JP5572438B2 - X-ray fluorescence analyzer - Google Patents

X-ray fluorescence analyzer Download PDF

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JP5572438B2
JP5572438B2 JP2010076377A JP2010076377A JP5572438B2 JP 5572438 B2 JP5572438 B2 JP 5572438B2 JP 2010076377 A JP2010076377 A JP 2010076377A JP 2010076377 A JP2010076377 A JP 2010076377A JP 5572438 B2 JP5572438 B2 JP 5572438B2
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恒郎 佐藤
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Hitachi High Tech Science Corp
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Description

本発明は、X線を照射した試料から発生する蛍光X線を解析することで、前記試料の定性・定量分析等を行う蛍光X線分析装置に関する。   The present invention relates to a fluorescent X-ray analyzer that performs qualitative and quantitative analysis of a sample by analyzing fluorescent X-rays generated from the sample irradiated with X-rays.

エネルギー分散型の蛍光X線装置で取得したスペクトルから特定元素から放射された蛍光X線の強度を算出するためには、蛍光X線ピーク波形とバックグラウンド波形を分離する必要がある。   In order to calculate the intensity of fluorescent X-rays emitted from a specific element from a spectrum acquired by an energy dispersive fluorescent X-ray apparatus, it is necessary to separate the fluorescent X-ray peak waveform from the background waveform.

従来は、ピークになっている部分の除去を繰り返すことによってバックグラウンド波形を生成し、蛍光X線ピーク波形とバックグラウンド波形の分離を行っていた(特許文献1参照)。   Conventionally, a background waveform is generated by repeating removal of a peaked portion, and a fluorescent X-ray peak waveform and a background waveform are separated (see Patent Document 1).

特開平7−146258号公報Japanese Patent Laid-Open No. 7-146258

しかしながら、従来のピーク部分の除去を繰り返す方法では、蛍光X線ピーク波形がバックグランド波形の急激に変化する偏曲点付近に存在するとき、偏曲点の形状が蛍光X線ピーク波形により隠されてしまうため、バックグラウンド波形の正確に生成することが困難であり、バックグラウンドが大きめに生成されてしまうという課題があった。   However, in the conventional method of repeatedly removing the peak portion, when the fluorescent X-ray peak waveform is present near the inflection point where the background waveform changes rapidly, the shape of the inflection point is hidden by the fluorescent X-ray peak waveform. Therefore, it is difficult to accurately generate the background waveform, and there is a problem that the background is generated in a large amount.

この発明は、このような事情を考慮してなされたもので、その目的は、バックグラウンド波形の急激に変化する偏曲点付近に存在するスペクトルであっても、蛍光X線ピーク波形とバックグラウンド波形の適当な分離ができる装置を提供することである。   The present invention has been made in consideration of such circumstances, and the object of the present invention is to determine the fluorescent X-ray peak waveform and the background even if the spectrum exists near the inflection point where the background waveform changes rapidly. It is an object to provide an apparatus capable of appropriately separating waveforms.

上記の目的を達成するために、この発明は以下の手段を提供している。典型的なバックグラウンド波形と強度を求めたい蛍光X線ピーク波形とそのピークの周辺にあり検出された複数の蛍光X線ピーク波形を使い、測定された波形を良く再現するようにバックグラウンド波形と蛍光X線ピーク波形の強度を変化させる。
そして、出来上がったスペクトルから、蛍光X線ピーク波形とバックグラウンド波形を分離する。
In order to achieve the above object, the present invention provides the following means. A typical background waveform and fluorescent X-ray peak waveform whose intensity is to be obtained and a plurality of fluorescent X-ray peak waveforms detected around the peak, and a background waveform to reproduce the measured waveform well. The intensity of the fluorescent X-ray peak waveform is changed.
Then, the fluorescent X-ray peak waveform and the background waveform are separated from the completed spectrum.

本発明に係る蛍光X線分析装置によれば、バックグラウンド波形の急激に変化する偏曲点付近に存在するスペクトルであっても、蛍光X線ピーク波形とバックグラウンド波形の適当な分離を図ることができる。   According to the fluorescent X-ray analyzer according to the present invention, appropriate separation of the fluorescent X-ray peak waveform and the background waveform can be achieved even for a spectrum that exists in the vicinity of the inflection point where the background waveform changes rapidly. Can do.

本発明の実施例を示す装置概略図である。It is an apparatus schematic diagram showing an example of the present invention. 本発明の実施例を示す装置のブロック図である。It is a block diagram of the apparatus which shows the Example of this invention. 本発明の実施例を示すフローチャートである。It is a flowchart which shows the Example of this invention. 本発明の実施例を示すX線スペクトルである。It is an X-ray spectrum which shows the Example of this invention.

以下、本発明に係る蛍光X線分析装置の実施形態について説明する。
図1は本発明の蛍光X線分析装置の概略図で、X線管11からX線12が試料13に照射され、発生した蛍光X線14は検出器15で検出された後、アンプ16で増幅され、データ処理装置1に送られる。ここで、検出器15は蛍光X線14の波長を識別してその強度を電気信号として出力する。
Hereinafter, embodiments of the X-ray fluorescence analyzer according to the present invention will be described.
FIG. 1 is a schematic diagram of an X-ray fluorescence analyzer according to the present invention. An X-ray tube 11 irradiates a sample 13 with an X-ray 12, and the generated fluorescent X-ray 14 is detected by a detector 15 and then amplified by an amplifier 16. Amplified and sent to the data processing device 1. Here, the detector 15 identifies the wavelength of the fluorescent X-ray 14 and outputs its intensity as an electrical signal.

図2はデータ処理装置1のブロック図である。1aはCPUで、種々の演算処理やメモリ1b、ディスプレイ1c、および元素特定手段1dに対して動作指示を行う。1bはメモリで、特定元素毎に予め求めたバックグラウンド関数および積分範囲を記憶する。1cはディスプレイで、対象となる試料について測定した蛍光X線からそのプロファイルデータ等の表示を行う。1dは元素特定手段で、ディスプレイ1cに表示されたプロファイルデータ等に基づいて定量分析すべき元素を特定し、その旨CPU1aに対して指示を与える。   FIG. 2 is a block diagram of the data processing apparatus 1. Reference numeral 1a denotes a CPU which instructs various arithmetic processes and operations to the memory 1b, the display 1c, and the element specifying means 1d. A memory 1b stores a background function and an integration range obtained in advance for each specific element. Reference numeral 1c denotes a display that displays profile data and the like from fluorescent X-rays measured for a target sample. 1d is an element specifying means that specifies an element to be quantitatively analyzed based on profile data displayed on the display 1c and gives an instruction to that effect to the CPU 1a.

図3は本発明による各元素の蛍光X線強度を求める手順を示すフローチャートである。まず、バックグラウンドの偏曲点に蛍光X線のピークがない基準試料を測定し、その偏曲点付近のバックグラウンドのプロファイルを得る(S101)。次に、定量を行う試料の測定を行い(S102)、定量分析を行う元素を特定する(S103)。定量元素の関数波形と対象試料の定性分析S102で得たバックグラウンド波形を用いて、蛍光X線ピーク波形とバックグラウンド波形を分離処理する(S104)。波形分離処理S104の結果から各元素の蛍光X線強度を求める。   FIG. 3 is a flowchart showing a procedure for obtaining the fluorescent X-ray intensity of each element according to the present invention. First, a reference sample having no fluorescent X-ray peak at the background inflection point is measured, and a background profile near the inflection point is obtained (S101). Next, a sample to be quantified is measured (S102), and an element for quantitative analysis is specified (S103). The fluorescent X-ray peak waveform and the background waveform are separated using the function waveform of the quantitative element and the background waveform obtained in the qualitative analysis S102 of the target sample (S104). The fluorescent X-ray intensity of each element is obtained from the result of the waveform separation process S104.

図4(a)は従来法によるバックグラウンドの見積りである。本来のバックグラウンド波形B1の偏曲点P1に蛍光X線ピーク波形が重なっている波形S1の場合、従来のピーク除去部分の除去を繰り返し、バックグラウンド波形を生成する方法では、バックグラウンド波形B2のように、バックグラウンド波形が本来のバックグラウンド波形B1よりも大きめに生成される。そこで、図4(b)に示すように、バックグラウンド波形の偏曲点付近に蛍光X線ピーク波形の存在しない基準試料で波形S2を取得する。基準試料としては、例えば、ポリエチレンを用いることができる。   FIG. 4A shows an estimation of the background according to the conventional method. In the case of the waveform S1 in which the fluorescent X-ray peak waveform is overlapped with the inflection point P1 of the original background waveform B1, the conventional method of repeatedly removing the peak removal and generating the background waveform, As described above, the background waveform is generated larger than the original background waveform B1. Therefore, as shown in FIG. 4B, the waveform S2 is acquired with a reference sample in which no fluorescent X-ray peak waveform exists near the inflection point of the background waveform. As the reference sample, for example, polyethylene can be used.

波形S1を良く再現するように定量したい試料に含まれる蛍光X線ピークの関数波形と波形S2の強度を変化させる。そして、出来上がった波形から、蛍光X線ピーク波形F1とバックグラウンド波形F2を分離する。これにより蛍光X線ピーク波形とバックグラウンド波形を適当に分離することができる。   The function waveform of the fluorescent X-ray peak contained in the sample to be quantified and the intensity of the waveform S2 are changed so as to reproduce the waveform S1 well. Then, the fluorescent X-ray peak waveform F1 and the background waveform F2 are separated from the completed waveform. Thereby, the fluorescent X-ray peak waveform and the background waveform can be appropriately separated.

1…データ処理装置
11…X線管
12…X線
13…試料
14…蛍光X線
15…検出器
16…アンプ
DESCRIPTION OF SYMBOLS 1 ... Data processor 11 ... X-ray tube 12 ... X-ray 13 ... Sample 14 ... Fluorescent X-ray 15 ... Detector 16 ... Amplifier

Claims (1)

試料にX線を照射するX線管と、
前記試料から発生した蛍光X線を検出する検出器と、
前記検出器で検出した検出信号を処理するデータ処理装置と、を有する蛍光X線分析装置において、
前記データ処理装置は、
所定の領域のバックグラウンドの偏曲点に蛍光X線のピークを有さない基準試料で測定した蛍光X線のプロファイルから求めたバックグラウンド波形と積分範囲のデータと定量分析対象の元素のピーク波形関数を記憶する記憶手段と、
前記元素を特定する元素特定手段と、
特定された前記元素に対応する前記バックグラウンド波形と前記積分範囲のデータと前記元素のピーク波形関数に基づくピーク波形を前記記憶手段から読みだし、前記バックグラウンド波形と前記ピーク波形を用いて前記試料の前記バックグラウンド波形と対応する領域のプロファイルを再現するように前記バックグラウンド波形と前記ピーク波形を変化させ、前記試料のバックグラウンド波形とピーク波形を分離し、分離したピーク波形の前記積分範囲での積分値を算出する演算手段と、を有する蛍光X線分析装置。
An X-ray tube for irradiating the sample with X-rays;
A detector for detecting fluorescent X-rays generated from the sample;
In a fluorescent X-ray analyzer having a data processing device for processing a detection signal detected by the detector,
The data processing device includes:
And background waveform and an integral range of data obtained from the profile of the fluorescent X-rays measured by the reference sample with no peaks of the fluorescent X-ray to the inflection point of the background of a given region, the peak of the element quantitative analysis target Storage means for storing a waveform function;
Element identification means for identifying the element;
Reading the background waveform peak waveform based on the peak waveform function of the data and the element of the integration range corresponding to the specified the elements from the storage unit, the sample using the peak waveform and the background waveform said back the ground wave and the corresponding to the background waveform to reproduce the profile of the region to change the peak waveform, separating the background waveform and the peak waveform of the sample, the integration range of the separated peak waveform of And a calculation means for calculating an integral value at x.
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