find the regression equation slope and stored in the computer.
If necessary, PHA adjustment should be repeated after each change of argon gas (5.1), and the measurement conditions are checked. Using flow
The gas proportional counter as a detector for the relevant elements (eg Al, Si, etc.) standard samples should be re-measured its strength for verification.
The calibration curve should be updated if necessary, or calibrated with drift calibration (11.1).
8.3 Sample measurement
The blank filter and the sample filter were measured according to the same measurement conditions (8.1) as the standard sample. According to the sample filter and empty
The characteristic value of the target element in the white filter was measured and the slope of the calibration curve was calculated.
9 Results calculation and representation
9.1 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 in the sample filter X - ray fluorescence intensity (kcps);
I 0 - the target element in the blank filter X - ray fluorescence intensity (kcps);
B - calibration curve slope [kcps/(g/cm2)];
V - standard volume (273 K, 101.325 Pa) sampling volume (m3);
- Target element content in particle samples (g/m3).
Elemental arsenic calculation results should be deducted according to the method of Appendix B lead interference.
9.2 The result is shown
The number of digitally retained digits after the decimal point of each element is consistent with the detection limit of the method, and the test result is retained up to 3
Bit effective number. Particulate sample test results can also be directly 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), 2 unorganized particulate 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 detailed in Appendix D.
11 quality assurance and quality control
11.1 drift correction
Changes in instrument status can result in deviations from the measurement results. In order to monitor and correct the drift of the instrument, it is necessary to divide
Before measuring the actual sample, use the standard sample provided by the instrument manufacturer to select the main target element to drift the instrument.
positive. The correction interval can be determined according to the stability of the instrument. Drift calibration samples should be measured in the same batch of samples
The amount of time to complete. The first measurement of the drift calibration sample should be the same as when using the calibration sample (8.2) to establish the calibration curve
A measurement cycle is completed. Drift calibration sample element strength measurement (count rate, cps) should be greater than 1000.
11.2 filter blank
Each batch of samples should be analyzed at least two samples of the same batch with the sample filter. Used to collect unorganized particles
The measured value of the target element in the blank sample of the filter shall not be greater than one tenth of the target heavy metal emission standard limit. otherwise,
May consider the appropriate increase in the amount of sample, so that the target element in the particle determination 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.
11.3 Calibration curve
The calibration curve should be checked before each batch. To be close to the calibration curve in the middle of the laboratory quality control sample (or different to
Source filter standard) for analysis to confirm, the relative error should meet the requirements of Table 1. Otherwise, the cause should be identified and reestablished
Calibration curve.
Table 1 quality control samples of the various elements of laboratory testing accuracy requirements
11.4 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, at least one sample should be measured. When the element content is high
In determining the lower limit, the parallel deviation of the test results should meet the requirements of Table 2.
Table 2 of the elements of the parallel measurement of precision requirements
Element Relative Deviation (%)
11.5 Accuracy
The method of this method should be verified by analyzing the standard sample of the film. If the measured value error exceeds the allowable range
, Stop the analysis of the sample, find the cause. Qualified, can also be used to verify the standard samples of certified particles. verification
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 laboratory quality
Control sample (or different source filter sample), when the element content is higher than the determination of the lower limit, 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 the sample is measured. The absolute value of the relative error between 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 uncertainty.
If the laboratory conditions are limited, you can consider the use of standard equipment provided by the manufacturer to verify.
12 Precautions
12.1 Experimental conditions
Each element corresponds to the maximum count of the dispersion angle and the pulse height distribution is the key monitoring of the test parameters. Should be passed on a regular basis
Standard qualitative scan, check whether the two parameters change. Daily analysis, should always be measured in the main laboratory quality control
Target element X-ray characteristic peak intensity value, if there is a significant change, you need to check the element of the dispersion angle and pulse height distribution.
After each change of the argon gas column, it is recommended to review the Na, Mg, Al, Si, Cl,
S and other elements PHA high and low limits, and adjust to the appropriate location.
12.2 Experimental operation
Teflon filter in the WD-XRF determination process, subject to X-ray irradiation is prone to cracks, or even damage. Suggest
Meet the measurement requirements under the premise of reducing the X-ray tube power and minimize the irradiation time, control the measurement time in 20min
Inside. For the next instrument, in order to ensure the integrity of Teflon film, you can consider in the filter sample surface covered with a layer
XRF special polypropylene film (6.7). In this way, even if the Teflon membrane rupture will not fall into the sample chamber, affecting the following beryllium window.
If you have the above measures in the determination of the sample, the establishment of calibration curve Determination of the standard sample strength to be taken when the same measures, two
The 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 (5.2 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, the measurement side down; if the instrument for the photo, then the first sample in the sample cup sample, the measurement side up, and then into
After the ring is fixed, so that the actual sample and the film standard X-ray irradiation distance consistent.
Appendix A
(Normative appendix)
Method detection limit and lower limit of determination
A.1 Elemental lines and methods Detection limits and determination limits
Note. The data expressed in g/m3 is based on the diameter of the particles with the diameter of 47mm and the sample volume of 24m3.
Appendix B
(Informative)
Calculation Example of Interference Element Correction Coefficient
The correction factor of the interfering element is determined experimentally. Experimental Scheme and Correction System of Interference Correction of Pb (Lα) for As (Kα)
The formula is as follows.
The Pb Lα line intensity was measured under the condition of As (Kα), and Pb was measured under the condition of Pb
Lβ line intensity. Assuming that the measured values are 17.930 kcps and 18.323 kcps, then Pb (L) on As (K)
The interference correction coefficient b is calculated as follows.
Let the As standard curve slope of 1.543, the actual particle samples in the K K line strength measurement for the I1, Pb Lβ line
Strength measurement value of I2, then As element content calculation formula is as follows.
If the laboratory has different levels of Pb standard, according to the above method were measured interference correction coefficient, whichever is the average
Value into the above formula.
Appendix C
(Informative)
Example of WD-XRF measurement conditions
Table C.1 WD-XRF measurement conditions Example 1
Note. Sample 1
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