JPH05119000A - Fluorescent x-ray analyzing device - Google Patents
Fluorescent x-ray analyzing deviceInfo
- Publication number
- JPH05119000A JPH05119000A JP30419891A JP30419891A JPH05119000A JP H05119000 A JPH05119000 A JP H05119000A JP 30419891 A JP30419891 A JP 30419891A JP 30419891 A JP30419891 A JP 30419891A JP H05119000 A JPH05119000 A JP H05119000A
- Authority
- JP
- Japan
- Prior art keywords
- ray
- rays
- sample
- fluorescent
- primary
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、試料に対して空気層よ
りなるＸ線パス部を介して一次Ｘ線を照射し、試料から
放出される二次Ｘ線に基づいて試料分析を行うようにし
た蛍光Ｘ線分析装置に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention irradiates a sample with primary X-rays through an X-ray path portion formed of an air layer, and performs sample analysis based on secondary X-rays emitted from the sample. The present invention relates to a fluorescent X-ray analyzer.
【０００２】[0002]
【従来の技術】蛍光Ｘ線分析装置は、例えば原油中に含
まれる硫黄分の含有量の測定や、鋼材の種類判別、ある
いは、メッキ組成の分析などに用いられるが、その測定
対象元素によっては、Ｘ線パス部の密度変化によってそ
の測定値に影響が及ばされるところから、次のような対
策が講じられていた。2. Description of the Related Art A fluorescent X-ray analyzer is used, for example, to measure the content of sulfur contained in crude oil, determine the type of steel material, or analyze the plating composition. Since the measurement value is affected by the change in the density of the X-ray path portion, the following measures have been taken.
【０００３】すなわち、Ｘ線パス部を真空にする、
Ｘ線パス部をヘリウムガスによってパージする、Ｘ線
パス部の気圧および温度を測定し、その値から測定値を
補正する（例えば特開昭57− 86030号公報）、Ｘ線パ
ス部の気圧および温度を測定し、その値から蛍光Ｘ線強
度を質量吸収係数などの物理定数を使って補正する（例
えば特開昭60− 61649号公報）、といった手段がある。That is, the X-ray path portion is evacuated,
The X-ray path portion is purged with helium gas, the atmospheric pressure and temperature of the X-ray path portion are measured, and the measured values are corrected from the measured values (for example, JP-A-57-86030). There is a means of measuring the temperature and correcting the fluorescent X-ray intensity from the measured value using a physical constant such as a mass absorption coefficient (for example, JP-A-60-61649).
【０００４】[0004]
【発明が解決しようとする課題】しかしながら、前記
の手法は、試料が液体の場合、適用が困難であり、の
手法は、高価なヘリウムガスを用いるためランニングコ
ストが高くつき、の手法は、気圧および温度の影響度
をそれぞれ予め把握しておく必要があり、の手法は、
蛍光Ｘ線分析において、試料の組成影響を補正する一手
法である散乱比法（試料に一次Ｘ線を照射したときに発
生する二次Ｘ線に含まれる蛍光Ｘ線の強度と散乱Ｘ線の
強度の比に基づいて試料の分析を行う手法）には適用で
きない、などの欠点がある。However, the above method is difficult to apply when the sample is a liquid, and the method requires high running cost because expensive helium gas is used. It is necessary to know in advance the degree of influence of temperature and temperature, and the method of
In the fluorescent X-ray analysis, the scattering ratio method, which is one method for correcting the influence of the composition of the sample (the intensity of the fluorescent X-ray and the scattered X-ray included in the secondary X-ray generated when the sample is irradiated with the primary X-ray It cannot be applied to a method of analyzing a sample based on the intensity ratio).
【０００５】ところで、散乱比法は、すでに説明したよ
うに、試料に一次Ｘ線を照射したときに発生する蛍光Ｘ
線の強度と散乱Ｘ線の強度の比に基づいて試料の分析を
行う手法であり、試料の組成影響を補正することができ
る。By the way, the scattering ratio method is, as described above, the fluorescence X generated when the sample is irradiated with the primary X-ray.
This is a method of analyzing the sample based on the ratio of the intensity of the X-ray and the intensity of the scattered X-ray, and the influence of the composition of the sample can be corrected.
【０００６】しかしながら、この散乱比法も必ずしも万
全の手法とは云えないのである。すなわち、試料に対し
て空気層よりなるＸ線パス部を介して一次Ｘ線を照射
し、試料から放出される二次Ｘ線に基づいて試料分析を
行うようにした場合、蛍光Ｘ線の強度のみならず散乱Ｘ
線の強度をも補正する必要がある。However, this scattering ratio method is not always a perfect method. That is, when the sample is irradiated with the primary X-rays through the X-ray path portion formed of the air layer and the sample analysis is performed based on the secondary X-rays emitted from the sample, the intensity of the fluorescent X-rays is increased. Not only scattered X
It is also necessary to correct the line intensity.
【０００７】今、例えば励起源として反射型のＸ線管を
用いた場合、一次Ｘ線はターゲット材料による特性Ｘ線
の他に、大量の連続Ｘ線を含んでいる。この連続Ｘ線を
励起源として使用した場合、散乱Ｘ線も連続的なエネル
ギー分布を持ち、そのエネルギーに応じてＸ線パス部に
おける空気密度の影響が異なる。従って、補正計算を行
う際には、連続Ｘ線をエネルギーで分割するなど煩雑な
操作が必要となる。その上、連続Ｘ線のうち、エネルギ
ーの高いＸ線は、コンプトン散乱の割合が大きく、しか
も、コンプトン散乱とレイリー散乱とのエネルギー差が
大きく、試料組成によりコンプトン散乱とレイリー散乱
との比も変化するため、散乱Ｘ線の平均エネルギー値が
変化し、厳密な意味での気圧および温度影響の補正が困
難である。Now, for example, when a reflection type X-ray tube is used as the excitation source, the primary X-rays include a large amount of continuous X-rays in addition to the characteristic X-rays by the target material. When this continuous X-ray is used as the excitation source, the scattered X-ray also has a continuous energy distribution, and the influence of the air density in the X-ray pass portion differs depending on the energy. Therefore, when performing the correction calculation, a complicated operation such as dividing continuous X-rays by energy is required. In addition, among continuous X-rays, high-energy X-rays have a large proportion of Compton scattering, a large energy difference between Compton scattering and Rayleigh scattering, and the ratio between Compton scattering and Rayleigh scattering also changes depending on the sample composition. Therefore, the average energy value of scattered X-rays changes, and it is difficult to correct the influence of atmospheric pressure and temperature in a strict sense.
【０００８】本発明は、上述の事柄に留意してなされた
もので、その目的とするところは、試料が液体であって
も測定することができ、しかも、Ｘ線パス部の気圧や温
度変化の影響を受けることなく、経済的に試料分析を行
うことができる蛍光Ｘ線分析装置を提供することにあ
る。The present invention has been made in consideration of the above-mentioned matters, and it is an object of the present invention that it is possible to measure even a sample is a liquid, and moreover, changes in atmospheric pressure and temperature in the X-ray pass portion. An object of the present invention is to provide a fluorescent X-ray analyzer capable of economically performing sample analysis without being affected by.
【０００９】[0009]
【課題を解決するための手段】上記目的を達成するた
め、本発明においては、試料に対して空気層よりなるＸ
線パス部を介して一次Ｘ線を照射し、試料から放出され
る二次Ｘ線に基づいて試料分析を行うようにした蛍光Ｘ
線分析装置において、前記一次Ｘ線として単一エネルギ
ーまたはそれに近い単色の一次Ｘ線を用いると共に、前
記Ｘ線パス部の気圧および温度を測定し、この測定され
た気圧および温度を用いて、前記蛍光Ｘ線および散乱Ｘ
線の強度を補正し、この補正された蛍光Ｘ線と散乱Ｘ線
との比をとるようにしている。In order to achieve the above object, in the present invention, an X layer consisting of an air layer is provided for the sample.
Fluorescent X irradiating primary X-rays through the line path part and performing sample analysis based on secondary X-rays emitted from the sample
In the line analyzer, a single energy or a monochromatic primary X-ray close to it is used as the primary X-ray, and the atmospheric pressure and temperature of the X-ray path portion are measured, and the measured atmospheric pressure and temperature are used to X-ray fluorescence and scattered X
The intensity of the rays is corrected and the ratio between the corrected fluorescent X-rays and scattered X-rays is taken.
【００１０】[0010]
【作用】上記構成の蛍光Ｘ線分析装置によれば、試料が
液体であっても測定を行うことができる。そして、一次
Ｘ線として単一エネルギーまたはそれに近い単色の一次
Ｘ線を用いているので、散乱Ｘ線の平均エネルギー値が
変化することがなくなり、しかも、Ｘ線パス部の気圧お
よび温度を測定し、この測定された気圧および温度を用
いて、蛍光Ｘ線および散乱Ｘ線の強度を補正しているの
で、蛍光Ｘ線と散乱Ｘ線との比をより正確に求めること
ができ、Ｘ線パス部の気圧や温度変化の影響を受けるこ
とがない。According to the X-ray fluorescence analyzer having the above structure, the measurement can be performed even if the sample is a liquid. Further, since the single energy or monochromatic primary X-rays close to it is used as the primary X-rays, the average energy value of the scattered X-rays does not change, and moreover, the pressure and temperature of the X-ray pass portion are measured. Since the intensities of the fluorescent X-rays and the scattered X-rays are corrected using the measured atmospheric pressure and temperature, the ratio between the fluorescent X-rays and the scattered X-rays can be obtained more accurately, and the X-ray path can be obtained. It is not affected by changes in atmospheric pressure or temperature.
【００１１】[0011]
【実施例】以下、本発明の実施例を、図面を参照しなが
ら説明する。Embodiments of the present invention will be described below with reference to the drawings.
【００１２】図１は、本発明に係る蛍光Ｘ線分析装置の
構成を概略的に示すもので、この図において、１は窓２
を備えた試料載置台で、この試料載置台１の窓２が形成
された部分には、試料収容容器３を載置するように構成
されている。試料収容容器３は、例えば筒状の枠体４
と、この枠体４の底部側を閉塞するように張設された樹
脂製のフィルムよりなるＸ線透過膜５とから構成され、
その内部には例えば原油などの液体試料６が収容されて
いる。FIG. 1 schematically shows the structure of an X-ray fluorescence analyzer according to the present invention. In this figure, 1 is a window 2
In the sample mounting table provided with, the sample storage container 3 is mounted on the portion of the sample mounting table 1 where the window 2 is formed. The sample container 3 includes, for example, a cylindrical frame body 4
And an X-ray transmission film 5 made of a resin film stretched so as to close the bottom side of the frame body 4,
A liquid sample 6 such as crude oil is contained in the inside thereof.
【００１３】前記試料載置台１の下方には、空気層より
なるＸ線パス部７を介してＸ線源８が設けられている。
このＸ線源８は、例えば図２に示すように、電子線９を
発する電子銃10と、入射された電子線９を、所定の一次
Ｘ線11に変えて反射するターゲット12とからなるＸ線管
13と、このＸ線管13から出力された一次Ｘ線11をそのエ
ネルギーが単一またはそれに近い状態の単色の一次Ｘ線
（以下、単色Ｘ線と云う）14とするためのＸ線フィルタ
15とからなり、反射型に構成されている。そして、この
Ｘ線源８から発せられた単色Ｘ線14は、Ｘ線パス部７を
およびＸ線透過膜５を介して液体試料６に照射され、液
体試料６からは蛍光Ｘ線および散乱Ｘ線などを含む二次
Ｘ線16が発せられる。An X-ray source 8 is provided below the sample mounting table 1 via an X-ray path unit 7 formed of an air layer.
For example, as shown in FIG. 2, the X-ray source 8 includes an electron gun 10 that emits an electron beam 9 and a target 12 that changes the incident electron beam 9 into a predetermined primary X-ray 11 and reflects it. Wire tube
13 and an X-ray filter for converting the primary X-rays 11 output from the X-ray tube 13 into monochromatic primary X-rays (hereinafter, referred to as monochromatic X-rays) 14 having a single energy or a state close to the energy.
It consists of 15 and is constructed as a reflection type. The monochromatic X-rays 14 emitted from the X-ray source 8 are applied to the liquid sample 6 through the X-ray pass portion 7 and the X-ray transmission film 5, and the liquid sample 6 emits fluorescent X-rays and scattered X-rays. Secondary X-rays 16 including rays are emitted.
【００１４】また、前記試料載置台１の下方には、前記
Ｘ線源８と異なった位置に、同じく空気層よりなるＸ線
パス部７を介して前記二次Ｘ線16を検出する二次Ｘ線検
出部17が設けられている。この二次Ｘ線検出部17は、計
測しようとする波長近傍のノイズを吸収するためのＸ線
フィルタ18、例えばＮｅガス封入比例係数管からなる検
出器19、プリアンプ20、パルス波高分析器21、計数器22
をこの順に備えている。そして、この二次Ｘ線検出部17
からは、測定元素（例えば硫黄）の濃度に応じた蛍光Ｘ
線と散乱Ｘ線の強度が計数値として得られ、この計数結
果はＣＰＵ23に入力される。Below the sample stage 1, at a position different from that of the X-ray source 8, a secondary X-ray 16 for detecting the secondary X-rays 16 is also detected through an X-ray path unit 7 also made of an air layer. An X-ray detector 17 is provided. The secondary X-ray detector 17 includes an X-ray filter 18 for absorbing noise near the wavelength to be measured, for example, a detector 19 including a Ne gas filled proportional coefficient tube, a preamplifier 20, a pulse height analyzer 21, Counter 22
Are provided in this order. Then, this secondary X-ray detector 17
From the fluorescence X depending on the concentration of the measurement element (for example, sulfur)
The intensity of the X-ray and the scattered X-ray is obtained as a count value, and the count result is input to the CPU 23.
【００１５】24, 25は前記空気層よりなるＸ線パス部７
の気圧および温度をそれぞれ測定する気圧計、温度計
で、これらの測定結果はＣＰＵ23に入力される。ＣＰＵ
23においては、気圧計24、温度計25によって測定された
Ｘ線パス部７の気圧および温度を、所定の補正式（例え
ば特開昭60− 61649号公報に開示された式）に入力する
ることにより、二次Ｘ線検出部17から入力された蛍光Ｘ
線と散乱Ｘ線の強度を補正する。そして、この補正され
た蛍光Ｘ線と散乱Ｘ線との比をとることにより、例えば
原油中の硫黄分を測定することができる。なお、26は表
示器である。Numerals 24 and 25 are X-ray pass portions 7 composed of the air layer.
A barometer and a thermometer for measuring the atmospheric pressure and the temperature, respectively, and these measurement results are input to the CPU 23. CPU
In 23, the atmospheric pressure and the temperature of the X-ray path unit 7 measured by the barometer 24 and the thermometer 25 are input to a predetermined correction formula (for example, the formula disclosed in Japanese Patent Laid-Open No. 60-61649). As a result, the fluorescence X input from the secondary X-ray detector 17
Correct the intensity of the X-ray and scattered X-ray. Then, for example, the sulfur content in crude oil can be measured by taking the ratio of the corrected fluorescent X-rays and scattered X-rays. In addition, 26 is a display.
【００１６】上述の説明から明らかなように、本発明に
係る蛍光Ｘ線分析装置においては、一次Ｘ線として単一
エネルギーまたはそれに近い単色の一次Ｘ線14を用いて
いるので、散乱Ｘ線の平均エネルギー値が変化すること
がなくなり、しかも、Ｘ線パス部７の気圧および温度を
測定し、この測定された気圧および温度を用いて、蛍光
Ｘ線および散乱Ｘ線の強度を補正しているので、蛍光Ｘ
線と散乱Ｘ線との比をより正確に求めることができ、Ｘ
線パス部７の気圧や温度変化の影響を受けることがな
い。また、Ｘ線パス部７は空気層よりなるので、固体試
料は勿論のこと、液体試料も測定することができる。As is clear from the above description, in the fluorescent X-ray analysis apparatus according to the present invention, since the primary X-rays are monoenergetic primary X-rays 14 having a single energy or a near single energy, scattered X-rays The average energy value does not change, and the atmospheric pressure and temperature of the X-ray pass portion 7 are measured, and the measured atmospheric pressure and temperature are used to correct the intensity of the fluorescent X-rays and scattered X-rays. So fluorescent X
The ratio between the X-ray and the scattered X-ray can be calculated more accurately, and X
It is not affected by changes in atmospheric pressure or temperature in the line pass section 7. Further, since the X-ray pass unit 7 is composed of an air layer, not only a solid sample but also a liquid sample can be measured.
【００１７】本発明は、上記実施例に限られるものでは
なく、例えばＸ線源８におけるＸ線フィルタ15に代えて
分光結晶を用いるようにしてもよい。また、Ｘ線源８
を、図３に示すように、透過型に構成してもよい。この
図において、27は薄膜状のターゲットで、Ｘ線フィルタ
の機能をも備えており、Ｘ線源８からのＸ線をこのター
ゲット27を通過させることにより、単色に近い一次Ｘ線
が得られる。The present invention is not limited to the above embodiment, and for example, a dispersive crystal may be used instead of the X-ray filter 15 in the X-ray source 8. In addition, the X-ray source 8
May be of a transmissive type, as shown in FIG. In this figure, 27 is a thin film target, which also has the function of an X-ray filter. By passing X-rays from the X-ray source 8 through the target 27, primary X-rays close to a single color can be obtained. ..
【００１８】[0018]
【発明の効果】以上説明したように、本発明によれば、
試料が固体の場合は勿論のこと、液体であっても測定す
ることができ、しかも、高価なヘリウムガスを用いなく
とも、Ｘ線パス部の気圧や温度変化の影響を受けない精
度の高い測定を行うことができると共に、標準試料によ
る装置の校正の間隔を長くすることができるので、経済
的に試料分析を行うことができる。As described above, according to the present invention,
Not only when the sample is a solid, but also when it is a liquid, it can be measured, and even if expensive helium gas is not used, it is highly accurate measurement that is not affected by changes in atmospheric pressure or temperature in the X-ray path section. In addition to being able to perform the above, it is possible to extend the interval of calibration of the device with the standard sample, so that the sample analysis can be performed economically.
【図１】本発明に係る蛍光Ｘ線分析装置の構成を概略的
に示す図である。FIG. 1 is a diagram schematically showing the configuration of an X-ray fluorescence analyzer according to the present invention.
【図２】Ｘ線源の構成例を示す図である。FIG. 2 is a diagram showing a configuration example of an X-ray source.
【図３】Ｘ線源の他の構成例を示す図である。FIG. 3 is a diagram showing another configuration example of an X-ray source.
６…試料、７…Ｘ線パス部、14…一次Ｘ線、16…二次Ｘ
線。6 ... Sample, 7 ... X-ray pass part, 14 ... Primary X-ray, 16 ... Secondary X
line.
Claims (1)
を介して一次Ｘ線を照射し、試料から放出される二次Ｘ
線に基づいて試料分析を行うようにした蛍光Ｘ線分析装
置において、前記一次Ｘ線として単一エネルギーまたは
それに近い単色の一次Ｘ線を用いると共に、前記Ｘ線パ
ス部の気圧および温度を測定し、この測定された気圧お
よび温度を用いて、前記蛍光Ｘ線および散乱Ｘ線の強度
を補正し、この補正された蛍光Ｘ線と散乱Ｘ線との比を
とるようにしたことを特徴とする蛍光Ｘ線分析装置。1. A secondary X emitted from the sample by irradiating the sample with a primary X-ray through an X-ray path portion formed of an air layer.
In a fluorescent X-ray analysis apparatus adapted to perform sample analysis based on X-rays, a single energy or a monochromatic primary X-ray close to it is used as the primary X-ray, and the atmospheric pressure and temperature of the X-ray pass portion are measured. The intensity of the fluorescent X-rays and the scattered X-rays is corrected by using the measured atmospheric pressure and temperature, and the ratio between the corrected fluorescent X-rays and the scattered X-rays is obtained. X-ray fluorescence analyzer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3304198A JP2613511B2 (en) | 1991-10-23 | 1991-10-23 | X-ray fluorescence analyzer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3304198A JP2613511B2 (en) | 1991-10-23 | 1991-10-23 | X-ray fluorescence analyzer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05119000A true JPH05119000A (en) | 1993-05-14 |
| JP2613511B2 JP2613511B2 (en) | 1997-05-28 |
Family
ID=17930201
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3304198A Expired - Fee Related JP2613511B2 (en) | 1991-10-23 | 1991-10-23 | X-ray fluorescence analyzer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2613511B2 (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2096431A1 (en) * | 2008-02-27 | 2009-09-02 | Oxford Instruments Analytical Oy | Portable X-ray fluorescence analyzer |
| JP2014145618A (en) * | 2013-01-28 | 2014-08-14 | Dkk Toa Corp | Energy dispersive fluorescent x-ray analyzer |
| KR20190041161A (en) * | 2017-10-12 | 2019-04-22 | 주식회사 포스코 | Apparatus for measuring component of coating |
| EP3745122A3 (en) * | 2019-05-31 | 2020-12-16 | Jeol Ltd. | X-ray analyzer |
| US20220365008A1 (en) * | 2021-05-14 | 2022-11-17 | Malvern Panalytical B.V. | Apparatus and Method for X-ray Fluorescence Analysis |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5160591A (en) * | 1974-11-22 | 1976-05-26 | Mitsubishi Electric Corp | Keiko x seniobunsekisochi |
| JPS5786030A (en) * | 1980-11-17 | 1982-05-28 | Idemitsu Kosan Co Ltd | Method and apparatus for analysis of fluorescence x-rays |
| JPS6061649A (en) * | 1983-09-16 | 1985-04-09 | Rigaku Denki Kogyo Kk | Correction of x-ray fluorescence analysis |
| JPH02257045A (en) * | 1989-03-30 | 1990-10-17 | Nkk Corp | Method and device for measuring plated deposit of plated steel sheet and composition of plated film |
-
1991
- 1991-10-23 JP JP3304198A patent/JP2613511B2/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5160591A (en) * | 1974-11-22 | 1976-05-26 | Mitsubishi Electric Corp | Keiko x seniobunsekisochi |
| JPS5786030A (en) * | 1980-11-17 | 1982-05-28 | Idemitsu Kosan Co Ltd | Method and apparatus for analysis of fluorescence x-rays |
| JPS6061649A (en) * | 1983-09-16 | 1985-04-09 | Rigaku Denki Kogyo Kk | Correction of x-ray fluorescence analysis |
| JPH02257045A (en) * | 1989-03-30 | 1990-10-17 | Nkk Corp | Method and device for measuring plated deposit of plated steel sheet and composition of plated film |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2096431A1 (en) * | 2008-02-27 | 2009-09-02 | Oxford Instruments Analytical Oy | Portable X-ray fluorescence analyzer |
| JP2014145618A (en) * | 2013-01-28 | 2014-08-14 | Dkk Toa Corp | Energy dispersive fluorescent x-ray analyzer |
| KR20190041161A (en) * | 2017-10-12 | 2019-04-22 | 주식회사 포스코 | Apparatus for measuring component of coating |
| EP3745122A3 (en) * | 2019-05-31 | 2020-12-16 | Jeol Ltd. | X-ray analyzer |
| US20220365008A1 (en) * | 2021-05-14 | 2022-11-17 | Malvern Panalytical B.V. | Apparatus and Method for X-ray Fluorescence Analysis |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2613511B2 (en) | 1997-05-28 |
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