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HJ 1211-2021: Solid waste - Determination of inorganic elements - Wavelength dispersive X-ray fluorescence spectrometry
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Solid waste - Determination of inorganic elements - Wavelength dispersive X-ray fluorescence spectrometry
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HJ 1211-2021
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Standard similar to HJ 1211-2021 HJ 1217 HJ 1202 HJ 1201 Basic data | Standard ID | HJ 1211-2021 (HJ1211-2021) | | Description (Translated English) | Solid waste - Determination of inorganic elements - Wavelength dispersive X-ray fluorescence spectrometry | | Sector / Industry | Environmental Protection Industry Standard | | Word Count Estimation | 36,397 | | Issuing agency(ies) | Ministry of Ecology and Environment | HJ 1211-2021: Solid waste - Determination of inorganic elements - Wavelength dispersive X-ray fluorescence spectrometry
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(Solid waste Determination of inorganic elements Wavelength dispersive X-ray fluorescence spectrometry)
National Ecological Environment Standard of the People's Republic of China
Determination of Inorganic Elements in Solid Waste
wavelength dispersive X-ray fluorescence spectrometry
Soild waste-Determination of inorganic elements-Wavelength dispersive
X-ray fluorescence spectrometry
This electronic version is the official standard text, which is reviewed and typeset by the Environmental Standards Institute of the Ministry of Ecology and Environment.
Published on 2021-11-18
2022-03-01 Implementation
Released by the Ministry of Ecology and Environment
directory
Foreword...ii
1 Scope...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...2
7 Samples...3
8 Analysis steps...3
9 Result calculation and representation...4
10 Accuracy...4
11 Quality Assurance and Quality Control...5
12 Waste Disposal...6
13 Precautions...6
Appendix A (normative appendix) detection limit and lower limit of determination of the method...7
Appendix B (Informative Appendix) Correction Methods for Matrix Effect and Spectral Line Overlapping Interference...8
Appendix C (Informative Appendix) Instrumental Analysis Reference Conditions...9
Appendix D (Informative) Calibration Curve Range...15
Appendix E (Informative Appendix) Qualitative and Standard-Free Quantitative Analysis...16
Appendix F (informative) Accuracy of the method...18
Determination of Inorganic Elements in Solid Waste by Wavelength Dispersive X-ray Fluorescence Spectrometry
Warning. When measuring toxic and harmful samples, avoid skin contact or inhalation through mouth and nose, and measures such as ventilation and exhaust should be taken during the test
To prevent contamination of the laboratory environment or other samples.
1 Scope of application
This standard specifies 16 categories for the determination of sludge, polluted soil, fly ash, soot, tailings waste rock and smelting slag in solid waste.
Wavelength Dispersive X-ray Fluorescence Spectroscopy of Inorganic Elements and 7 Oxides.
This standard applies to 16 types of inorganic solid wastes, such as sludge, polluted soil, fly ash, soot, tailings waste rock and smelting slag.
Determination of elements and 7 oxides including arsenic (As), barium (Ba), chlorine (Cl), cobalt (Co), chromium (Cr), copper (Cu), manganese (Mn),
Nickel (Ni), Phosphorus (P), Lead (Pb), Sulfur (S), Strontium (Sr), Titanium (Ti), Vanadium (V), Zinc (Zn), Zirconium (Zr), Silicon Dioxide (SiO2),
Aluminum oxide (Al2O3), iron oxide (Fe2O3), potassium oxide (K2O), sodium oxide (Na2O), calcium oxide (CaO), oxide
Magnesium (MgO).
This standard adopts the molten glass tablet method or powder compression method to prepare solid waste samples. The molten glass sheet method is suitable for sludge, polluted soil,
Preparation of solid waste samples such as fly ash, smoke dust, tailings waste rock, smelting slag, etc., but not suitable for the determination of chlorine (Cl) content;
The powder tableting method is suitable for the preparation of solid waste samples such as sludge, polluted soil, fly ash, and soot.
The detection limit of the method for the preparation and determination of 15 inorganic elements by the molten glass sheet method is 5 mg/kg～70 mg/kg, and the lower determination limit is
20 mg/kg～280 mg/kg; the detection limit of 7 oxides is 0.01%～0.03%, and the lower limit of determination is 0.04%～0.12%. powder
The detection limit of the method for the preparation and determination of 16 inorganic elements by the uncompressed tablet method is 2 mg/kg～30 mg/kg, and the lower determination limit is 8 mg/kg～120 mg/kg;
The detection limit of the method for 7 oxides is 0.01%-0.03%, and the lower limit of determination is 0.04%-0.12%. See Appendix A for details.
2 Normative references
This standard refers to the following documents or clauses thereof. For dated references, only the dated version applies to this standard.
For undated references, the latest edition (including all amendments) applies to this standard.
HJ/T 20 Technical Specification for Sampling and Sample Preparation of Industrial Solid Waste
HJ 298 Technical Specification for Hazardous Waste Identification
3 Principles of the method
The samples were prepared by the molten glass plate method or the powder pressing method, and each element atom in the sample was excited in a wavelength dispersive X-ray fluorescence spectrometer.
It emits characteristic X-ray spectral lines, whose intensity is proportional to the mass fraction of the element in the sample after the overlap and matrix effect correction.
By measuring the characteristic X-ray intensity of the target in the sample, the mass fraction of each element in the sample can be quantitatively analyzed.
4 Interference and cancellation
4.1 Matrix interference
The matrix interference in the sample includes the absorption and enhancement effect of the matrix element on the X-ray spectral intensity of the target element. through the empirical coefficient method or
Mathematical analysis methods such as the basic parameter method can reduce the influence of this matrix effect after calculation and processing. See Appendix B for common matrix effect correction methods.
4.2 Spectral line overlap interference
During sample analysis, the analytical lines of the target element may be interfered by the lines of other elements in the matrix. Select target elemental analysis
The interference of the spectral lines of other elements in the matrix should be avoided when the spectral lines are used, and the spectral line overlap interference correction can also be calculated by analyzing the measurement results of multiple standard samples.
Positive coefficient for noise cancellation. See Appendix B for common spectral line interference and spectral line correction methods.
4.3 Particle effect
When the sample is prepared by the powder compression method, the particle size, inhomogeneity and surface structure of the sample will affect the characteristic X-ray of the target element.
The intensity of spectral lines has an influence, and these factors should be controlled. The particle size of the measured sample should be consistent with that of the standard sample.
reduce or eliminate these effects.
5 Reagents and Materials
Unless otherwise stated, analytical reagents that meet national standards were used in the analysis, and the experimental water was freshly prepared deionized water or distilled water.
5.1 Anhydrous lithium tetraborate (Li2B4O7). excellent grade pure.
5.2 Anhydrous lithium metaborate (LiBO2). excellent grade.
5.3 Lithium nitrate (LiNO3).
5.4 Lithium Bromide (LiBr).
5.5 Boric acid (H3BO3) or high density low pressure polyethylene powder.
5.6 Lithium nitrate solution. ρ(LiNO3)=220 g/L.
Weigh 22.0 g of lithium nitrate (5.3) and dissolve it in an appropriate amount of water. After dissolving, add water to make up to 100 ml, and shake well.
5.7 Lithium bromide solution. ρ(LiBr)=60 g/L.
Weigh 6.0 g of lithium bromide (5.4) and dissolve it in an appropriate amount of water. After dissolving, add water to make up to 100 ml, and shake well.
5.8 Standard samples. commercially available certified standard samples. Including but not limited to soil composition analysis standard material series, water system sediment composition analysis
Reference material series, coal ash reference material series, iron ore reference material series, slag reference material series.
5.9 Plastic Rings.
5.10 Argon gas-methane gas. φ(Ar)=90%, φ(CH4)=10%, in terms of volume fraction.
6 Instruments and equipment
6.1 X-ray fluorescence spectrometer. wavelength dispersion type, with computer control system.
6.2 Powder pressing machine. pressure≥3.9×105N.
6.3 Muffle furnace. can be heated to 800 ℃.
6.4 Fusion sample maker. can be heated to 1200 ℃.
6.5 Platinum-gold alloy crucible. w(Pt)=95%, w(Au)=5%, in mass fraction.
6.6 Platinum-gold alloy casting mold. w(Pt)=95%, w(Au)=5%, in mass fraction.
6.7 Balance. The actual division value is better than 1 mg.
6.8 Non-metal sieve. the aperture is 75 μm (200 mesh).
6.9 Oven. The temperature can be controlled at 105 ℃±5 ℃.
6.10 General laboratory instruments and equipment.
7 samples
7.1 Collection and storage of samples
The collection and preservation of solid waste samples shall be carried out in accordance with the relevant regulations of HJ/T 20 and HJ 298.
7.2 Sample preparation
The sample air-drying, rough grinding, fine grinding and other operations are carried out in accordance with the relevant regulations of HJ/T 20 and HJ 298, and then all pass through.200 mesh non-metallic
Sieve (6.8), and dry it in an oven (6.9) at 105 °C for later use.
7.3 Preparation of test specimens
7.3.1 Fused glass sheet method
Take 34 mm sample cup molten glass sheet preparation as an example.
Weigh 1.000 g ± 0.005 g of sample (7.2) and flux 6.700 g ± 0.005 g of anhydrous lithium tetraborate (5.1), 3.300 g ± 0.005 g
Mix with anhydrous lithium metaborate (5.2), place in platinum-gold alloy crucible (6.5), add 1 ml lithium nitrate solution (5.6) and 1 ml lithium bromide
The solution (5.7) was pre-oxidized by heating at 600 °C for 10 min in the muffle furnace (6.3), then transferred to the melting sample maker (6.4), and heated to 1050 °C
molten. During the melting process, shake the crucible to drive out the air bubbles and mix the melt. Pouring the melt in a platinum-gold alloy casting mould (6.6)
forming. The glassy fused sample should be uniform and transparent, with a smooth surface and no bubbles.
Note. The dilution ratio of the sample to the flux, the preparation ratio of the flux, and the melting time can be adjusted according to the actual situation of the sample.
7.3.2 Powder tableting method
With boric acid or high density low pressure polyethylene powder (5.5) backing, rim, or rim with plastic ring (5.9), place about 5 g of sample (7.2) in place.
On a powder pressing machine, a sheet with a smooth surface and no cracks is made with a certain pressure.
Note. For some samples that are not easy to form, the pressure strength and tableting time can be increased, or 10% to 20% of binders (such as microcrystalline cellulose, boric acid,
polyethylene, graphite, etc.), stir, grind and mix evenly and then press and shape. The standard sample of the calibration curve should be treated in the same way, and the ratio of sample and binder preparation should be
Examples should be consistent.
8 Analysis steps
8.1 Establishing the measurement method
According to the determined target elements, select and optimize the analysis spectral lines, and select the best working conditions from the instrument database, mainly including the analysis of the elements.
spectroscopic lines, voltage and current for X-ray tubes, spectroscopic crystals, collimators, goniometers, detectors, pulse height distribution (PHA or PHD),
Background correction, etc., in which the analysis line peaks, background point positions and pulse height distribution (PHA or PHD) can be scanned according to the standard sample.
If adjustment is confirmed. Appropriate reference conditions can be selected according to the brand of the instrument. Please refer to Appendix C for the reference conditions of the instrument.
8.2 Establishment of calibration curve
According to the same operation steps as the sample preparation, at least 15 standard samples with different mass fractions and uniform mass fraction distribution (5.8)
It is melted to make glass tablets or compressed into tablets, in which the powder tableting method is based on the solid waste category, and standard samples with similar substrates should be selected separately
Create a calibration curve. See Appendix D for the calibration curve ranges for 16 inorganic elements and 7 oxides. Under the best working conditions of the instrument, the
Measure on the machine, record the intensity of the characteristic spectral lines of the target element and related elements. Taking the mass fraction of inorganic elements or oxides as independent variables, the target
The characteristic spectral line intensity after element correction is used as the dependent variable, and a calibration model is established. Calibration parameters include spectral line overlap interference factor, matrix effect correction
Coefficients, calibration curve slope and intercept. When measuring solid waste samples of unknown origin and unknown matrix, and it is difficult to obtain standard samples, you can refer to the
For qualitative and standard-free quantitative analysis methods, see Appendix E.
8.3 Determination
Test the sample (7.3) under the same conditions as for the establishment of the calibration curve (8.2).
9 Result calculation and presentation
9.1 Result calculation
The mass fraction (mg/kg) of inorganic elements or the mass fraction (%) of oxides in the solid waste sample is calculated according to formula (1).
9.2 Result representation
The results of inorganic elements and oxides are retained to a maximum of 3 significant figures. The determination result of inorganic elements (mg/kg) is reserved to the integer place,
Oxide determination results (%) are rounded to 2 decimal places.
10 Accuracy
10.1 Precision
6 laboratories have certified 5 solid wastes such as contaminated soil, smoke, sediment, slag and iron ore by using the molten glass sheet method.
Standard samples and actual samples of fly ash were prepared and repeated six times. The relative standard deviations in the laboratory for 15 inorganic elements were
0%～23%, relative standard deviation between laboratories is 1.0%～30%, repeatability limit is 5 mg/kg～1.4×103 mg/kg, repeatability limit
It is 7 mg/kg～4.6×103 mg/kg; the relative standard deviation of the seven oxides in the laboratory is 0%～14%, and the relative standard deviation between the laboratories is 0%～14%.
The difference was 1.5% to 18%, the repeatability limit was 0.02% to 21%, and the reproducibility limit was 0.04% to 20%.
6 laboratories used the powder tableting method to separate the certified standard samples of contaminated soil, soot, soil and other three solid wastes, and fly ash,
The actual samples of 4 solid wastes such as sludge, polluted soil and soil were prepared and repeated 6 times, and the laboratory of 16 inorganic elements
The internal relative standard deviation was 0% to 20%, the interlaboratory relative standard deviation was 2.7% to 28%, and the repeatability limit was 2 mg/kg to 3.7 × 103 mg/kg.
The reproducibility limit is 3 mg/kg～5.4×103 mg/kg; the relative standard deviation of the seven oxides within the laboratory is 0%～12%, and the interlaboratory
The standard deviation is 1.6% to 18%, the repeatability limit is 0.01% to 2.8%, and the reproducibility limit is 0.06% to 15%.
Preparation and determination of 15 inorganic elements and 7 oxides in solid waste by the molten glass sheet method, the precision data are shown in Table F.1 in Appendix F;
16 inorganic elements and 7 oxides in solid waste were prepared and determined by powder compression method. The precision data are shown in Table F.2 in Appendix F.
10.2 Correctness
The 6 laboratories used the molten glass sheet method to analyze the certified standard samples of 4 kinds of solid wastes such as contaminated soil, soot, sediment and iron ore, respectively.
The relative error of the 15 inorganic elements was -22% to 27%, and the final value of the relative error was -9.6%.
±8.1%～13%±13%; the relative error of 7 oxides is -16%～30%, and the final value of relative error is -6.7%±11%～14%±
27%.
6 laboratories used the powder tablet method to separate certified standard samples of contaminated soil, smoke, soil, iron ore, etc.
The relative error of the 16 inorganic elements was -19% to 20%, and the final value of the relative error was -11% ±
17%～11%±16%; the relative error of 7 oxides is -20%～50%, and the final value of relative error is -5.1%±9.8%～27%±35%.
Preparation and determination of 15 inorganic elements and 7 oxides in solid waste by the molten glass sheet method, see Table F.3 in Appendix F for the accuracy data;
The powder tablet method was used to prepare and determine 16 inorganic elements and 7 oxides in solid waste. For the accuracy data, see Table F.4 in Appendix F.
11 Quality Assurance and Quality Control
11.1 Every 20 samples or each batch (less than 20 samples/batch) shall determine at least one certified standard sample, and the correctness of the measured value shall be determined.
The qualified indicators are shown in Table 1.
11.2 At least one replicate shall be determined for every 20 samples or batches (less than 20 samples). The maximum allowable relative deviation of the measurement results
See Table 2.
12 Waste Disposal
The waste liquid and waste generated in the experiment should be collected by classification, kept in a centralized manner, and should be marked accordingly, and the qualified unit should be entrusted to deal with it according to law.
reason.
13 Notes
13.1 When preparing powder samples, wet grinding is usually carried out manually or mechanically, that is, adding an appropriate amount of alcohol, ether or
Mixing and grinding method of organic reagents such as ethylamine alcohol.
13.2 After each replacement of argon-methane gas, the element determination conditions related to the gas flow proportional counter, that is, the pulse height distribution, should be reviewed.
Whether there is a significant change in the high and low limits (PHA or PHD). If there are significant changes, drift correction should be performed or the calibration curve should be re-established.
13.3 Sulfur and chlorine have the characteristics of being unstable after being irradiated by high-energy rays and being highly susceptible to pollution.
When taking samples, it is recommended to use the powder compression method and measure it immediately. At the same time, in the process of instrument measurement, after the sample is irradiated with X-rays, the chlorine element
The mass fraction of ions will increase significantly, therefore, if the chlorine element needs to be determined, the chlorine element should be placed in the first place in the determination order. The molten glass sheet method is not suitable
For the determination of chlorine element, the element loss should be paid attention to when determining sulfur element.
13.4 After replacing the X-ray tube, when adjusting the voltage and current, it should be gradually adjusted from low voltage and low current to working voltage and working current.
Each time the instrument is turned on, the voltage and current should be adjusted gradually, not all at once.
13.5 When the determination result of the element mass fraction is outside the range of the calibration curve, other analytical methods should be used for verification.
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