JP2001221753A - Wavelength dispersive type fluorescent x-ray analytical method and device - Google Patents

Wavelength dispersive type fluorescent x-ray analytical method and device

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Publication number
JP2001221753A
JP2001221753A JP2000032878A JP2000032878A JP2001221753A JP 2001221753 A JP2001221753 A JP 2001221753A JP 2000032878 A JP2000032878 A JP 2000032878A JP 2000032878 A JP2000032878 A JP 2000032878A JP 2001221753 A JP2001221753 A JP 2001221753A
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JP
Japan
Prior art keywords
voltage
pulse
predetermined
rays
ray
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
Application number
JP2000032878A
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Japanese (ja)
Other versions
JP3394936B2 (en
Inventor
Yoshiyuki Kataoka
由行 片岡
Takashi Nishimura
隆 西村
Etsuhisa Yamamoto
悦久 山本
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Rigaku Corp
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Rigaku Industrial Corp
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Abstract

PROBLEM TO BE SOLVED: To provide a method or the like capable of selecting accurately the pulse of a voltage corresponding to the wavelength of a fluorescent X-ray to be measured among pulses generated from a detector and sent to a pulse height analyzer, and thereby executing accurate analysis, in a wavelength dispersive type and scanning type fluorescent X-ray analytical method or the like. SOLUTION: Deviation from a proportional relation between energy E of an incident secondary X-ray 7 and the voltage of a generated pulse at a detector 8 is obtained beforehand, for example, as a function of energy f (E), and correction is executed by applying the function f (E) when a prescribed amplification factor G of an amplifier 16 or the like is adjusted.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は、いわゆる波長分散
型であって走査型の蛍光X線分析方法および装置に装置
に関するものである。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a so-called wavelength dispersive and scanning X-ray fluorescence analysis method and apparatus.

【0002】[0002]

【従来の技術】従来より、例えば波長分散型の蛍光X線
分析においては、試料に1次X線を照射し、試料から発
生する蛍光X線を分光素子で分光し、分光された蛍光X
線を検出器で検出してパルスを発生させる。このパルス
の電圧すなわち波高値は蛍光X線のエネルギーに応じた
ものであり、具体的には、比例関係にあると考えられて
いる。また、パルスの単位時間あたりの数は蛍光X線の
強度に応じたものである。そこで、パルスのうち所定の
電圧の範囲のものを波高分析器で選別して、その計数率
(単位時間あたりのパルス数)をスケーラ等の計数手段
で求めている。なお、検出器が発生するパルスは微弱で
あるので、検出器内蔵のプリアンプと、外部のリニアア
ンプによって、それぞれ所定の増幅率で増幅されて、波
高分析器へ送られる。リニアアンプを波高分析器に含め
ることもある。
2. Description of the Related Art Conventionally, for example, in a wavelength-dispersive X-ray fluorescence analysis, a sample is irradiated with primary X-rays, X-rays generated from the sample are separated by a spectroscopic element, and the separated fluorescent X-rays are used.
The line is detected by a detector to generate a pulse. The voltage of the pulse, that is, the peak value, depends on the energy of the fluorescent X-rays, and specifically, is considered to have a proportional relationship. The number of pulses per unit time depends on the intensity of fluorescent X-rays. Therefore, pulses having a predetermined voltage range among the pulses are selected by a pulse height analyzer, and the counting rate (the number of pulses per unit time) is obtained by a counting means such as a scaler. Since the pulse generated by the detector is weak, the pulse is amplified at a predetermined amplification factor by a preamplifier built in the detector and an external linear amplifier, and sent to the pulse height analyzer. A linear amplifier may be included in the pulse height analyzer.

【0003】ここで、走査(スキャン)型の分析におい
ては、いわゆるゴニオメータ等の連動手段により、分光
素子で分光される蛍光X線の波長を変えながら、その分
光された蛍光X線が検出器に入射するように、分光素子
と検出器を連動させて走査させ、広い波長範囲において
蛍光X線の強度を測定する。このとき、検出器に入射す
る蛍光X線の波長が変化し、すなわち蛍光X線のエネル
ギーが変化するから、このままでは、検出器から発生し
波高分析器へ送られるパルスの電圧も変化する。そうす
ると、測定すべき蛍光X線の波長に対応した電圧のパル
スを選別するには、波高分析器における前記所定の電圧
の範囲、具体的には通過させるパルスの電圧の上限値と
下限値を、送られてくるパルスの電圧の変化に追従させ
て設定し直さなければならず、煩雑である。
Here, in a scanning (scan) type analysis, while the wavelength of the fluorescent X-rays separated by the spectroscopic element is changed by interlocking means such as a so-called goniometer, the separated fluorescent X-rays are sent to a detector. The spectroscopic element and the detector are scanned so as to be incident so as to be incident, and the intensity of the fluorescent X-ray is measured in a wide wavelength range. At this time, since the wavelength of the fluorescent X-rays incident on the detector changes, that is, the energy of the fluorescent X-rays changes, the voltage of the pulse generated from the detector and sent to the pulse height analyzer also changes. Then, in order to select the pulse of the voltage corresponding to the wavelength of the fluorescent X-ray to be measured, the predetermined voltage range in the pulse height analyzer, specifically, the upper limit and the lower limit of the voltage of the pulse to be passed, The setting must be reset following the change in the voltage of the transmitted pulse, which is complicated.

【0004】そこで、従来は、連動手段により、例え
ば、前記リニアアンプ(以下、増幅器という)における
所定の増幅率を、検出器に入射する蛍光X線のエネルギ
ーに反比例するように、具体的には分光素子での回折角
θについてのsin θに比例するように連続的に調節し
て、波高分析器へ送られるパルスの電圧が一定になるよ
うにし、前記所定の電圧の範囲の設定変更を不要にして
いる。このように調節するのは、前述したように、検出
器において入射される蛍光X線のエネルギーと発生する
パルスの電圧とが比例関係にあるとの前提に立っている
からである。
Therefore, conventionally, the interlocking means is used to set a predetermined amplification factor in the linear amplifier (hereinafter, referred to as an amplifier, for example) so as to be inversely proportional to the energy of the fluorescent X-ray incident on the detector. The diffraction angle θ of the spectroscopic element is continuously adjusted so as to be proportional to sin θ, so that the voltage of the pulse sent to the pulse height analyzer becomes constant, and it is unnecessary to change the setting of the predetermined voltage range. I have to. The reason for this adjustment is that, as described above, it is based on the premise that the energy of the fluorescent X-rays incident on the detector and the voltage of the generated pulse are in a proportional relationship.

【0005】[0005]

【発明が解決しようとする課題】しかし、検出器が例え
ばシンチレーションカウンタである場合には、前記比例
関係からのずれがあるため、従来技術によっては、測定
すべき蛍光X線の波長に対応した電圧のパルスを正確に
選別できず、したがって正確な分析ができない。
However, when the detector is, for example, a scintillation counter, there is a deviation from the above proportional relationship. Cannot be accurately selected, and thus cannot be analyzed accurately.

【0006】本発明は前記従来の問題に鑑みてなされた
もので、波長分散型であって走査型の蛍光X線分析方法
および装置において、検出器から発生して波高分析器へ
送られるパルスのうち、測定すべき蛍光X線の波長に対
応した電圧のパルスを正確に選別でき、したがって正確
な分析ができる方法および装置を提供することを目的と
する。
SUMMARY OF THE INVENTION The present invention has been made in view of the above-mentioned conventional problems. In a wavelength-dispersive and scanning X-ray fluorescence analysis method and apparatus, there is provided a method for detecting a pulse generated from a detector and sent to a pulse height analyzer. It is an object of the present invention to provide a method and an apparatus capable of accurately selecting a pulse having a voltage corresponding to the wavelength of the fluorescent X-ray to be measured, and thus performing an accurate analysis.

【0007】[0007]

【課題を解決するための手段】前記目的を達成するため
に、請求項1の波長分散型蛍光X線分析方法は、試料に
1次X線を照射し、発生した2次X線を分光素子で分光
し、分光される2次X線の波長を変化させながら、所定
の電圧を印加した検出器に入射させて、前記所定の印加
電圧と2次X線のエネルギーに応じた電圧のパルスを2
次X線の強度に応じた数だけ発生させる。そして、発生
したパルスの電圧を増幅器により所定の増幅率で増幅
し、増幅されたパルスのうち所定の電圧の範囲のものを
波高分析器で選別するとともに、前記波高分析器へ送ら
れるパルスの電圧を一定にするために、前記所定の印加
電圧または所定の増幅率を調節し、前記選別されたパル
スの計数率を計数手段で求める。すなわち、波長分散型
であって走査型の蛍光X線分析方法である。
According to a first aspect of the present invention, there is provided a wavelength-dispersive X-ray fluorescence analysis method comprising: irradiating a sample with primary X-rays; While changing the wavelength of the secondary X-ray to be separated, the light is incident on a detector to which a predetermined voltage is applied, and a pulse of a voltage corresponding to the predetermined applied voltage and the energy of the secondary X-ray is generated. 2
It is generated by the number corresponding to the intensity of the next X-ray. Then, the voltage of the generated pulse is amplified at a predetermined amplification rate by an amplifier, and those in a predetermined voltage range among the amplified pulses are selected by a pulse height analyzer, and the voltage of the pulse sent to the pulse height analyzer is selected. Is adjusted to adjust the predetermined applied voltage or the predetermined amplification factor, and the counting rate of the selected pulse is obtained by the counting means. That is, it is a wavelength-dispersive and scanning X-ray fluorescence analysis method.

【0008】さらに、請求項1の方法では、前記検出器
における入射される2次X線のエネルギーと発生するパ
ルスの電圧との比例関係からのずれを、前記エネルギー
の関数または前記分光素子の格子面間隔と回折角の関数
としてあらかじめ求めておき、前記所定の印加電圧また
は所定の増幅率を調節する際に、前記関数を適用して補
正する。
Further, in the method according to the first aspect, the deviation from the proportionality between the energy of the incident secondary X-rays and the voltage of the generated pulse in the detector is determined by a function of the energy or the grating of the spectroscopic element. It is obtained in advance as a function of the surface spacing and the diffraction angle, and is adjusted by applying the function when adjusting the predetermined applied voltage or the predetermined amplification factor.

【0009】請求項1の方法によれば、検出器における
入射される2次X線のエネルギーと発生するパルスの電
圧との比例関係からのずれを、エネルギー等の関数とし
てあらかじめ求めておき、増幅器の所定の増幅率等を調
節する際に、前記関数を適用して補正するので、検出器
から発生して波高分析器へ送られるパルスのうち、測定
すべき蛍光X線等の2次X線の波長に対応した電圧のパ
ルスを正確に選別でき、したがって正確な分析ができ
る。
According to the method of the first aspect, the deviation from the proportional relationship between the energy of the incident secondary X-ray and the voltage of the generated pulse in the detector is obtained in advance as a function of the energy and the like, and When adjusting the predetermined amplification factor or the like, the above-mentioned function is applied for correction, so that among the pulses generated from the detector and sent to the pulse height analyzer, secondary X-rays such as fluorescent X-rays to be measured are included. The pulse of the voltage corresponding to the wavelength can be accurately selected, and the accurate analysis can be performed.

【0010】請求項2の波長分散型蛍光X線分析方法
は、検出器から発生したパルスの電圧を増幅して、所定
の電圧の範囲のものを波高分析器で選別し、選別された
パルスの計数率を計数手段で求める点は、請求項1の方
法と同様であるが、波高分析器へ送られるパルスの電圧
の変化に追従するために、波高分析器が選別する前記所
定の電圧の範囲を調節する点が異なる。それに対応し
て、検出器における入射される2次X線のエネルギーと
発生するパルスの電圧との比例関係からのずれを、前記
エネルギーの関数または前記分光素子の格子面間隔と回
折角の関数としてあらかじめ求めておく点は、請求項1
の方法と同様であるが、前記所定の電圧の範囲を調節す
る際に、前記関数を適用して補正する点が異なる。
According to a second aspect of the present invention, a voltage of a pulse generated from a detector is amplified, and a voltage within a predetermined voltage range is selected by a pulse height analyzer. The point at which the counting rate is determined by the counting means is the same as that of the method of claim 1, but the range of the predetermined voltage selected by the pulse height analyzer in order to follow a change in the voltage of the pulse sent to the pulse height analyzer. The point of adjusting is different. Correspondingly, the deviation from the proportionality between the energy of the incident secondary X-rays and the voltage of the generated pulse in the detector is calculated as a function of the energy or a function of the lattice spacing and diffraction angle of the spectral element. The point to be determined in advance is claim 1
The method is the same as that described above, except that the function is applied and corrected when the predetermined voltage range is adjusted.

【0011】請求項2の方法によれば、検出器における
入射される2次X線のエネルギーと発生するパルスの電
圧との比例関係からのずれを、エネルギー等の関数とし
てあらかじめ求めておき、波高分析器が選別する所定の
電圧の範囲を調節する際に、前記関数を適用して補正す
るので、やはり、検出器から発生して波高分析器へ送ら
れるパルスのうち、測定すべき蛍光X線等の2次X線の
波長に対応した電圧のパルスを正確に選別でき、したが
って正確な分析ができる。
According to the second aspect of the present invention, the deviation from the proportional relationship between the energy of the incident secondary X-ray and the voltage of the generated pulse in the detector is obtained in advance as a function of the energy or the like, and the wave height is determined. When adjusting the predetermined voltage range selected by the analyzer, correction is performed by applying the above-described function, so that the fluorescent X-ray to be measured is also included in the pulses generated from the detector and sent to the pulse height analyzer. And the like, and a pulse of a voltage corresponding to the wavelength of the secondary X-ray can be accurately selected, and thus accurate analysis can be performed.

【0012】請求項3の波長分散型蛍光X線分析装置
は、まず、試料に1次X線を照射するX線源と、試料か
ら発生した2次X線を分光する分光素子と、所定の電圧
が印加され、前記分光素子で分光された2次X線が入射
されて、前記所定の印加電圧と2次X線のエネルギーに
応じた電圧のパルスを2次X線の強度に応じた数だけ発
生させる検出器と、その検出器で発生したパルスの電圧
を所定の増幅率で増幅する増幅器と、その増幅器で増幅
されたパルスのうち所定の電圧の範囲のものを選別する
波高分析器と、その波高分析器で選別されたパルスの計
数率を求める計数手段とを備えている。そして、前記検
出器に入射する2次X線の波長を変化させるとともに、
前記波高分析器へ送られるパルスの電圧を一定にするた
めに、前記所定の印加電圧または所定の増幅率を調節す
る連動手段を備えている。すなわち、波長分散型であっ
て走査型の蛍光X線分析装置である。
According to a third aspect of the present invention, an X-ray source for irradiating a sample with primary X-rays, a spectroscopic element for dispersing secondary X-rays generated from the sample, A voltage is applied, secondary X-rays dispersed by the spectral element are incident, and a pulse of a voltage corresponding to the predetermined applied voltage and the energy of the secondary X-ray is generated according to the intensity of the secondary X-ray. And a pulse height analyzer that amplifies the voltage of the pulse generated by the detector at a predetermined amplification rate, and a pulse height analyzer that selects pulses within a predetermined voltage range among the pulses amplified by the amplifier. Counting means for determining the counting rate of the pulses selected by the wave height analyzer. Then, while changing the wavelength of the secondary X-ray incident on the detector,
There is provided interlocking means for adjusting the predetermined applied voltage or the predetermined amplification factor in order to keep the voltage of the pulse sent to the pulse height analyzer constant. That is, it is a wavelength-dispersive and scanning X-ray fluorescence analyzer.

【0013】さらに、請求項3の装置は、前記検出器に
おける入射される2次X線のエネルギーと発生するパル
スの電圧との比例関係からのずれを、あらかじめ求めら
れた前記エネルギーの関数または前記分光素子の格子面
間隔と回折角の関数として記憶する記憶手段を備え、前
記連動手段が、前記所定の印加電圧または所定の増幅率
を調節する際に、前記記憶手段に記憶した関数を適用し
て補正する。請求項3の装置によれば、請求項1の方法
と同様の作用効果がある。
Further, the apparatus according to the present invention is characterized in that the deviation from the proportionality between the energy of the incident secondary X-rays and the voltage of the generated pulse in the detector is determined by a function of the energy determined in advance or the deviation. Storage means for storing as a function of the grating plane spacing and diffraction angle of the spectral element, wherein the interlocking means applies the function stored in the storage means when adjusting the predetermined applied voltage or the predetermined amplification factor. To correct. According to the device of the third aspect, the same operation and effect as those of the method of the first aspect are obtained.

【0014】請求項4の波長分散型蛍光X線分析装置
は、X線源、分光素子、検出器、増幅器、波高分析器お
よび計数手段を備える点は、請求項3の装置と同様であ
るが、連動手段が、前記検出器に入射する2次X線の波
長を変化させるとともに、前記波高分析器へ送られるパ
ルスの電圧の変化に追従するために、前記所定の電圧の
範囲を調節する点が異なる。それに対応して、記憶手段
を備える点は、請求項3の装置と同様であるが、前記連
動手段が、前記所定の電圧の範囲を調節する際に、前記
関数を適用して補正する点が異なる。請求項4の装置に
よれば、請求項2の方法と同様の作用効果がある。
A wavelength dispersive X-ray fluorescence analyzer according to a fourth aspect is similar to the apparatus according to the third aspect in that it comprises an X-ray source, a spectroscopic element, a detector, an amplifier, a pulse height analyzer and a counting means. The interlocking means changes the wavelength of the secondary X-rays incident on the detector and adjusts the predetermined voltage range in order to follow the change in the voltage of the pulse sent to the pulse height analyzer. Are different. Correspondingly, the point that the storage means is provided is the same as that of the device of claim 3, except that the interlocking means corrects by applying the function when adjusting the predetermined voltage range. different. According to the device of the fourth aspect, the same operation and effect as those of the method of the second aspect are obtained.

【0015】[0015]

【発明の実施の形態】以下、本発明の第1実施形態の方
法について説明する。まず、この方法に用いる装置につ
いて、図1にしたがって説明する。この装置は、試料1
が載置される試料台2と、試料1に1次X線3を照射す
るX線管等のX線源4と、試料1から発生した蛍光X線
等の2次X線5を分光する分光素子6と、所定の電圧が
印加され、分光素子6で分光された2次X線7が入射さ
れて、前記所定の印加電圧と2次X線7のエネルギーに
応じた電圧のパルスを2次X線7の強度に応じた数だけ
発生させる検出器8と、検出器8で発生したパルスの電
圧を所定の増幅率で増幅する増幅器16と、増幅器16
で増幅されたパルスのうち所定の電圧の範囲のものを選
別する波高分析器13と、波高分析器13で選別された
パルスの計数率を求める計数手段14とを備えている。
分光素子は、複数を交換(選択)して使用してもよい。
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, a method according to a first embodiment of the present invention will be described. First, an apparatus used in this method will be described with reference to FIG. This device uses sample 1
, A sample X-ray source 4 such as an X-ray tube for irradiating the sample 1 with primary X-rays 3 and a secondary X-ray 5 such as fluorescent X-rays generated from the sample 1. The spectroscopic element 6 is applied with a predetermined voltage, the secondary X-rays 7 separated by the spectroscopic element 6 are incident, and a pulse of a voltage corresponding to the predetermined applied voltage and the energy of the secondary X-ray 7 is generated. A detector 8 for generating a number corresponding to the intensity of the next X-ray 7, an amplifier 16 for amplifying a voltage of a pulse generated by the detector 8 at a predetermined amplification factor, and an amplifier 16
The pulse height analyzer 13 includes a pulse height analyzer 13 for selecting pulses within a predetermined voltage range among the pulses amplified by the pulse generator, and a counting unit 14 for determining a count rate of the pulses selected by the pulse height analyzer 13.
A plurality of spectroscopic elements may be exchanged (selected) for use.

【0016】そして、検出器8に入射する2次X線7の
波長が変化するように、分光素子6と検出器8を連動さ
せる連動手段10、すなわちいわゆるゴニオメータを備
えている。2次X線5がある入射角θで分光素子6へ入
射すると、その2次X線5の延長線9と分光素子6で分
光(回折)された2次X線7は入射角(回折角)θの2
倍の分光角2θをなすが、連動手段10は、分光角2θ
を変化させて分光される2次X線7の波長を変化させつ
つ、その分光された2次X線7が検出器8に入射し続け
るように、分光素子6を、その表面の中心を通る紙面に
垂直な軸Oを中心に回転させ、その回転角の2倍だけ、
検出器8を、軸Oを中心に円12に沿って回転させる。
Further, there is provided a linking means 10 for linking the spectroscopic element 6 and the detector 8, that is, a so-called goniometer, so that the wavelength of the secondary X-ray 7 incident on the detector 8 changes. When the secondary X-rays 5 enter the spectroscopic element 6 at a certain incident angle θ, the extension line 9 of the secondary X-rays 5 and the secondary X-rays 7 spectrally (diffracted) by the spectroscopic element 6 become incident angles (diffraction angles). ) 2 of θ
The interlocking means 10 has a spectral angle of 2θ.
The spectroscopic element 6 passes through the center of the surface of the spectroscopic element 6 so that the spectroscopic secondary X-ray 7 continues to be incident on the detector 8 while changing the wavelength of the secondary X-ray 7 that is spectroscopically changed. Rotate around the axis O perpendicular to the plane of the paper, and twice the rotation angle,
The detector 8 is rotated along the circle 12 about the axis O.

【0017】連動手段10において、例えば、前記軸O
に取り付けられたギアを駆動するパルスモータに出力し
たパルス数をカウントすることにより、分光素子6およ
び検出器8が回転した結果形成される入射角(回折角)
θ、分光角2θが確認され、分光素子6の格子面間隔d
とから、次式(1)のブラッグの条件、式(2)の関係
に基づいて、測定中の2次X線の波長λ、エネルギーE
を求めることができる。なお、nは反射の次数である
が、通常は1次線を測定するのでn=1であり、hはプ
ランク定数、cは光速である。
In the interlocking means 10, for example, the shaft O
By counting the number of pulses output to a pulse motor that drives a gear attached to the lens, an incident angle (diffraction angle) formed as a result of rotation of the spectroscopic element 6 and the detector 8
θ and the spectral angle 2θ are confirmed, and the lattice spacing d of the spectral element 6 is determined.
From the above, based on the Bragg condition of the following equation (1) and the relationship of the equation (2), the wavelength λ and energy E of the secondary X-ray being measured are
Can be requested. Note that n is the order of reflection, but since a primary line is usually measured, n = 1, h is Planck's constant, and c is the speed of light.

【0018】2d sinθ=nλ …(1)2d sin θ = nλ (1)

【0019】E=hc/λ …(2)E = hc / λ (2)

【0020】この連動手段10は、前述のように検出器
8に入射する2次X線7の波長を変化させるとともに、
波高分析器13へ送られるパルスの電圧を一定にするた
めに、前記増幅器16の所定の増幅率を調節する。以上
のように、この装置は、波長分散型であって走査型の蛍
光X線分析装置である。
The interlocking means 10 changes the wavelength of the secondary X-ray 7 incident on the detector 8 as described above,
In order to make the voltage of the pulse sent to the peak analyzer 13 constant, a predetermined amplification factor of the amplifier 16 is adjusted. As described above, this apparatus is a wavelength-dispersive and scanning X-ray fluorescence analyzer.

【0021】さて、この装置の連動手段10における前
記所定の増幅率Gの調節について、説明する。まず、従
来のように、検出器8において入射される2次X線7の
エネルギーEと発生するパルスの電圧とが比例関係にあ
ると考えると、検出器8に入射される2次X線7のエネ
ルギーE、増幅器16の増幅率(ゲイン)G、波高分析
器13へ送られるパルスの電圧(波高値)PH の間に
は、次式(3)が成立し、さらに前式(1)、(2)を
代入すれば、式(4)が成立する。なお、k1 ,k2
定数である。
Now, adjustment of the predetermined gain G in the interlocking means 10 of this device will be described. First, assuming that the energy E of the secondary X-rays 7 incident on the detector 8 and the voltage of the generated pulse are in a proportional relationship as in the related art, the secondary X-rays 7 incident on the detector 8 are considered. energy E, the amplification factor of the amplifier 16 (gain) G, between the pulse of the voltage (peak value) P H sent to the pulse height analyzer 13, the following equation (3) is satisfied, further equation (1) , (2), equation (4) holds. Note that k 1 and k 2 are constants.

【0022】PH =k1 EG …(3)P H = k 1 EG (3)

【0023】PH =k2 G/2d sinθ …(4)P H = k 2 G / 2d sin θ (4)

【0024】これに基づいて、従来は、波高分析器13
が選別する前記所定の電圧の範囲を設定変更せずに済む
ように、すなわち、波高分析器13へ送られるパルスの
電圧PH を一定にすべく、増幅器16の増幅率Gを、次
式(5)のように装置付属のコンピュータで計算して調
節していた。なお、k3 は定数である。
Based on this, conventionally, the wave height analyzer 13
In order that the range of the predetermined voltage to be selected does not need to be changed, that is, in order to keep the voltage P H of the pulse sent to the pulse height analyzer 13 constant, the amplification factor G of the amplifier 16 is set as follows: As described in 5), it was calculated and adjusted by the computer attached to the device. Incidentally, k 3 are constants.

【0025】G=k3 ・2d sinθ …(5)G = k 3 · 2d sin θ (5)

【0026】このとき、PH =k2 3 で一定となるは
ずである。しかし、前述したように、検出器8が例えば
シンチレーションカウンタである場合には、入射される
2次X線7のエネルギーEと発生するパルスの電圧とが
正確には比例関係にないため、このままでは、波高分析
器13へ送られるパルスの電圧PH が一定にならず、測
定すべき蛍光X線7の波長λに対応した電圧PH のパル
スを正確に選別できない。
At this time, it should be constant at P H = k 2 k 3 . However, as described above, when the detector 8 is, for example, a scintillation counter, the energy E of the incident secondary X-ray 7 and the voltage of the generated pulse are not exactly in a proportional relationship. , not the voltage P H of pulses sent to the pulse height analyzer 13 is constant, can not be accurately sorted pulse voltage P H corresponding to the wavelength λ of the fluorescent X-ray 7 to be measured.

【0027】そこで、この装置においては、検出器8に
おける入射される2次X線7のエネルギーEと発生する
パルスの電圧との比例関係からのずれを、例えばエネル
ギーEの関数f(E)として、実際の測定によりあらか
じめ求めて記憶手段15に記憶させておき、連動手段1
0は、増幅率Gを調節する際に、記憶手段15に記憶し
た関数f(E)を適用して補正する。すなわち、連動手
段10は、増幅器16の増幅率Gを、次式(6)のよう
に調節する。なお、k4 は定数である。
Therefore, in this apparatus, the deviation from the proportional relationship between the energy E of the incident secondary X-ray 7 and the voltage of the generated pulse in the detector 8 is defined as a function f (E) of the energy E, for example. In advance, it is determined in advance by actual measurement and stored in the storage means 15 so that the interlocking means 1
0 is corrected by applying the function f (E) stored in the storage means 15 when adjusting the amplification factor G. That is, the interlocking means 10 adjusts the gain G of the amplifier 16 as in the following equation (6). Incidentally, k 4 are constants.

【0028】 G=k4 ・2d sinθ・f(E) …(6)[0028] G = k 4 · 2d sinθ · f (E) ... (6)

【0029】関数f(E)は、実測値に基づく表として
記憶され、表にない値が必要になった場合には、補間計
算により算出される。また、前式(1)、(2)の関係
があることから、前記比例関係からのずれは、分光素子
6の格子面間隔dと回折角θの関数f(2d sinθ)と
して求めてもよい。
The function f (E) is stored as a table based on measured values, and is calculated by interpolation when a value not in the table is required. Further, since there is the relationship of the above formulas (1) and (2), the deviation from the proportional relationship may be obtained as a function f (2d sin θ) of the grating plane distance d of the spectral element 6 and the diffraction angle θ. .

【0030】また、検出器8から発生するパルスの電圧
は検出器8に印加される電圧Vに対して指数関数的に変
化するので、波高分析器13へ送られるパルスの電圧P
H を一定にするためには、増幅器16の増幅率Gを調節
する代わりに、検出器8への印加電圧Vを調節してもよ
い。この場合、連動手段10では、前式(6)に代えて
次式(7)が用いられる。なお、V0 は基準となる電圧
で定数である。
Since the voltage of the pulse generated from the detector 8 changes exponentially with respect to the voltage V applied to the detector 8, the voltage P of the pulse sent to the pulse height analyzer 13 is changed.
In order to keep H constant, instead of adjusting the gain G of the amplifier 16, the voltage V applied to the detector 8 may be adjusted. In this case, in the interlocking means 10, the following equation (7) is used instead of the previous equation (6). V 0 is a reference voltage and is a constant.

【0031】 V=V0 +ln2d+ln sinθ+ ln f(E) …(7)V = V 0 + ln2d + ln sin θ + ln f (E) (7)

【0032】次に、この装置を用いる第1実施形態の方
法について説明する。まず、試料台2に載置した試料1
に1次X線3を照射し、発生した2次X線5を分光素子
6で分光し、分光される2次X線7の波長を連動手段1
0で変化させながら、所定の電圧Vを印加した検出器8
に入射させて、前記所定の印加電圧Vと2次X線7のエ
ネルギーEに応じた電圧のパルスを2次X線7の強度に
応じた数だけ発生させる。そして、発生したパルスの電
圧を増幅器16により所定の増幅率で増幅し、増幅され
たパルスのうち所定の電圧の範囲のものを波高分析器1
3で選別するとともに、波高分析器へ送られるパルスの
電圧PH を一定にするために、連動手段10で前記所定
の印加電圧Vまたは所定の増幅率Gを調節し、前記選別
されたパルスの計数率を計数手段14で求める。すなわ
ち、第1実施形態の方法は、波長分散型であって走査型
の蛍光X線分析方法である。
Next, a method of the first embodiment using this apparatus will be described. First, the sample 1 placed on the sample stage 2
Is irradiated with primary X-rays 3, the generated secondary X-rays 5 are separated by a spectroscopic element 6, and the wavelength of the secondary X-rays 7 to be split is linked to the interlocking means 1.
Detector 8 applying a predetermined voltage V while changing at 0
To generate pulses of a voltage corresponding to the predetermined applied voltage V and the energy E of the secondary X-rays 7 in a number corresponding to the intensity of the secondary X-rays 7. Then, the voltage of the generated pulse is amplified by the amplifier 16 at a predetermined amplification rate, and the amplified pulse having a predetermined voltage range is used as the pulse height analyzer 1.
In step 3, the predetermined applied voltage V or the predetermined amplification factor G is adjusted by the interlocking means 10 in order to keep the voltage P H of the pulse sent to the pulse height analyzer constant. The counting rate is obtained by the counting means 14. That is, the method of the first embodiment is a wavelength-dispersive and scanning X-ray fluorescence analysis method.

【0033】さらに、この方法では、検出器8における
入射される2次X線7のエネルギーEと発生するパルス
の電圧との比例関係からのずれを、エネルギーEの関数
f(E)または分光素子6の格子面間隔dと回折角θの
関数f(2d sinθ)としてあらかじめ求めて記憶手段
15に記憶させておき、連動手段10で前記所定の印加
電圧Vまたは所定の増幅率Gを調節する際に、前記関数
f(E)またはf(2d sinθ)を適用して補正する。
Further, in this method, the deviation from the proportionality between the energy E of the incident secondary X-ray 7 in the detector 8 and the voltage of the generated pulse is determined by the function f (E) of the energy E or the spectroscopic element. 6 is obtained in advance as a function f (2d sin θ) of the lattice plane distance d and the diffraction angle θ and stored in the storage means 15, and when the interlocking means 10 adjusts the predetermined applied voltage V or the predetermined amplification factor G Then, the correction is performed by applying the function f (E) or f (2d sin θ).

【0034】第1実施形態の方法によれば、検出器8に
おける入射される2次X線7のエネルギーEと発生する
パルスの電圧との比例関係からのずれを、例えばエネル
ギーEの関数f(E)としてあらかじめ求めておき、増
幅器16の所定の増幅率G等を調節する際に、前式
(6)等にしたがい前記関数f(E)を適用して補正す
るので、検出器8が例えばシンチレーションカウンタで
あって前記比例関係からのずれがある場合に、走査によ
り検出器8に入射する2次X線7の波長が変化しても、
波高分析器13へ送られるパルスの電圧PH は正確に一
定になる。これにより、波高分析器13が選別する前記
所定の電圧の範囲を設定変更せずとも、検出器8から発
生して波高分析器13へ送られるパルスのうち、測定す
べき蛍光X線等の2次X線7の波長に対応した電圧PH
のパルスを正確に選別でき、したがって正確な分析がで
きる。
According to the method of the first embodiment, the deviation from the proportionality between the energy E of the incident secondary X-ray 7 and the voltage of the generated pulse in the detector 8 is determined by, for example, the function f ( E) is obtained in advance, and when the predetermined gain G or the like of the amplifier 16 is adjusted, the function f (E) is corrected by applying the function f (E) according to the above equation (6). If the scintillation counter has a deviation from the proportional relationship, even if the wavelength of the secondary X-ray 7 incident on the detector 8 by scanning changes,
The voltage P H of the pulse sent to the wave height analyzer 13 becomes exactly constant. Thereby, without changing the setting of the predetermined voltage range selected by the pulse height analyzer 13, two of the pulses generated from the detector 8 and sent to the pulse height analyzer 13, such as fluorescent X-rays to be measured, voltage P H corresponding to the wavelength of the next X-ray 7
Can be accurately sorted out, and thus an accurate analysis can be performed.

【0035】次に、本発明の第2実施形態の方法につい
て説明する。まず、この方法に用いる装置について、図
1にしたがって説明する。この装置は、試料台2、X線
源4、分光素子6、検出器8、増幅器16、波高分析器
13および計数手段14を備える点は、第1実施形態の
方法に用いる装置と同様であるが、連動手段20が、検
出器8に入射する2次X線7の波長を変化させるととも
に、波高分析器13へ送られるパルスの電圧の変化に追
従するために、前記所定の電圧の範囲を調節する点が異
なる。すなわち、走査により検出器8に入射する2次X
線7の波長が変化すると、検出器8が発生するパルスの
電圧が変化し、検出器8への印加電圧も増幅器16の増
幅率も調節しなければ、波高分析器13へ送られるパル
スの電圧が変化し、波高分析器13が選別する前記所定
の電圧の範囲を設定変更しなければならないが、これを
連動手段20により自動的に調節し、波高分析器13へ
送られるパルスの電圧の変化に容易に追従する。
Next, a method according to a second embodiment of the present invention will be described. First, an apparatus used in this method will be described with reference to FIG. This device is the same as the device used in the method of the first embodiment in that it has a sample stage 2, an X-ray source 4, a spectroscopic element 6, a detector 8, an amplifier 16, a pulse height analyzer 13, and a counting means 14. However, in order for the interlocking means 20 to change the wavelength of the secondary X-ray 7 incident on the detector 8 and to follow the change in the voltage of the pulse sent to the pulse height analyzer 13, the predetermined voltage range is changed. The point of adjustment is different. That is, the secondary X incident on the detector 8 by scanning
When the wavelength of the line 7 changes, the voltage of the pulse generated by the detector 8 changes. If neither the voltage applied to the detector 8 nor the amplification factor of the amplifier 16 is adjusted, the voltage of the pulse sent to the pulse height analyzer 13 is adjusted. Must be changed and the range of the predetermined voltage selected by the pulse height analyzer 13 must be changed. This is automatically adjusted by the interlocking means 20 to change the voltage of the pulse sent to the pulse height analyzer 13. Follows easily.

【0036】ここで、波高分析器13へ送られるパルス
の電圧の変化に正確に追従するために、この装置は、第
1実施形態の方法に用いる装置と同様の記憶手段15を
備え、連動手段20が、前記所定の電圧の範囲を調節す
る際に、前記関数f(E)またはf(2d sinθ)を適
用して補正する。例えば、前記所定の電圧の範囲の上限
値または下限値PS を、次式(8)のように調節する。
なお、PS0は、2次X線7の波長によらず、例えば、1
次線の波高値を2.0としたとき、上限値に3.0、下
限値に1.0を設定するものであり、k5 は定数であ
る。
Here, in order to accurately follow the change in the voltage of the pulse sent to the pulse height analyzer 13, this apparatus is provided with a storage means 15 similar to the apparatus used in the method of the first embodiment. 20 adjusts by applying the function f (E) or f (2d sin θ) when adjusting the predetermined voltage range. For example, the upper limit or lower limit P S of the predetermined voltage range is adjusted as in the following equation (8).
Note that P S0 is, for example, 1 regardless of the wavelength of the secondary X-ray 7.
When 2.0 the peak value of the next line, 3.0 to the upper limit value, which sets the 1.0 to the lower limit value, k 5 are constants.

【0037】 PS =PS0・k5 /(2d sinθ・f(E)) …(8)P S = P S0 · k 5 / (2d sin θ · f (E)) (8)

【0038】すなわち、この装置を用いる第2実施形態
の方法は、検出器8から発生したパルスの電圧を増幅し
て、所定の電圧の範囲のものを波高分析器13で選別
し、選別されたパルスの計数率を計数手段14で求める
点は、第1実施形態の方法と同様であるが、波高分析器
13へ送られるパルスの電圧PH の変化に追従するため
に、波高分析器13が選別する前記所定の電圧の範囲P
S を調節する点が異なる。それに対応して、検出器8に
おける入射される2次X線7のエネルギーEと発生する
パルスの電圧との比例関係からのずれを、前記エネルギ
ーの関数f(E)または前記分光素子の格子面間隔と回
折角の関数f(2d sinθ)としてあらかじめ求めてお
く点は、第1実施形態の方法と同様であるが、前記所定
の電圧の範囲PS を調節する際に、前記関数f(E)ま
たはf(2d sinθ)を適用して補正する点が異なる。
That is, in the method according to the second embodiment using this device, the voltage of the pulse generated from the detector 8 is amplified, and the voltage within a predetermined voltage range is selected by the wave height analyzer 13 and the selected voltage is selected. The point that the counting rate of the pulse is obtained by the counting means 14 is the same as that of the method of the first embodiment, but in order to follow the change in the voltage P H of the pulse sent to the pulse height analyzer 13, the pulse height analyzer 13 The predetermined voltage range P to be selected
The difference is that S is adjusted. Correspondingly, the deviation from the proportionality between the energy E of the incident secondary X-ray 7 in the detector 8 and the voltage of the generated pulse is determined by the function f (E) of the energy or the lattice plane of the spectral element. the points determined in advance as the interval as a function of diffraction angle f (2d sin [theta), is similar to the method of the first embodiment, when adjusting the range P S of the predetermined voltage, the function f (E )) Or f (2d sin θ).

【0039】第2実施形態の方法によれば、検出器8に
おける入射される2次X線7のエネルギーEと発生する
パルスの電圧との比例関係からのずれを、例えばエネル
ギーEの関数f(E)としてあらかじめ求めておき、波
高分析器13が選別する所定の電圧の範囲PS を調節す
る際に、前式(8)にしたがい前記関数f(E)を適用
して補正するので、検出器8が例えばシンチレーション
カウンタであって前記比例関係からのずれがある場合
に、走査により検出器8に入射する2次X線7の波長が
変化し、波高分析器13へ送られるパルスの電圧PH
変化しても、波高分析器13が選別する所定の電圧の範
囲PS は正確に追従する。これにより、検出器8から発
生して波高分析器13へ送られるパルスのうち、測定す
べき蛍光X線等の2次X線7の波長に対応した電圧PH
のパルスを正確に選別でき、したがって正確な分析がで
きる。
According to the method of the second embodiment, the deviation from the proportionality between the energy E of the incident secondary X-rays 7 in the detector 8 and the voltage of the generated pulse is determined by, for example, the function f ( E) obtained in advance as, when the pulse height analyzer 13 to adjust the range P S of a predetermined voltage to screen, is corrected by applying the function f (E) in accordance with equation (8), detecting When the detector 8 is, for example, a scintillation counter and there is a deviation from the proportional relationship, the wavelength of the secondary X-ray 7 incident on the detector 8 changes by scanning, and the voltage P of the pulse sent to the pulse height analyzer 13 is changed. Even if H changes, the predetermined voltage range P S selected by the pulse height analyzer 13 accurately follows. Thus, of the pulses generated from the detector 8 and sent to the pulse height analyzer 13, the voltage P H corresponding to the wavelength of the secondary X-ray 7 such as the fluorescent X-ray to be measured.
Can be accurately sorted out, and thus an accurate analysis can be performed.

【0040】[0040]

【発明の効果】以上詳細に説明したように、本発明によ
れば、波長分散型であって走査型の蛍光X線分析方法お
よび装置において、検出器から発生して波高分析器へ送
られるパルスのうち、測定すべき蛍光X線の波長に対応
した電圧のパルスを正確に選別でき、したがって正確な
分析ができる。
As described above in detail, according to the present invention, in a wavelength-dispersive and scanning X-ray fluorescence analysis method and apparatus, a pulse generated from a detector and sent to a pulse height analyzer is provided. Among them, the pulse of the voltage corresponding to the wavelength of the fluorescent X-ray to be measured can be accurately selected, and thus the accurate analysis can be performed.

【図面の簡単な説明】[Brief description of the drawings]

【図1】本発明の第1、第2実施形態の方法に用いる波
長分散型蛍光X線分析装置を示す概略図である。
FIG. 1 is a schematic diagram showing a wavelength-dispersive X-ray fluorescence spectrometer used in the methods of the first and second embodiments of the present invention.

【符号の説明】[Explanation of symbols]

1…試料、3…1次X線、4…X線源、5…試料から発
生した2次X線、6…分光素子、7…分光素子で分光さ
れた2次X線、8…検出器、10,20…連動手段、1
3…波高分析器、14…計数手段、15…記憶手段、1
6…増幅器。
Reference Signs List 1 ... sample, 3 ... primary X-ray, 4 ... X-ray source, 5 ... secondary X-ray generated from sample, 6 ... spectroscopic element, 7 ... secondary X-ray separated by spectroscopic element, 8 ... detector , 10, 20 ... interlocking means, 1
3 ... height analyzer, 14 ... counting means, 15 ... storage means, 1
6 ... Amplifier.

フロントページの続き (72)発明者 山本 悦久 大阪府高槻市赤大路町14番8号 理学電機 工業株式会社内 Fターム(参考) 2G001 AA01 BA04 CA01 DA01 EA01 EA03 EA08 FA03 FA06 FA24 GA09 JA06 Continued on the front page (72) Inventor Etsuhisa Yamamoto 14-8 Akaoji-cho, Takatsuki-shi, Osaka F-term (reference) 2G001 AA01 BA04 CA01 DA01 EA01 EA03 EA08 FA03 FA06 FA24 GA09 JA06

Claims (4)

【特許請求の範囲】[Claims] 【請求項1】 試料に1次X線を照射し、 発生した2次X線を分光素子で分光し、 分光される2次X線の波長を変化させながら、所定の電
圧を印加した検出器に入射させて、前記所定の印加電圧
と2次X線のエネルギーに応じた電圧のパルスを2次X
線の強度に応じた数だけ発生させ、 発生したパルスの電圧を増幅器により所定の増幅率で増
幅し、 増幅されたパルスのうち所定の電圧の範囲のものを波高
分析器で選別するとともに、 前記波高分析器へ送られるパルスの電圧を一定にするた
めに、前記所定の印加電圧または所定の増幅率を調節
し、 前記選別されたパルスの計数率を計数手段で求める波長
分散型蛍光X線分析方法において、 前記検出器における入射される2次X線のエネルギーと
発生するパルスの電圧との比例関係からのずれを、前記
エネルギーの関数または前記分光素子の格子面間隔と回
折角の関数としてあらかじめ求めておき、 前記所定の印加電圧または所定の増幅率を調節する際
に、前記関数を適用して補正することを特徴とする波長
分散型蛍光X線分析方法。
1. A detector which irradiates a sample with primary X-rays, splits the generated secondary X-rays with a spectroscopic element, and applies a predetermined voltage while changing the wavelength of the secondary X-rays to be split. And a pulse of a voltage corresponding to the predetermined applied voltage and the energy of the secondary X-ray is applied to the secondary X-ray.
The voltage of the generated pulse is amplified at a predetermined amplification rate by an amplifier, and the amplified pulse within a predetermined voltage range is selected by a pulse height analyzer, and In order to make the voltage of the pulse sent to the pulse height analyzer constant, the predetermined applied voltage or the predetermined amplification rate is adjusted, and the counting rate of the selected pulse is obtained by the counting means. In the method, a deviation from the proportionality between the energy of the incident secondary X-rays and the voltage of the generated pulse in the detector is previously determined as a function of the energy or a function of the lattice spacing and diffraction angle of the spectral element. A wavelength-dispersive X-ray fluorescence analysis method, wherein the function is applied and corrected when adjusting the predetermined applied voltage or the predetermined amplification factor.
【請求項2】 試料に1次X線を照射し、 発生した2次X線を分光素子で分光し、 分光される2次X線の波長を変化させながら、所定の電
圧を印加した検出器に入射させて、前記所定の印加電圧
と2次X線のエネルギーに応じた電圧のパルスを2次X
線の強度に応じた数だけ発生させ、 発生したパルスの電圧を増幅器により所定の増幅率で増
幅し、 増幅されたパルスのうち所定の電圧の範囲のものを波高
分析器で選別するとともに、 前記波高分析器へ送られるパルスの電圧の変化に追従す
るために、前記所定の電圧の範囲を調節し、 前記選別されたパルスの計数率を計数手段で求める波長
分散型蛍光X線分析方法において、 前記検出器における入射される2次X線のエネルギーと
発生するパルスの電圧との比例関係からのずれを、前記
エネルギーの関数または前記分光素子の格子面間隔と回
折角の関数としてあらかじめ求めておき、 前記所定の電圧の範囲を調節する際に、前記関数を適用
して補正することを特徴とする波長分散型蛍光X線分析
方法。
2. A detector which irradiates a sample with primary X-rays, splits the generated secondary X-rays with a spectroscopic element, and applies a predetermined voltage while changing the wavelength of the secondary X-rays to be split. And a pulse of a voltage corresponding to the predetermined applied voltage and the energy of the secondary X-ray is applied to the secondary X-ray.
The voltage of the generated pulse is amplified at a predetermined amplification rate by an amplifier, and the amplified pulse within a predetermined voltage range is selected by a pulse height analyzer, and In order to follow the change in the voltage of the pulse sent to the pulse height analyzer, in the wavelength dispersion type fluorescent X-ray analysis method of adjusting the predetermined voltage range, the counting rate of the selected pulse is obtained by the counting means, A deviation from the proportional relationship between the energy of the incident secondary X-rays and the voltage of the generated pulse in the detector is determined in advance as a function of the energy or a function of the lattice spacing and diffraction angle of the spectral element. A wavelength dispersive X-ray fluorescence analysis method, wherein the function is applied and corrected when the predetermined voltage range is adjusted.
【請求項3】 試料に1次X線を照射するX線源と、 試料から発生した2次X線を分光する分光素子と、 所定の電圧が印加され、前記分光素子で分光された2次
X線が入射されて、前記所定の印加電圧と2次X線のエ
ネルギーに応じた電圧のパルスを2次X線の強度に応じ
た数だけ発生させる検出器と、 その検出器で発生したパルスの電圧を所定の増幅率で増
幅する増幅器と、 その増幅器で増幅されたパルスのうち所定の電圧の範囲
のものを選別する波高分析器と、 その波高分析器で選別されたパルスの計数率を求める計
数手段と、 前記検出器に入射する2次X線の波長を変化させるとと
もに、前記波高分析器へ送られるパルスの電圧を一定に
するために、前記所定の印加電圧または所定の増幅率を
調節する連動手段とを備えた波長分散型蛍光X線分析装
置において、 前記検出器における入射される2次X線のエネルギーと
発生するパルスの電圧との比例関係からのずれを、あら
かじめ求められた前記エネルギーの関数または前記分光
素子の格子面間隔と回折角の関数として記憶する記憶手
段を備え、 前記連動手段が、前記所定の印加電圧または所定の増幅
率を調節する際に、前記記憶手段に記憶した関数を適用
して補正することを特徴とする波長分散型蛍光X線分析
装置。
3. An X-ray source for irradiating a sample with primary X-rays, a spectroscopic element for dispersing secondary X-rays generated from the sample, and a secondary voltage separated by the spectroscopic element when a predetermined voltage is applied. A detector that receives X-rays and generates pulses of a voltage corresponding to the predetermined applied voltage and the energy of the secondary X-ray by a number corresponding to the intensity of the secondary X-ray; and a pulse generated by the detector. An amplifier that amplifies the voltage at a predetermined amplification rate, a pulse height analyzer that selects pulses within a predetermined voltage range among the pulses amplified by the amplifier, and a counting rate of the pulses selected by the pulse height analyzer Counting means for determining, while changing the wavelength of the secondary X-rays incident on the detector, and keeping the voltage of the pulse sent to the pulse height analyzer constant, the predetermined applied voltage or the predetermined amplification factor Wavelength dispersion type with interlocking means for adjusting In the X-ray fluorescence spectrometer, the deviation from the proportionality between the energy of the incident secondary X-rays and the voltage of the generated pulse in the detector is determined by a function of the energy determined in advance or the lattice plane of the spectroscopic element. Storage means for storing as a function of an interval and a diffraction angle, wherein the interlocking means adjusts by applying the function stored in the storage means when adjusting the predetermined applied voltage or the predetermined amplification factor. Characteristic wavelength-dispersive X-ray fluorescence spectrometer.
【請求項4】 試料に1次X線を照射するX線源と、 試料から発生した2次X線を分光する分光素子と、 所定の電圧が印加され、前記分光素子で分光された2次
X線が入射されて、前記所定の印加電圧と2次X線のエ
ネルギーに応じた電圧のパルスを2次X線の強度に応じ
た数だけ発生させる検出器と、 その検出器で発生したパルスの電圧を所定の増幅率で増
幅する増幅器と、 その増幅器で増幅されたパルスのうち所定の電圧の範囲
のものを選別する波高分析器と、 その波高分析器で選別されたパルスの計数率を求める計
数手段と、 前記検出器に入射する2次X線の波長を変化させるとと
もに、前記波高分析器へ送られるパルスの電圧の変化に
追従するために、前記所定の電圧の範囲を調節する連動
手段とを備えた波長分散型蛍光X線分析装置において、 前記検出器における入射される2次X線のエネルギーと
発生するパルスの電圧との比例関係からのずれを、あら
かじめ求められた前記エネルギーの関数または前記分光
素子の格子面間隔と回折角の関数として記憶する記憶手
段を備え、 前記連動手段が、前記所定の電圧の範囲を調節する際
に、前記記憶手段に記憶した関数を適用して補正するこ
とを特徴とする波長分散型蛍光X線分析装置。
4. An X-ray source for irradiating a sample with primary X-rays, a spectroscopic element for dispersing secondary X-rays generated from the sample, a secondary voltage applied with a predetermined voltage, and separated by the spectroscopic element A detector that receives X-rays and generates pulses of a voltage corresponding to the predetermined applied voltage and the energy of the secondary X-ray by a number corresponding to the intensity of the secondary X-ray; and a pulse generated by the detector. An amplifier that amplifies the voltage at a predetermined amplification rate, a pulse height analyzer that selects pulses within a predetermined voltage range among the pulses amplified by the amplifier, and a counting rate of the pulses selected by the pulse height analyzer Counting means for determining, and interlocking, changing the wavelength of the secondary X-rays incident on the detector and adjusting the predetermined voltage range in order to follow the change in the voltage of the pulse sent to the pulse height analyzer Dispersive X-ray fluorescence analysis with means In the apparatus, the deviation from the proportional relationship between the energy of the incident secondary X-rays and the voltage of the generated pulse in the detector is determined by a previously determined function of the energy or the lattice spacing and diffraction angle of the spectral element. A wavelength-dispersive fluorescent light X, wherein the interlocking means corrects by applying the function stored in the memory when adjusting the predetermined voltage range. Line analyzer.
JP2000032878A 2000-02-10 2000-02-10 Wavelength dispersive X-ray fluorescence analysis method and apparatus Expired - Fee Related JP3394936B2 (en)

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