WO2011027613A1 - 蛍光x線分析方法 - Google Patents
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- WO2011027613A1 WO2011027613A1 PCT/JP2010/061250 JP2010061250W WO2011027613A1 WO 2011027613 A1 WO2011027613 A1 WO 2011027613A1 JP 2010061250 W JP2010061250 W JP 2010061250W WO 2011027613 A1 WO2011027613 A1 WO 2011027613A1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/076—X-ray fluorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/60—Specific applications or type of materials
- G01N2223/637—Specific applications or type of materials liquid
Definitions
- the present invention relates to a fluorescent X-ray analysis method using a so-called scattered radiation internal standard method.
- the Compton scattered ray is an internal standard line that the intensity of the Compton scattered ray of the characteristic X-ray of the primary X-ray is approximately inversely proportional to the mass absorption coefficient of the analysis target element with respect to the fluorescent X-ray. This is known to mean (see Non-Patent Document 1).
- the background near the wavelength of the analytical line that is, the scattered radiation having the bottom wavelength in the fluorescent X-ray spectrum of the analysis target element is used as the internal standard line (see Patent Documents 2 and 3 and Non-Patent Document 2).
- JP-A-10-8249 paragraphs 0037 to 0040
- Japanese Patent No. 3567734 paragraphs 0039, 0036, 0075
- JP 2008-298679 A paragraphs 0001 to 0005, 0024
- the main components are samples such as oils, organic solvents, aqueous solutions, that is, at least one element of carbon, oxygen and nitrogen and hydrogen (all of which are so-called non-measurable elements that cannot practically measure fluorescent X-rays).
- samples such as oils, organic solvents, aqueous solutions, that is, at least one element of carbon, oxygen and nitrogen and hydrogen (all of which are so-called non-measurable elements that cannot practically measure fluorescent X-rays).
- the present invention has been made in view of the above-described conventional problems.
- a fluorescent X-ray analysis method using an internal standard method for scattered radiation in a liquid sample mainly containing at least one element of carbon, oxygen and nitrogen and hydrogen. It is an object of the present invention to provide a method capable of accurately calculating the concentration of an analysis target element having atomic numbers 9 to 20.
- the inventor of the present application uses a primary X-ray continuous X-ray scattered ray as an internal standard line, and analyzes the wavelength of the primary X-ray continuous X-ray scattered ray from the atomic numbers 9 to 20 described above.
- the measurement intensity and the mass absorption coefficient of the scattered light of the continuous X-rays of the primary X-rays are in inverse proportion to the wavelength of the fluorescent X-rays generated from the target element and within the range of composition variation in the liquid sample.
- the inventors found that the internal standard line can accurately reflect the composition of the sample and the concentration of the analysis target element can be accurately calculated, and the present invention has been made.
- the fluorescent X-ray analysis method of the present invention first, at least one element of carbon, oxygen and nitrogen and a liquid sample mainly containing hydrogen are irradiated with primary X-rays, and the atomic number in the liquid sample is determined.
- the intensity of fluorescent X-rays generated from each element from 9 to 20 and the intensity of scattered X-rays of primary X-rays scattered by the liquid sample are measured, and the fluorescent X-rays generated from each element Is a fluorescent X-ray analysis method for calculating the concentration of an element in the liquid sample based on the ratio of the measured intensity of the primary X-ray and the measured intensity of scattered X-rays of the primary X-ray.
- the wavelength of the scattered light of the continuous X-rays of the primary X-ray is shorter than the wavelength of the fluorescent X-rays generated from the respective elements, and the primary X-ray is within the variation range of the composition in the liquid sample. It sets so that the measurement intensity
- a continuous primary X-ray with a wavelength set as described above as an internal standard line Since the scattered radiation internal standard method using X-ray scattered radiation is applied, the internal standard radiation can accurately reflect the composition of the liquid sample, and the concentration of the element to be analyzed from atomic numbers 9 to 20 can be accurately calculated.
- the wavelength of the scattered X-rays of the primary X-ray it is preferable to set the wavelength of the scattered X-rays of the primary X-ray to 0.1042 nm or more and 0.2505 nm or less. Moreover, it is preferable to set the wavelength of the scattered X-rays of the primary X-rays to 0.123 nm or more and 0.193 nm or less for the elements having atomic numbers 15 to 17 in the liquid sample.
- FIG. 4 is a diagram showing a relationship in which scattered X-rays of primary X-rays having a wavelength of 0.2776 nm are examined in the same manner as in FIG. 2. It is a conceptual diagram which shows the penetration
- this apparatus generates from a sample stage 8 on which a sample 3 is placed, an X-ray source 1 such as an X-ray tube that irradiates the sample 3 with primary X-rays 2, and the sample 3. And a detecting means 9 for measuring the intensity of the fluorescent X-rays 4 and the scattered radiation 12.
- the detection means 9 includes a spectroscopic element 5 that separates fluorescent X-rays 4 and scattered rays 12 generated from the sample 3, and a detector 7 that measures the intensity of each spectroscopic fluorescent X-ray 6 or scattered ray 13.
- the apparatus used for the fluorescent X-ray analysis method of this embodiment may be a wavelength dispersion type or an energy dispersion type.
- the irradiation of the primary X-ray 2 to the sample 3 may be an upper surface irradiation from above or a lower surface irradiation from below.
- the apparatus further calculates a concentration of an element in the sample 3 based on the measured intensity of the fluorescent X-ray 4 generated from each element of atomic numbers 9 to 20 in the sample 3 measured by the detection means 9.
- the calculation means 10 and the wavelength of the fluorescent X-ray 4 and the scattered radiation 12 to be measured by the detection means 9 and the fact that the calculation means 10 should calculate the element concentration in the sample 3 using the standard method for scattered radiation are input.
- Input means 11 such as a mouse, a keyboard, and a touch panel.
- the subject of analysis in the fluorescent X-ray analysis method of this embodiment is a liquid sample 3A mainly composed of at least one element of carbon, oxygen and nitrogen and hydrogen. (The composition of the main component also varies depending on the liquid sample 3A) and is hermetically stored in a known holder having a window that transmits X-rays.
- the detection means 10 Measured intensity of fluorescent X-rays 4 generated from each element of atomic numbers 9 to 20 in the sample 3A measured in 9 and measured intensity of scattered X-rays 12 of primary X-rays measured by the detecting means 9 Based on the ratio, the element concentration in the sample 3A is calculated.
- the wavelength of the scattered X-rays 12 of the primary X-rays to be measured is shorter than the wavelength of the fluorescent X-rays 4 generated from the respective elements, and within the composition variation range of the liquid sample 3A.
- the measurement intensity and the mass absorption coefficient for the scattered X-ray 12 of the primary X-ray are set and input in advance. More specifically, the wavelength of the continuous X-ray scattered radiation 12 of the primary X-ray to be measured is set to 0.1042 nm to 0.2505 nm and input.
- the fluorescent X-ray analysis method of the embodiment of the present invention first irradiates the liquid sample 3A mainly composed of at least one element of carbon, oxygen, and nitrogen and hydrogen with the primary X-ray 2 to obtain the liquid sample.
- the intensity of fluorescent X-rays 4 generated from each element of atomic numbers 9 to 20 in 3A and the intensity of scattered X-rays 12 of primary X-rays scattered by the liquid sample 3A are measured.
- the wavelength of the scattered X-rays 12 of the primary X-rays is shorter than the wavelength of the fluorescent X-rays 4 generated from each element, and the primary X-ray is within the composition variation range in the liquid sample 3A. More specifically, it is set to 0.1042 nm or more and 0.2505 nm or less so that the measured intensity and the mass absorption coefficient of the scattered X-ray scattered rays 12 are in inverse proportion.
- the primary X-ray scattered X-rays having such a wavelength are used as the internal standard line.
- Light element such as sulfur by applying the scattered radiation standard method to liquid samples mainly containing at least one element of carbon, oxygen and nitrogen and hydrogen, such as oils, organic solvents, aqueous solutions, etc.
- the concentration of the element to be analyzed in the present invention, the element of atomic number 9 to 20
- the ratio of the Compton scattering and Thomson scattering scattering power is important for the scattered radiation used as the internal standard line. .
- Compton scattering ability is relatively small for elements with atomic number 2 or higher, but only hydrogen has a scattering ability approximately twice that of other elements.
- a characteristic X-ray Compton scattered ray such as a primary X-ray cannot be used as an internal standard ray.
- the primary X-ray continuous X-ray scattered radiation includes both Compton scattered radiation and Thomson scattered radiation.
- Equation (2) is obtained when the sample has an infinite X-ray thickness for this wavelength.
- the intensity of fluorescent X-rays having the same wavelength when the sample has a finite thickness can be simply expressed as in equation (3).
- Equation (4) is obtained when the sample has an infinite thickness with respect to the fluorescent X-ray of this wavelength.
- the intensity ratio between fluorescent X-rays having substantially the same wavelength and scattered X-ray rays can be expressed by equation (5) regardless of the thickness of the sample.
- the total of the Compton scattering power and the Thomson scattering power It is necessary that the scattering power P Comp + P Thom is constant regardless of the sample composition.
- the total scattering power of Compton scattering power and Thomson scattering power is constant regardless of the sample composition. This is equivalent to the fact that the intensity is inversely proportional to the mass absorption coefficient of the wavelength of the scattered radiation.
- the ratio between Compton scattering power and Thomson scattering power depends on the wavelength of the scattered X-rays, and the longer the wavelength, the higher the Thomson scattering power.
- hydrogen is about twice that of other elements, but conversely, with respect to Thomson scattering power, hydrogen is extremely small. From these facts, it is conceivable that the dependence of the total scattering power of Compton scattering power and Thomson scattering power on the sample composition can be reduced if the wavelength of the scattered X-ray scattering light is appropriately set.
- the intensity of continuous X-ray scattering was measured on a sample that was considered to be infinite thickness, and the relationship with the mass absorption coefficient was investigated. Specifically, with respect to continuous X-ray scattered radiation having a wavelength of 0.1607 nm in a liquid sample such as oil containing hydrogen, carbon, and oxygen having different compositions, the reciprocal of the measurement intensity (relative intensity) and the mass absorption coefficient This relationship was examined and shown in FIG. Similarly, the continuous X-ray scattered radiation having a wavelength of 0.2776 nm was examined and shown in FIG.
- FIG. 4 shows the primary X-ray in the case of bottom surface irradiation in which the liquid sample 3A accommodated in the holder 14 having the window 14a that transmits X-rays on the bottom surface is irradiated with the primary X-ray 2 from below.
- the conceptual diagram of the penetration depth and the detection range of the scattered X ray 12 of a continuous X ray is shown.
- the sample amount is gradually increased for the same sample, and the measured intensity and the theoretical intensity calculated by the fundamental parameter method (FP method) are linearly related to the scattered X-ray scattered radiation of the two types of wavelengths.
- the infinite thickness was determined as the amount of sample in which the strength was not increased.
- the measured intensity and the theoretical intensity deviate from the linear relationship when the sample amount is increased.
- FIG. 5A sintered ray wavelength 0.1344 nm
- FIG. 5B sintered ray wavelength 0.1607 nm
- An example of this is shown in FIG. 6 (wavelength of scattered radiation: 0.0653 nm).
- the measured intensity and the inverse of the mass absorption coefficient are in a good proportional relationship, that is, the measured intensity and the mass absorption coefficient are good. In inverse proportion.
- a good correlation was not obtained between the measured intensity and the reciprocal of the mass absorption coefficient.
- the wavelength at which a good correlation as shown in FIG. 2 can be obtained depends on the optical system of the apparatus, the type of liquid sample, and the concentration of the element to be analyzed, but in the apparatus used for the experiment, mineral oil, vegetable oil, alcohol, and water are used. When each liquid sample was used and sulfur having a concentration of 0 to 5 mass% was used as an analysis target element, a good correlation was obtained with respect to continuous X-ray scattered radiation having a wavelength of 0.1042 to 0.2505 nm.
- the sample thickness is also important.
- the intensity ratio between the fluorescent X-ray of the element to be analyzed and the background near the wavelength is used. This intensity ratio is expressed by equation (6). It becomes like this and said (5) Formula.
- the amount of the sample is set to the infinite thickness as described above, and the scattered X-rays of the analysis target element generated from the sample and the continuous X-rays of the primary X-rays are all detected without being shielded. If this is the case, the intensity ratio between the two is given by equation (8).
- FIG. 7 shows a calibration curve in the case where no correction is performed, and the scattered X-ray standard correction of the present invention was performed using the continuous X-ray scattered X-rays having a wavelength of 0.1607 nm as the inner standard line.
- the calibration curve in this case is shown in FIG.
- fluorescent X-rays of the element to be analyzed (here, S with a wavelength of 0.5373 nm)
- a continuous X-ray scattered ray having a shorter wavelength than ( ⁇ K ⁇ ray) is effective as an internal standard ray.
- the sample When the liquid sample is a lubricating oil, the sample contains a relatively high concentration of additive elements, and the base oil varies depending on the type of lubricating oil.
- the mass absorption coefficient (cm 2 / g) of calcium with respect to the fluorescent X-ray S-K ⁇ ray (wavelength 0.5373 nm) of the element to be analyzed is a continuous X of primary X-rays.
- Table 4 shows the mass absorption coefficient (cm 2 / g) of calcium with respect to the scattered radiation (wavelength 0.1607 nm) and the ratio of both mass absorption coefficients.
- the absorption edge of Ca-K is 0.307 nm, and the wavelength of the fluorescent X-ray S-K ⁇ ray of the element to be analyzed and the wavelength of the scattered X-rays of the primary X-ray as the internal standard line. Exists in between.
- the ratio of both mass absorption coefficients in calcium is significantly different from the ratio of carbon, nitrogen and oxygen shown in Table 1, and unlike the case of hydrogen, the absolute value of the mass absorption coefficient of calcium is the same as that of carbon, nitrogen and oxygen. Since it is larger than the absolute value of the mass absorption coefficient, the influence of the mass absorption coefficient of calcium on the mass absorption coefficient of the entire sample cannot be ignored.
- the sample when the sample includes an element having an absorption edge between the wavelength of the fluorescent X-ray of the analysis target element and the wavelength of the scattered X-ray of the primary X-ray as the internal standard line
- the intensity of fluorescent X-rays can be measured using the element as an additional correction element, and so-called matrix correction can be performed using equation (9).
- the matrix correction constant ⁇ j may be obtained by experimentally calculating regression samples by measuring different standard samples including the analysis target element and the correction element and having different compositions, or by using the FP method to detect fluorescent X-rays and scattered rays. It may be obtained by calculating the theoretical strength of. In the latter case, it becomes a kind of semi-fundamental parameter method (SFP method) of the calibration curve method.
- SFP method semi-fundamental parameter method
- FIG. 9 shows a calibration curve when the standard correction for scattered radiation according to the present invention is performed using a line.
- the calibration curve of FIG. 9 it is understood that the influence of the sample composition is appropriately removed by correction.
- it is between the wavelength of the fluorescent X-ray of the element to be analyzed and the wavelength of the scattered X-ray of the primary X-ray as the internal standard line.
- the intensity of the fluorescent X-ray is measured using the element as an additional correction element, and the matrix correction is performed by the equation (9) for more accurate analysis. Is desirable.
- the wavelength is set as described above as the internal standard line for the liquid sample 3A mainly containing at least one element of carbon, oxygen, and nitrogen and hydrogen. Since the scattered X-ray internal standard method using the primary X-ray scattered X-ray scattered line 12 is applied, the internal standard line can accurately reflect the composition of the liquid sample 3A, and the analysis target elements having atomic numbers 9 to 20 Concentration can be calculated accurately.
- the present invention can also be applied to a fluorescent X-ray analysis method using a fundamental parameter method, and the same operational effects can be obtained.
- fluorescent X-ray S-K ⁇ ray wavelength: 0.5373 nm
- primary X-ray scattered X-rays wavelength: 0.1344 nm
- FIG. 10 shows a favorable apparatus sensitivity curve obtained with respect to the intensity ratio. It will be understood that in the X-ray fluorescence analysis method using the fundamental parameter method, the influence of the sample composition is appropriately removed by the standard correction in scattered radiation of the present invention.
- the accuracy is 15 ppm or less at a wavelength of scattered light of continuous X-rays of primary X-rays of 0.1042 nm to 0.2505 nm, and based on this, in the fluorescent X-ray analysis method of the embodiment,
- the wavelength of the scattered radiation of the continuous X-rays of the primary X-rays is set to be 0.1042 nm or more and 0.2505 nm or less for the elements of atomic numbers 9 to 20 centered on sulfur in the liquid sample.
- the accuracy is 5 ppm or less at a wavelength of scattered light of continuous X-rays of primary X-rays of 0.123 nm to 0.193 nm, atoms centered on sulfur in the liquid sample.
- the wavelength of the scattered X-rays of the primary X-rays it is preferable to set the wavelength of the scattered X-rays of the primary X-rays to 0.123 nm or more and 0.193 nm or less.
Abstract
Description
2 1次X線
3 試料
3A 液体試料
4 蛍光X線
9 検出手段
10 算出手段
11 入力手段
12 1次X線の連続X線の散乱線
Claims (3)
- 炭素、酸素および窒素のうちの少なくとも1元素ならびに水素を主成分とする液体試料に1次X線を照射し、
前記液体試料中の原子番号9から20までの各元素から発生する蛍光X線の強度と、前記液体試料で散乱する1次X線の連続X線の散乱線の強度とを測定し、
前記各元素から発生する蛍光X線の測定強度と前記1次X線の連続X線の散乱線の測定強度との比に基づいて、前記液体試料における元素の濃度を算出する蛍光X線分析方法であって、
前記1次X線の連続X線の散乱線の波長を、前記各元素から発生する蛍光X線の波長よりも短く、かつ、前記液体試料における組成の変動範囲内で、前記1次X線の連続X線の散乱線についての測定強度と質量吸収係数とが反比例するように、設定する蛍光X線分析方法。 - 請求項1に記載の蛍光X線分析方法において、
前記1次X線の連続X線の散乱線の波長を0.1042nm以上0.2505nm以下に設定する蛍光X線分析方法。 - 請求項1に記載の蛍光X線分析方法において、
前記液体試料中の原子番号15から17までの元素に対して、前記1次X線の連続X線の散乱線の波長を0.123nm以上0.193nm以下に設定する蛍光X線分析方法。
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EP10813564.1A EP2333529B1 (en) | 2009-09-07 | 2010-07-01 | X-ray fluorescence analyzing method |
CN2010800029349A CN102187208B (zh) | 2009-09-07 | 2010-07-01 | 荧光x射线分析方法 |
BRPI1005172A BRPI1005172B8 (pt) | 2009-09-07 | 2010-07-01 | método de analisar fluorescência de raio-x |
US13/123,121 US8433035B2 (en) | 2009-09-07 | 2010-07-01 | X-ray fluorescence analyzing method |
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CN106908466A (zh) * | 2017-03-29 | 2017-06-30 | 中国科学院过程工程研究所 | 一种在线x射线荧光光谱分析系统 |
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EP2333529B1 (en) | 2013-10-16 |
BRPI1005172B8 (pt) | 2020-09-08 |
EP2333529A1 (en) | 2011-06-15 |
CN102187208B (zh) | 2013-12-04 |
EP2333529A4 (en) | 2011-09-07 |
US8433035B2 (en) | 2013-04-30 |
JP4629158B1 (ja) | 2011-02-09 |
CN102187208A (zh) | 2011-09-14 |
JP2011075542A (ja) | 2011-04-14 |
BRPI1005172A2 (pt) | 2017-04-25 |
US20110243301A1 (en) | 2011-10-06 |
BRPI1005172B1 (pt) | 2019-09-10 |
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