JP2010066085A - Cell of fluorescent x-ray analyzer and fluorescent x-ray analyzer - Google Patents

Cell of fluorescent x-ray analyzer and fluorescent x-ray analyzer Download PDF

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JP2010066085A
JP2010066085A JP2008231754A JP2008231754A JP2010066085A JP 2010066085 A JP2010066085 A JP 2010066085A JP 2008231754 A JP2008231754 A JP 2008231754A JP 2008231754 A JP2008231754 A JP 2008231754A JP 2010066085 A JP2010066085 A JP 2010066085A
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cell
sample
fluorescent
sample chamber
ray
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Yumeo Sakiide
夢生 崎出
Atsushi Midorikawa
淳 緑川
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Newly Corp
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Newly Corp
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<P>PROBLEM TO BE SOLVED: To provide the cell of a fluorescent X-ray analyzer capable of certainly eliminating wrinkles or slackening (bending) from the region of an elastic film where a sample chamber is formed. <P>SOLUTION: In the cell 1 of the fluorescent X-ray analyzer configured such that the outer peripheral part of the elastic film 11 is locked with a cell body 12 when the elastic film 11 is fixed across the cell body 12 and a film fixture 13, the cell body 12 has an annular support part 121b around a recess 121a in order to support the elastic film 11, of which the outer peripheral part is locked, in a planar state and the film fixture 13 has an annular pressing part 131c in order to press the region, which is inside the support part 121b and outside an opening 132, of the elastic film 11 supported in the planar state. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

本発明は、試料中の所定元素（例えば、軽油中の硫黄）を測定すべく、試料を収容する試料室の一部がＸ線透過性を有する弾性膜で形成される蛍光Ｘ線分析装置のセル、及びそのセルを備える蛍光Ｘ線分析装置に関する。   The present invention relates to a fluorescent X-ray analyzer in which a part of a sample chamber containing a sample is formed of an elastic film having X-ray permeability so as to measure a predetermined element in the sample (for example, sulfur in light oil). The present invention relates to a cell and a fluorescent X-ray analysis apparatus including the cell.

従来、蛍光Ｘ線分析装置のセルとして、Ｘ線透過性を有する弾性膜と、弾性膜に覆われることにより試料を収容するための試料室を形成するセル本体と、弾性膜の外周部をセル本体と挾んで固定する膜固定体とを備えるセルが知られている。そして、例えば、弾性膜がセル本体と膜固定体とに挟まれて固定される際に、弾性膜の外周部がセル本体に係止されるように構成されるセルが提案されている（例えば、特許文献１）。
特開平１０−１９７４６０号公報 Conventionally, as a cell of a fluorescent X-ray analyzer, an elastic membrane having X-ray permeability, a cell body forming a sample chamber for containing a sample by being covered with the elastic membrane, and an outer peripheral portion of the elastic membrane as a cell A cell is known that includes a main body and a membrane fixing body that is fixed by holding. For example, a cell is proposed in which the outer peripheral portion of the elastic membrane is locked to the cell main body when the elastic membrane is sandwiched and fixed between the cell main body and the membrane fixing body (for example, Patent Document 1).
JP-A-10-197460

しかしながら、特許文献１に記載されるセルは、例えば、弾性膜の外周部がセル本体に十分に係止されていない場合には、弾性膜の外周部がセル本体に対して位置ずれを起こすため、弾性膜にしわや弛み（撓み）を発生させることがある。さらに、しわや弛み（撓み）のある弾性膜で形成された試料室に収容された試料に対して、弾性膜を介してＸ線を照射して、試料から発生する蛍光Ｘ線を検出しても、測定データにばらつきが生じるため、正確な測定データを取得することができない。   However, in the cell described in Patent Document 1, for example, when the outer peripheral portion of the elastic membrane is not sufficiently locked to the cell main body, the outer peripheral portion of the elastic membrane causes a positional shift with respect to the cell main body. In some cases, wrinkles or slack (deflection) may occur in the elastic membrane. Furthermore, X-rays are irradiated through the elastic film to a sample housed in a sample chamber formed of an elastic film having wrinkles or slack (deflection), and fluorescent X-rays generated from the sample are detected. However, since measurement data varies, accurate measurement data cannot be acquired.

よって、本発明は、かかる事情に鑑み、弾性膜の試料室を形成する部位に、しわや弛み（撓み）を確実に無くすことができる蛍光Ｘ線分析装置のセルを提供することを課題とする。また、本発明は、正確な測定データを取得することができる蛍光Ｘ線分析装置を提供することを課題とする。   Therefore, in view of such circumstances, it is an object of the present invention to provide a cell of an X-ray fluorescence analyzer that can surely eliminate wrinkles and slack (deflection) at a site where the sample chamber of the elastic membrane is formed. . Another object of the present invention is to provide an X-ray fluorescence analyzer that can acquire accurate measurement data.

本発明に係る蛍光Ｘ線分析装置のセルは、Ｘ線透過性を有する弾性膜と、弾性膜に覆われることにより試料を収容するための試料室となる凹部を有するセル本体と、弾性膜をセル本体との間に介在させて固定すると共に、弾性膜を介して試料室内の試料にＸ線を照射させるための開口部を有する膜固定体とを備え、弾性膜がセル本体と膜固定体との間に固定される際に、弾性膜の外周部がセル本体に係止されるように構成される蛍光Ｘ線分析装置のセルにおいて、セル本体は、外周部が係止された弾性膜を平面状にして支持すべく、凹部の周りに環状の支持部を備え、膜固定体は、平面状にして支持された弾性膜における支持部よりも内方且つ開口部よりも外方の部位を押圧すべく、環状の押圧部を備えることを特徴とする。   The cell of the fluorescent X-ray analyzer according to the present invention comprises an elastic film having X-ray permeability, a cell main body having a recess serving as a sample chamber for receiving a sample by being covered with the elastic film, and an elastic film. And a membrane fixing body having an opening for irradiating the sample in the sample chamber with X-rays through the elastic membrane, the elastic membrane being provided between the cell main body and the membrane fixing body. In the cell of the fluorescent X-ray analyzer configured so that the outer peripheral portion of the elastic film is locked to the cell body when being fixed between the two, the cell main body is an elastic film whose outer peripheral portion is locked In order to support the substrate in a flat shape, an annular support portion is provided around the recess, and the membrane fixing body is located on the inner side of the support portion and on the outer side of the opening portion of the elastic membrane supported in a flat shape. In order to press, an annular pressing portion is provided.

本発明によれば、セル本体が凹部の周りに環状の支持部を備えるため、支持部が弾性膜を平面状にして支持する。そして、膜固定体が環状の押圧部を備えるため、押圧部が、平面状にして支持された弾性膜における支持部よりも内方且つ開口部よりも外方の部位を押圧する。したがって、弾性膜における試料室を形成する部位に張力を加えることができる。   According to the present invention, since the cell body includes the annular support portion around the recess, the support portion supports the elastic film in a planar shape. And since a film | membrane fixed body is provided with the cyclic | annular press part, a press part presses a site | part inside from the support part in an elastic membrane supported in flat form, and an outer side rather than an opening part. Therefore, tension can be applied to the portion of the elastic membrane that forms the sample chamber.

また、本発明に係る蛍光Ｘ線分析装置のセルにおいては、支持部は、押圧部を内嵌するように構成され、弾性膜は、支持部の内周部と押圧部の外周部とに挟まれて固定されてもよい。   Further, in the cell of the fluorescent X-ray analyzer according to the present invention, the support portion is configured to fit the pressing portion, and the elastic film is sandwiched between the inner peripheral portion of the support portion and the outer peripheral portion of the pressing portion. It may be fixed.

かかる構成によれば、支持部が押圧部を内嵌するように構成されるため、支持部と押圧部との位置関係、即ち、位置決めを正確に行うことができる。また、弾性膜が支持部の内周部と押圧部の外周部とに挟まれて固定されるため、弾性膜をより確実に固定することができる。   According to such a configuration, since the support portion is configured to fit the pressing portion, the positional relationship between the support portion and the pressing portion, that is, positioning can be accurately performed. Moreover, since the elastic membrane is sandwiched and fixed between the inner peripheral portion of the support portion and the outer peripheral portion of the pressing portion, the elastic membrane can be more reliably fixed.

また、本発明に係る蛍光Ｘ線分析装置は、上記のセルと、試料室内の試料にＸ線を照射するＸ線源と、試料から発生する蛍光Ｘ線を検出する検出部とを備えることを特徴とする。   In addition, an X-ray fluorescence analyzer according to the present invention includes the above cell, an X-ray source that irradiates the sample in the sample chamber with X-rays, and a detection unit that detects the X-ray fluorescence generated from the sample. Features.

かかる構成によれば、平面状に維持された弾性膜を介して、Ｘ線源が試料室内の試料にＸ線を照射する。そして、検出部が試料から発生する蛍光Ｘ線を検出する。   According to this configuration, the X-ray source irradiates the sample in the sample chamber with X-rays through the elastic film maintained in a flat shape. The detection unit detects fluorescent X-rays generated from the sample.

また、本発明に係る蛍光Ｘ線分析装置は、内部に収容する試料を先端部から注出する注出手段をさらに備え、セルは、試料を試料室へ導入するための導入部と、試料室を介して導入部と連通し、試料を試料室から導出するための導出部とを備え、導入部は、注出手段の先端部と嵌合する入口部を備えてもよい。   The fluorescent X-ray analysis apparatus according to the present invention further includes a pouring means for pouring the sample accommodated in the inside from the tip portion, and the cell includes an introducing portion for introducing the sample into the sample chamber, a sample chamber, And a lead-out part communicating with the lead-in part through which the sample is led out from the sample chamber, and the lead-in part may be provided with an inlet part fitted to the tip part of the extraction means.

かかる構成によれば、注出手段が内部に収容する試料を先端部から外部へ注出することにより、導入部により、試料を試料室内に導入すると共に、導入部と試料室を介して連通している導出部により、試料室に収容されていた（測定済みの）試料や洗浄液を試料室外へ導出することができる。そして、導入部の入口部が注出手段の先端部と嵌合しているため、入口部から外気を侵入させることなく試料を試料室内に導入することができる。   According to such a configuration, the sample contained in the extraction means is extracted from the tip portion to the outside, whereby the sample is introduced into the sample chamber by the introduction portion and communicated via the introduction portion and the sample chamber. Thus, the (measured) sample or cleaning liquid stored in the sample chamber can be led out of the sample chamber. And since the inlet part of the introducing | transducing part is fitted with the front-end | tip part of the extraction | pouring means, a sample can be introduce | transduced into a sample chamber, without making external air penetrate | invade from an inlet part.

以上の如く、本発明に係る蛍光Ｘ線分析装置のセルによれば、弾性膜における試料室を形成する部位に張力を加えることができるため、弾性膜における試料室を形成する部位に、しわや弛み（撓み）を確実に無くすことができるという優れた効果を奏する。   As described above, according to the cell of the fluorescent X-ray analysis apparatus according to the present invention, tension can be applied to the portion of the elastic membrane where the sample chamber is formed. There is an excellent effect that slack (deflection) can be surely eliminated.

また、本発明に係る蛍光Ｘ線分析装置によれば、平面状に維持された弾性膜を介して、Ｘ線源が試料室内の試料にＸ線を照射し、そして、検出部が試料から発生する蛍光Ｘ線を検出するため、正確な測定データを取得することができるという優れた効果を奏する。   Further, according to the X-ray fluorescence analyzer according to the present invention, the X-ray source irradiates the sample in the sample chamber via the elastic film maintained in a flat shape, and the detection unit is generated from the sample. In order to detect the fluorescent X-rays to be performed, there is an excellent effect that accurate measurement data can be acquired.

以下、本発明に係る蛍光Ｘ線分析装置のセル及び蛍光Ｘ線分析装置における一実施形態について、図１〜図７を参酌して説明する。   Hereinafter, an embodiment of a cell of an X-ray fluorescence analyzer and an X-ray fluorescence analyzer according to the present invention will be described with reference to FIGS.

本実施形態に係る蛍光Ｘ線分析装置は、図１〜図３に示すように、Ｘ線透過性の部位を有する試料室１ａに液体（液状）の試料（例えば軽油）を収容するセル１と、試料室１ａ内の試料にＸ線を照射するＸ線源２と、試料から発生する蛍光Ｘ線を検出する検出部３と、セル１及びＸ線源２並びに検出部３を保持する保持部４とを備える。   As shown in FIGS. 1 to 3, the X-ray fluorescence analyzer according to the present embodiment includes a cell 1 that contains a liquid (liquid) sample (for example, light oil) in a sample chamber 1 a having an X-ray transmissive portion. The X-ray source 2 that irradiates the sample in the sample chamber 1a with X-rays, the detection unit 3 that detects fluorescent X-rays generated from the sample, and the holding unit that holds the cell 1, the X-ray source 2, and the detection unit 3 4.

また、蛍光Ｘ線分析装置は、セル１に試料や洗浄液を供給すべく、内部に収容する試料を先端部から注出する注出手段５と、セル１から排出される試料や洗浄液を受けるための排液受手段６とを備える。なお、本実施形態においては、注出手段５を、注射器とし、また、排液受手段６を、ホース６１及びボトル６２としている。   The fluorescent X-ray analyzer receives the sample and the cleaning liquid discharged from the cell 1 and the discharging means 5 for discharging the sample accommodated in the cell 1 from the tip in order to supply the sample and the cleaning liquid to the cell 1. The drainage receiving means 6 is provided. In the present embodiment, the dispensing means 5 is a syringe, and the drainage receiving means 6 is a hose 61 and a bottle 62.

そして、蛍光Ｘ線分析装置は、検出部３で検出した蛍光Ｘ線から所定元素（例えば軽油中の硫黄）を分析（演算、測定）するように構成され、その分析結果を出力する出力手段７を備える。なお、本実施形態においては、出力手段７を、分析結果が印刷され、紙片排出口７１から排出される紙片（図示していない）としている。   The fluorescent X-ray analyzer is configured to analyze (calculate and measure) a predetermined element (for example, sulfur in light oil) from the fluorescent X-ray detected by the detection unit 3, and output means 7 for outputting the analysis result. Is provided. In the present embodiment, the output means 7 is a paper piece (not shown) on which the analysis result is printed and discharged from the paper piece discharge port 71.

さらに、蛍光Ｘ線分析装置は、分析者が各種コマンドや各種データを入力するために操作し、また、その操作内容等が表示される操作パネル８を備える。加えて、蛍光Ｘ線分析装置は、セル１、Ｘ線源２、検出部３、保持部４、注出手段５、排液受手段６、出力手段７、及び操作パネル８を収容する筐体９を備える。   Further, the X-ray fluorescence analyzer is provided with an operation panel 8 that is operated by an analyst to input various commands and various data, and the operation content and the like are displayed. In addition, the X-ray fluorescence analyzer includes a cell 1, an X-ray source 2, a detection unit 3, a holding unit 4, a dispensing unit 5, a drainage receiving unit 6, an output unit 7, and an operation panel 8. 9 is provided.

なお、図示していないが、蛍光Ｘ線分析装置は、試料を加温するための加熱手段（ヒータ）と、分析データを補正するための各種センサ（温度センサや気圧センサ）と、Ｘ線が外部に漏出するのを防止するためのＸ線遮蔽カバーと、Ｘ線遮蔽カバーが装着された状態にてＸ線を照射させるためのインターロック機構とを備える。   Although not shown, the X-ray fluorescence analyzer has a heating means (heater) for heating the sample, various sensors (temperature sensor and pressure sensor) for correcting analysis data, and X-rays. An X-ray shielding cover for preventing leakage to the outside and an interlock mechanism for irradiating X-rays with the X-ray shielding cover attached.

セル１は、図４〜図７に示すように、Ｘ線透過性を有する弾性膜１１と、弾性膜１１に覆われることにより試料を収容するための試料室１ａとなる凹部１２１ａを有するセル本体１２と、弾性膜１１をセル本体１２との間に介在させて固定する膜固定体１３とを備える。また、セル１は、試料室１ａから試料が漏出するのを防止する弾性のシール部材１４と、セル本体１２と膜固定体１３とを固定するための固定手段１５とを備える。   As shown in FIGS. 4 to 7, the cell 1 has a cell main body having an elastic film 11 having X-ray permeability and a recess 121 a that becomes a sample chamber 1 a for receiving a sample by being covered with the elastic film 11. 12 and a membrane fixing body 13 for fixing the elastic membrane 11 between the cell body 12 and the elastic membrane 11. The cell 1 also includes an elastic seal member 14 that prevents the sample from leaking out of the sample chamber 1a, and a fixing means 15 for fixing the cell body 12 and the membrane fixing body 13.

弾性膜１１は、Ｘ線を透過する樹脂で、薄膜状に形成される。具体的には、弾性膜１１は、ポリイミドで形成され、円形状のシート状に形成されている。また、弾性膜１１は、外周部をセル本体１２と膜固定体１３とに挾まれて固定される。そして、弾性膜１１は、セル本体１２の凹部１２１ａとにより、試料室１ａを形成する。なお、試料室１ａにおいて、弾性膜１１で形成される部位を、一般的に、窓部という（以下、弾性膜における試料室を形成する部位を「弾性膜の窓部」という）。   The elastic film 11 is a resin that transmits X-rays and is formed in a thin film shape. Specifically, the elastic film 11 is made of polyimide and is formed in a circular sheet shape. Further, the elastic membrane 11 is fixed by being sandwiched between the cell main body 12 and the membrane fixing body 13 at the outer peripheral portion. The elastic film 11 forms the sample chamber 1 a with the recess 121 a of the cell body 12. In the sample chamber 1a, a portion formed by the elastic film 11 is generally referred to as a window portion (hereinafter, a portion forming the sample chamber in the elastic film is referred to as an “elastic film window portion”).

セル本体１２は、Ｘ線が装置外部に漏出するのを防止すべく、Ｘ線を透過しない材質（例えばステンレス）で形成される（なお、一部においては、弾性のシール部材１２ａ，１２ｂで形成される）。そして、セル本体１２は、弾性膜１１を介して、膜固定体１３に外嵌される（内嵌する）被嵌合部１２１を備える。また、セル本体１２は、試料を試料室１ａに導入するための導入部１２２と、試料を試料室１ａから導出するための導出部１２３とを備える。   The cell body 12 is formed of a material that does not transmit X-rays (for example, stainless steel) in order to prevent X-rays from leaking out of the apparatus (partly formed by elastic seal members 12a and 12b). ) And the cell main body 12 is provided with the to-be-fitted part 121 fitted to the film | membrane fixed body 13 through the elastic film | membrane 11 (it fits in). The cell body 12 includes an introduction part 122 for introducing a sample into the sample chamber 1a and a lead-out part 123 for leading the sample from the sample chamber 1a.

被嵌合部１２１は、セル本体１２の端部に、円柱状に突出して形成される。そして、被嵌合部１２１は、弾性膜１１がセル本体１２と膜固定体１３との間に固定される際に、膜固定体１３との間に弾性膜１１の外周部が挟まることにより、弾性膜１１の外周部が係止されるように構成される。また、被嵌合部１２１は、外周部が係止された弾性膜１１の窓部よりも大きい部位を平面状にして支持する支持部１２１ｂを備える。   The fitted portion 121 is formed at the end of the cell body 12 so as to protrude in a columnar shape. Then, when the elastic membrane 11 is fixed between the cell body 12 and the membrane fixing body 13, the fitted portion 121 is sandwiched between the outer periphery of the elastic membrane 11 and the membrane fixing body 13. It is comprised so that the outer peripheral part of the elastic film 11 may be latched. Further, the fitted part 121 includes a support part 121b that supports a part larger than the window part of the elastic film 11 with which the outer peripheral part is locked in a planar shape.

凹部１２１ａは、円柱状に形成される被嵌合部１２１の端面部１２１ｃに設けられる。そして、凹部１２１ａは、試料室１ａが円錐台形状の内空間を形成するように構成される。具体的には、凹部１２１ａは、平面状に形成される円形面と、該円形面の外縁に傾斜して連設される環状の側面とを備え、検出部３（図２参照）に向けて開口が拡がるように構成される。   The recessed part 121a is provided in the end surface part 121c of the to-be-fitted part 121 formed in a column shape. And the recessed part 121a is comprised so that the sample chamber 1a may form the internal space of a truncated cone shape. Specifically, the concave portion 121a includes a circular surface formed in a planar shape, and an annular side surface that is inclined and connected to the outer edge of the circular surface, and faces the detection unit 3 (see FIG. 2). The opening is configured to expand.

支持部１２１ｂは、凹部１２１ａの周りに環状に形成されると共に、凸状に形成される。具体的には、支持部１２１ｂは、被嵌合部１２１の端面部１２１ｃに、被嵌合部１２１の凹部１２１ａより大きい、即ち、凹部１２１ａを囲うような環状に形成されると共に、端面部１２１ｃに対向する膜固定体１３の部位（後述する嵌合部１３１の内面部１３１ａ）に向けて突出する凸状に形成される。   The support portion 121b is formed in an annular shape around the concave portion 121a and is formed in a convex shape. Specifically, the support part 121b is formed in the end surface part 121c of the fitted part 121 in a ring shape larger than the recessed part 121a of the fitted part 121, that is, surrounding the recessed part 121a, and the end face part 121c. Is formed in a convex shape projecting toward a portion of the membrane fixing body 13 (an inner surface portion 131a of the fitting portion 131 described later).

より具体的には、支持部１２１ｂは、被嵌合部１２１の端面部１２１ｃの外縁に、環状且つ凸状に形成される。そして、支持部１２１ｂは、セル本体１２（被嵌合部１２１）が弾性膜１１の外周部を係止する際に、弾性膜１１の窓部より大きい部位を平面状にして支持する。   More specifically, the support part 121b is formed in an annular and convex shape on the outer edge of the end surface part 121c of the fitted part 121. And the support part 121b supports the site | part larger than the window part of the elastic film 11 planarly, when the cell main body 12 (fitting part 121) latches the outer peripheral part of the elastic film 11.

導入部１２２は、セル１の外部から試料を入れるべく、注出手段５（図１参照）の先端部と嵌合する入口部１２２ａを備え、入口部１２２ａから試料室１ａに向けて斜め下方に試料を導入するように構成される。そして、導入部１２２は、傾斜して配置される試料室１ａの下端部に接続され、下端部から試料室１ａ内に試料を導入するように構成される。   The introduction part 122 is provided with an inlet part 122a fitted to the tip part of the pouring means 5 (see FIG. 1) so as to put a sample from the outside of the cell 1, and obliquely downward from the inlet part 122a toward the sample chamber 1a. Configured to introduce a sample. And the introduction part 122 is connected to the lower end part of the sample chamber 1a arranged at an inclination, and is configured to introduce the sample into the sample chamber 1a from the lower end part.

導出部１２３は、試料室１ａを介して、導入部１２２と連通して構成される。また、導出部１２３は、セル１の外部に試料を出すべく、排液受手段６のホース６１（図１参照）の端部に接続される出口部１２３ａを備え、試料室１ａから出口部１２３ａに向けて斜め上方に試料を導出するように構成される。そして、導出部１２３は、傾斜して配置される試料１ａの上端部に接続され、上端部から試料室１ａ外へ試料を導出するように構成される。   The derivation unit 123 is configured to communicate with the introduction unit 122 via the sample chamber 1a. The outlet 123 includes an outlet 123a connected to the end of the hose 61 (see FIG. 1) of the drainage receiving means 6 in order to take the sample out of the cell 1, and the outlet 123a from the sample chamber 1a. It is comprised so that a sample may be derived | led-out diagonally upward toward. And the derivation | leading-out part 123 is connected to the upper end part of the sample 1a arrange | positioned in inclination, and is comprised so that a sample may be derived | led-out from the upper end part out of the sample chamber 1a.

膜固定体１３は、Ｘ線が装置外部に漏出するのを防止すべく、Ｘ線を透過しない材質（例えばステンレス）で形成される。そして、膜固定体１３は、弾性膜１１を介して、セル本体１２の被嵌合部１２１を外嵌する嵌合部１３１を備える。また、膜固定体１３は、弾性膜１１を介して試料室１ａ内の試料にＸ線を照射させるための開口部１３２を備える。   The membrane fixing body 13 is formed of a material that does not transmit X-rays (for example, stainless steel) in order to prevent X-rays from leaking out of the apparatus. The membrane fixing body 13 includes a fitting portion 131 that externally fits the fitted portion 121 of the cell body 12 via the elastic membrane 11. Further, the membrane fixing body 13 includes an opening 132 for irradiating the sample in the sample chamber 1 a with X-rays through the elastic membrane 11.

嵌合部１３１は、円筒状に形成され、セル本体１２と膜固定体１３とが弾性膜１１を挟んで固定した際に、内面部１３１ａが被嵌合部１２１の端面部１２１ｃと所定の隙間を有して対向し、内周部１３１ｂが被嵌合部１２１の外周部１２１ｄと所定の隙間を有して対向して配置される。また、膜固定体１３は、セル本体１２との間に弾性膜１１を固定した際に、弾性膜１１の窓部より大きい部位を平面状に押圧する押圧部１３１ｃを備える。   The fitting portion 131 is formed in a cylindrical shape, and when the cell body 12 and the membrane fixing body 13 are fixed with the elastic membrane 11 sandwiched therebetween, the inner surface portion 131a and the end surface portion 121c of the fitted portion 121 have a predetermined gap. The inner peripheral part 131b is arranged to face the outer peripheral part 121d of the fitted part 121 with a predetermined gap. The membrane fixing body 13 includes a pressing portion 131 c that presses a portion of the elastic membrane 11 larger than the window portion in a planar shape when the elastic membrane 11 is fixed to the cell body 12.

押圧部１３１ｃは、嵌合部１３１の内面部１３１ａに、環状に形成されると共に、凸状に形成される。そして、押圧部１３１ｃは、セル本体１２の支持部１２１ｂよりも小さく且つセル本体１２の凹部１２１ａよりも大きく形成され、平面状にして支持された弾性膜１１における支持部１２１ｂよりも内方且つ開口部１３２よりも外方の部位を、セル本体１２（具体的には被嵌合部１２１の端面部１２１ｃ）側に向けて押圧する。   The pressing portion 131c is formed in an annular shape and a convex shape on the inner surface portion 131a of the fitting portion 131. The pressing portion 131c is smaller than the supporting portion 121b of the cell main body 12 and larger than the concave portion 121a of the cell main body 12, and is inwardly opened than the supporting portion 121b in the elastic film 11 supported in a planar shape. A portion outside the portion 132 is pressed toward the cell body 12 (specifically, the end surface portion 121c of the fitted portion 121).

また、押圧部１３１ｃは、支持部１２１ｂに内嵌されると共に、押圧部１３１ｃの外周部は、支持部１２１ｂの内周部とにより、弾性膜１１を挟んで固定する。具体的には、押圧部１３１ｃは、弾性膜１１における試料室を形成する部位、即ち、中央の平面状の部位よりも外方の部位を凹凸状に変形させると共に、当該変形させた部位を支持部１２１ｂとにより挟んで固定する。   The pressing portion 131c is fitted into the support portion 121b, and the outer peripheral portion of the pressing portion 131c is fixed with the elastic film 11 sandwiched between the inner peripheral portion of the support portion 121b. Specifically, the pressing portion 131c deforms the portion of the elastic film 11 that forms the sample chamber, that is, the portion outside the central planar portion into an uneven shape, and supports the deformed portion. It is sandwiched and fixed by the part 121b.

開口部１３２は、弾性膜１１の窓部より大きく形成される。また、開口部１３２は、弾性膜１１の窓部を露出させるべく、円形状に形成されると共に、弾性膜１１側から検出部３側に向けて拡がるようにして形成される。そして、開口部１３２は、セル本体１の凹部１２１ａとにより、弾性膜１１を介して、円錐台形状の内空間を形成する。具体的には、開口部１３２の内周面は、被嵌合部１２１の凹部１２１ａの側面と略面一となるように構成される。   The opening 132 is formed larger than the window of the elastic film 11. Further, the opening 132 is formed in a circular shape so as to expose the window portion of the elastic film 11 and is formed so as to expand from the elastic film 11 side toward the detection unit 3 side. The opening 132 forms a frustoconical inner space through the elastic film 11 by the recess 121 a of the cell body 1. Specifically, the inner peripheral surface of the opening 132 is configured to be substantially flush with the side surface of the recess 121 a of the fitted portion 121.

シール部材１４は、弾性膜１１と、セル本体１２の被嵌合部１２１の端面部１２１ｃとの間に配置され、被嵌合部１２１の端面部１２１ｃと嵌合部１３１の内面部１３１ｂとに押圧される。なお、本実施形態においては、シール部材１４を、Ｏリングとし、被嵌合部１２１の端面部１２１ｃに設けられる環状溝に収容されて位置決めされる。   The seal member 14 is disposed between the elastic film 11 and the end surface portion 121c of the fitted portion 121 of the cell body 12, and is provided between the end surface portion 121c of the fitted portion 121 and the inner surface portion 131b of the fitted portion 131. Pressed. In the present embodiment, the seal member 14 is an O-ring, and is accommodated and positioned in an annular groove provided in the end surface portion 121c of the fitted portion 121.

そして、図１〜図３に戻り、Ｘ線源２は、平面状に形成される弾性膜１１（試料室１ａの窓部）に対して、照射するＸ線の光軸が傾斜するように配置される。そして、Ｘ線源２は、膜固定体１３の開口部１３２内を通過し、弾性膜１１の窓部を介して、試料室１ａ内の試料にＸ線を照射する。なお、本実施形態においては、Ｘ線源２を、Ｘ線管としている。   1 to 3, the X-ray source 2 is arranged so that the optical axis of the X-ray to be irradiated is inclined with respect to the elastic film 11 (window portion of the sample chamber 1a) formed in a flat shape. Is done. The X-ray source 2 passes through the opening 132 of the membrane fixing body 13 and irradiates the sample in the sample chamber 1 a with X-rays through the window of the elastic membrane 11. In the present embodiment, the X-ray source 2 is an X-ray tube.

検出部３は、試料室１ａ内の試料中に含まれる所定元素により、励起される蛍光Ｘ線を検出するように構成される。そして、検出部３は、さまざまな方向に放たれる蛍光Ｘ線を漏れなく、しかも、エネルギーが大きい状態で検出すべく、弾性膜１１の近傍に配置される。なお、本実施形態においては、検出部３を、比例係数管としているが、半導体検出器としてもよい。   The detection unit 3 is configured to detect fluorescent X-rays excited by a predetermined element contained in the sample in the sample chamber 1a. And the detection part 3 is arrange | positioned in the vicinity of the elastic film 11 in order to detect the fluorescent X-rays emitted in various directions without leaking and with a large energy. In the present embodiment, the detection unit 3 is a proportional coefficient tube, but may be a semiconductor detector.

保持部４は、セル１及びＸ線源２並びに検出部３を一体的にさせて保持する。具体的には、保持部４は、セル１及びＸ線源２並びに検出部３の配置が相違することにより、分析誤差が生じるのを防止すべく、セル１及びＸ線源２並びに検出部３を設定された所定位置に配置させる。なお、保持部４は、アルミニウムで形成される。   The holding unit 4 holds the cell 1, the X-ray source 2, and the detection unit 3 integrally. Specifically, the holding unit 4 includes the cell 1, the X-ray source 2, and the detection unit 3 in order to prevent an analysis error due to a difference in the arrangement of the cell 1, the X-ray source 2, and the detection unit 3. Is placed at a predetermined position. The holding part 4 is made of aluminum.

筐体９は、操作パネル７及び出力手段８を有する装置本体９１と、装置本体９１に開閉自在に取り付けられる蓋体９２とを備える。また、筐体９は、分析者が持ち運びするのを容易とすべく、把持部９３を備える。   The housing 9 includes an apparatus main body 91 having an operation panel 7 and output means 8, and a lid 92 attached to the apparatus main body 91 so as to be freely opened and closed. In addition, the housing 9 includes a grip portion 93 so that an analyst can easily carry it.

装置本体９１は、保持部４にて一体化された、セル１及びＸ線源２並びに検出部３を着脱可能に構成される。また、装置本体９１は、セル１から取り外された注出手段５及び排液受手段６を空きスペースに収容可能に構成される。   The apparatus main body 91 is configured so that the cell 1, the X-ray source 2, and the detection unit 3 integrated with the holding unit 4 can be attached and detached. Moreover, the apparatus main body 91 is comprised so that the extraction | pouring means 5 and the drainage receiving means 6 removed from the cell 1 can be accommodated in an empty space.

本実施形態に係る蛍光Ｘ線分析装置及びセル１の構成は以上の通りであり、次に、本実施形態に係るセル１の組み立て方法と、蛍光Ｘ線分析装置の分析方法（作動）とについて説明する。   The configurations of the fluorescent X-ray analyzer and the cell 1 according to the present embodiment are as described above. Next, the assembly method of the cell 1 according to the present embodiment and the analysis method (operation) of the fluorescent X-ray analyzer. explain.

はじめに、セル１の組み立て方法について、図４〜図７を参酌して説明する。図４〜図６に示すように、セル本体１２の被嵌合部１２１の端面部１２１ｃを弾性膜１１で覆った状態にて、セル本体１２の被嵌合部１２１に、膜固定体１３の嵌合部１３１を嵌め込ませる（図４、図５、図６の順）。なお、弾性膜１１で覆うことにより、シール部材１４を、被嵌合部１２１の端面部１２１ｃの環状溝に収容させている。   First, a method for assembling the cell 1 will be described with reference to FIGS. As shown in FIGS. 4 to 6, in the state where the end face part 121 c of the fitted part 121 of the cell main body 12 is covered with the elastic film 11, the membrane fixed body 13 is attached to the fitted part 121 of the cell main body 12. The fitting part 131 is fitted (in order of FIG. 4, FIG. 5, FIG. 6). In addition, the sealing member 14 is accommodated in the annular groove of the end surface part 121 c of the fitted part 121 by covering with the elastic film 11.

このとき、被嵌合部１２１の外周部１２１ｄと嵌合部１３１の内周部１３１ｂとの間に弾性膜１１の外周部が挟まれるため、嵌合部１３１の内周部１３１ｂが弾性膜１１の外周部を被嵌合部１２１の外周部に向けて押圧する。これにより、弾性膜１１の外周部がセル本体１２の嵌合部１２１（具体的には、外周部１２１ｄ）に係止される一方、環状で且つ凸状に形成される支持部１２１ｂにより、弾性膜１１の窓部より大きい部位が平面状に支持されることになる。   At this time, since the outer peripheral part of the elastic film 11 is sandwiched between the outer peripheral part 121d of the fitted part 121 and the inner peripheral part 131b of the fitting part 131, the inner peripheral part 131b of the fitting part 131 is Is pressed toward the outer peripheral portion of the fitted portion 121. Accordingly, the outer peripheral portion of the elastic film 11 is locked to the fitting portion 121 (specifically, the outer peripheral portion 121d) of the cell main body 12, while the support portion 121b formed in an annular and convex shape is elastic. A portion larger than the window portion of the film 11 is supported in a planar shape.

そして、セル本体１２の被嵌合部１２１に膜固定体１３の嵌合部１３１をさらに嵌め込むと、図７に示すように、環状で且つ凸状に形成される押圧部１３１ｃにより、弾性膜１１における支持部１２１ｂで支持される部位よりも内方で且つ開口部１３２（又は窓部）よりも外方の部位が押圧される。   Then, when the fitting portion 131 of the membrane fixing body 13 is further fitted into the fitted portion 121 of the cell body 12, as shown in FIG. 7, an elastic membrane is formed by the annular pressing portion 131c. 11 is pressed inward from the portion supported by the support portion 121b and outward from the opening 132 (or window portion).

これにより、弾性膜１１においては、外周部が係止された状態にて、押圧される部位が凹凸状に変形するため、窓部が伸びてさらに平面状になる。即ち、弾性膜１１の窓部に、張力がさらに加えられることになる。   Thereby, in the elastic film 11, in the state which the outer peripheral part was latched, since the site | part pressed is deform | transformed into an uneven | corrugated shape, a window part is extended and becomes planar shape. That is, a tension is further applied to the window portion of the elastic film 11.

その一方、環状で且つ凸状の支持部１２１ｂが環状で且つ凸状の押圧部１３１ｃに内嵌するため、支持部１２１ｂの内周部と押圧部１３１ｃの外周部とが弾性膜１１を挟さんで固定し、さらには、シール部材１４がセル本体１２と膜固定体１３とにより押圧されて圧縮するため、弾性膜１１とセル本体１２との間をシールする。   On the other hand, since the annular and convex support portion 121b is fitted into the annular and convex pressing portion 131c, the inner peripheral portion of the support portion 121b and the outer peripheral portion of the pressing portion 131c sandwich the elastic film 11. Further, since the seal member 14 is pressed and compressed by the cell body 12 and the membrane fixing body 13, the space between the elastic membrane 11 and the cell body 12 is sealed.

そして、固定手段１５にて、セル本体１２と膜固定体１３とを固定することにより、弾性膜１１が被嵌合部１２１と嵌合部１３１とにより圧接される。このようにして、セル本体１２と膜固定体１３との間に弾性膜１１を固定したセル１が組み立てられる。   Then, by fixing the cell body 12 and the membrane fixing body 13 by the fixing means 15, the elastic membrane 11 is pressed by the fitted portion 121 and the fitting portion 131. In this way, the cell 1 in which the elastic membrane 11 is fixed between the cell body 12 and the membrane fixing body 13 is assembled.

次に、蛍光Ｘ線分析装置の分析方法について、図１及び図２を参酌して説明する。図１及び図２に示すように、注出手段５の先端部を入口部１２２ａに嵌合させ、注出手段５の内部に収容される試料を注出手段５の先端部から注出させる。   Next, an analysis method of the fluorescent X-ray analyzer will be described with reference to FIGS. As shown in FIGS. 1 and 2, the tip of the pouring means 5 is fitted into the inlet 122 a, and the sample stored in the pouring means 5 is poured out from the tip of the pouring means 5.

すると、注出された試料が、導入部１２２により斜め下方（図２におけるＡ矢印方向）に流れ、試料室１ａの下端から試料室１ａ内に導入される。このとき、注出手段５の先端部と導入部１２２の入口部１２２ａとが密着しているため、入口部１２２ａから外気が侵入するのを防止している。   Then, the poured out sample flows obliquely downward (in the direction of arrow A in FIG. 2) by the introducing portion 122 and is introduced into the sample chamber 1a from the lower end of the sample chamber 1a. At this time, since the front end portion of the pouring means 5 and the inlet portion 122a of the introducing portion 122 are in close contact with each other, the outside air is prevented from entering from the inlet portion 122a.

さらに、注出手段５から試料を注出し続けると、注出された試料が、導入部１２２により試料室１ａ内に導入されるのに伴い、試料室１ａ内の試料が、試料室１ａ内を斜め上方に流れ、導出部１２３により試料室１ａの上端から試料室１ａ外へ導出される。そして、試料室１ａから導出された試料が、導出部１２３により斜め上方（図２におけるＢ矢印方向）に流れ、出口部１２３ａに接続されるホース６１を介してボトル６２内に受け入れられる。   Furthermore, if the sample is continuously poured out from the dispensing means 5, the sample in the sample chamber 1a is moved into the sample chamber 1a as the sample poured out is introduced into the sample chamber 1a by the introduction unit 122. It flows obliquely upward and is led out of the sample chamber 1a from the upper end of the sample chamber 1a by the lead-out part 123. The sample led out from the sample chamber 1a flows obliquely upward (in the direction of arrow B in FIG. 2) by the lead-out part 123 and is received in the bottle 62 via the hose 61 connected to the outlet part 123a.

これにより、試料室１ａ内、具体的には、導入部１２２及び試料室１ａ並びに導出部１２３内に、試料が満たされた状態となる。なお、試料室１ａ内の試料に気泡（外気）が混入した場合においても、試料室１ａが傾斜して配置されると共に、試料室１ａの上端に導出部１２３が接続されているため、気泡が試料室１ａ内に留まることなく、導出部１２３を介してセル１の外部に排出される。   Thus, the sample is filled in the sample chamber 1a, specifically, the introduction unit 122, the sample chamber 1a, and the lead-out unit 123. Even when bubbles (outside air) are mixed into the sample in the sample chamber 1a, the sample chamber 1a is inclined and the outlet 123 is connected to the upper end of the sample chamber 1a. Without remaining in the sample chamber 1 a, the sample is discharged to the outside of the cell 1 through the lead-out portion 123.

その後、操作パネル８を操作することにより、分析が開始され、Ｘ線源２が、平面状に形成される弾性膜１１に対して、光軸を傾斜させてＸ線を照射する（図２におけるＣ矢印は、Ｘ線の光軸を示す）。すると、照射されたＸ線が、膜固定体１３の開口部１３２を通過し、弾性膜１１に透過されることにより、試料室１ａ内の試料に照射される。なお、Ｘ線は、放射状に拡がって照射される。   Thereafter, the operation is started by operating the operation panel 8, and the X-ray source 2 irradiates the elastic film 11 formed in a planar shape with X-rays with the optical axis inclined (in FIG. 2). C arrow indicates the optical axis of X-ray). Then, the irradiated X-rays pass through the opening 132 of the membrane fixing body 13 and are transmitted through the elastic film 11 to irradiate the sample in the sample chamber 1a. Note that X-rays are irradiated while spreading radially.

そして、試料中の所定元素により、試料から蛍光Ｘ線が発生する（放出される）と共に、発生した蛍光Ｘ線が、弾性膜１１に透過され、さらに、膜固定体１３の開口部１３２を通過した後に、検出部３にて検出される（図２におけるＤ矢印は、検出される蛍光Ｘ線の一例を示す）。   Then, a predetermined element in the sample generates (emits) fluorescent X-rays from the sample, and the generated fluorescent X-rays are transmitted through the elastic film 11 and further pass through the opening 132 of the membrane fixing body 13. Then, it is detected by the detection unit 3 (D arrow in FIG. 2 shows an example of the detected fluorescent X-ray).

このとき、セル本体１２の凹部１２１ａ及び膜固定体１３の開口部１３２が、検出部３に向けて拡がるように形成されているため、発生した蛍光Ｘ線が、セル本体１２や膜固定体１３と干渉して（例えばステンレスで形成される部位の中に存在する所定元素を検出して）、検出部３にて検出されるのを抑制している。   At this time, since the concave portion 121a of the cell main body 12 and the opening 132 of the membrane fixing body 13 are formed so as to expand toward the detection section 3, the generated fluorescent X-rays are generated by the cell main body 12 and the membrane fixing body 13. (For example, by detecting a predetermined element present in a portion formed of stainless steel), the detection by the detection unit 3 is suppressed.

さらに、検出部３で検出した蛍光Ｘ線から所定元素を分析し、その分析結果を紙片に印刷する。そして、紙片が紙片排出口７１から排出されることにより、所定の試料についての分析が終了する。   Furthermore, a predetermined element is analyzed from the fluorescent X-rays detected by the detection unit 3, and the analysis result is printed on a piece of paper. Then, when the paper piece is discharged from the paper piece discharge port 71, the analysis of the predetermined sample is completed.

また、別の試料を続けて分析する場合には、注出手段５により、試料室１ａ内に洗浄液を流し、試料室１ａ内を洗浄する。具体的には、導入部１２２及び試料室１ａ並びに導出部１２３の内空間の容積を超える洗浄液を、導入部１２２及び試料室１ａ並びに導出部１２３内に流す。   When another sample is continuously analyzed, a cleaning liquid is poured into the sample chamber 1a by the extraction means 5 to clean the sample chamber 1a. Specifically, a cleaning liquid that exceeds the volume of the inner space of the introduction unit 122, the sample chamber 1a, and the derivation unit 123 is caused to flow into the introduction unit 122, the sample chamber 1a, and the derivation unit 123.

そして、注出手段５により、次に分析する試料を試料室１ａ内に導入させて、分析する。このとき、試料室１ａにおいては、試料や洗浄液が下端部から導入され且つ上端部から導出されるため、残存する試料や洗浄液を重力により押し出しことができ、その結果、容易に置換することができる。これにより、コンタミネーションを防止することができる。   Then, the sample to be analyzed next is introduced into the sample chamber 1a by the dispensing means 5 and analyzed. At this time, in the sample chamber 1a, since the sample and the cleaning liquid are introduced from the lower end portion and led out from the upper end portion, the remaining sample and cleaning liquid can be pushed out by gravity, and as a result, can be easily replaced. . Thereby, contamination can be prevented.

以上より、本実施形態に係る蛍光Ｘ線分析装置のセル１は、セル本体１２が凹部１２１ａの周りに環状の支持部１２１ｂを備えるため、支持部１２１ｂが弾性膜１１を平面状にして支持する。そして、膜固定体１３が環状の押圧部１３１ｃを備えるため、押圧部１３１ｃが、平面状にして支持された弾性膜１１における支持部１２１ｂよりも内方且つ開口部１３２よりも外方の部位を押圧する。   As described above, in the cell 1 of the X-ray fluorescence spectrometer according to the present embodiment, since the cell body 12 includes the annular support portion 121b around the recess 121a, the support portion 121b supports the elastic film 11 in a planar shape. . And since the film | membrane fixed body 13 is provided with the cyclic | annular press part 131c, the press part 131c is a part in the inner side rather than the support part 121b in the elastic film 11 supported by planar shape, and an outer side rather than the opening part 132. Press.

これにより、弾性膜１１の窓部（試料室を形成する部位）に張力を加えることができるため、弾性膜１１の窓部（試料室を形成する部位）に、しわや弛み（撓み）を確実に無くすことができる。したがって、しわや弛み（撓み）を無くすために、例えば、厚い丈夫な弾性膜を採用することなく、Ｘ線透過性に優れる薄い弾性膜１１を採用することもできるため、分析精度を向上させることができる。   Thereby, tension can be applied to the window part (part forming the sample chamber) of the elastic film 11, so that wrinkles and slack (deflection) are surely applied to the window part (part forming the sample chamber) of the elastic film 11. Can be eliminated. Therefore, in order to eliminate wrinkles and slack (deflection), for example, it is possible to adopt the thin elastic film 11 having excellent X-ray permeability without adopting a thick and strong elastic film, thereby improving the analysis accuracy. Can do.

さらに、セル１を組み立てるのに習熟性が要求されないため、セル１の組み立て状況の再現性を向上させることができる。したがって、セル１の組み立て状況に起因する測定誤差が発生するのを防止できる。   Furthermore, since skill is not required for assembling the cell 1, the reproducibility of the assembly state of the cell 1 can be improved. Therefore, it is possible to prevent a measurement error due to the assembly state of the cell 1 from occurring.

また、本実施形態に係る蛍光Ｘ線分析装置のセル１は、セル本体１２の支持部１２１ｂが膜固定体１３の押圧部１３１ｃを内嵌するように構成されるため、支持部１２１ｂと押圧部１３１ｃとの位置関係（位置決め）を正確に行うことができる。また、弾性膜１１が支持部１２１ｂの内周部と押圧部１３１ｃの外周部とに挟まれて固定されるため、弾性膜１１が平面状の部位（押圧される部位よりも内方の部位）に対して、凹凸状に変形された部位で支持部１２１ｂ及び押圧部１３１ｃに固定される。   Moreover, since the cell 1 of the X-ray fluorescence spectrometer according to the present embodiment is configured such that the support part 121b of the cell body 12 fits the pressing part 131c of the membrane fixing body 13, the support part 121b and the pressing part The positional relationship (positioning) with 131c can be accurately performed. Further, since the elastic film 11 is sandwiched and fixed between the inner peripheral part of the support part 121b and the outer peripheral part of the pressing part 131c, the elastic film 11 is a flat part (an inner part from the pressed part). On the other hand, it is fixed to the support part 121b and the pressing part 131c at the part deformed in an uneven shape.

これにより、弾性膜１１がセル本体１２（支持部１２１ｂ）及び膜固定体１３（押圧部１３１ｃ）に固定された後に、弾性膜１１が試料室１ａの内圧により伸びるように変形した場合、弾性膜１１が内方に向けて引っ張られることになるが、例えば、平面状の部位を挟んで固定するのに対して、凹凸状に変形された部位を挟んで掛止するようにして固定する方が、弾性膜１１の位置ずれを防止することができる。   Accordingly, when the elastic film 11 is fixed to the cell body 12 (support part 121b) and the membrane fixing body 13 (pressing part 131c) and then the elastic film 11 is deformed so as to be stretched by the internal pressure of the sample chamber 1a, the elastic film 11 is pulled inward. For example, it is fixed by sandwiching a portion deformed in a concavo-convex shape while being fixed by sandwiching a flat portion. In addition, the displacement of the elastic film 11 can be prevented.

また、本実施形態に係る蛍光Ｘ線分析装置のセル１は、試料室１ａ内の容積を小さくすることにより（例えば、１ｃｃ以下）、試料が接する表面積を小さくし、その結果、洗浄性を向上させることができ、さらには、分析する試料や洗浄液を少なくすることもできる。   Further, the cell 1 of the fluorescent X-ray analyzer according to the present embodiment reduces the volume in the sample chamber 1a (for example, 1 cc or less), thereby reducing the surface area in contact with the sample and, as a result, improving the cleanability. Furthermore, it is possible to reduce the number of samples and cleaning liquid to be analyzed.

また、本実施形態に係る蛍光Ｘ線分析装置は、平面状に維持された弾性膜１１を介して、Ｘ線源２が試料室１ａ内の試料にＸ線を照射する。そして、検出部３が試料から発生する蛍光Ｘ線を検出するため、正確な測定データを取得することができる。   In the X-ray fluorescence analyzer according to the present embodiment, the X-ray source 2 irradiates the sample in the sample chamber 1a with X-rays via the elastic film 11 maintained in a planar shape. And since the detection part 3 detects the fluorescent X-ray | X_line generate | occur | produced from a sample, exact measurement data can be acquired.

また、本実施形態に係る蛍光Ｘ線分析装置は、注出手段５が内部に収容する試料を先端部から注出することにより、導入部１２２により、試料を試料室１ａ内に導入すると共に、導入部１２２と試料室１ａを介して連通している導出部１２３により、試料室１ａに収容されていた測定済みの試料や洗浄液を試料室１ａ外へ導出することができる。   In addition, the fluorescent X-ray analyzer according to the present embodiment introduces the sample into the sample chamber 1a by the introduction unit 122 by pouring out the sample accommodated in the extraction means 5 from the tip portion, The measured sample and the cleaning liquid stored in the sample chamber 1a can be led out of the sample chamber 1a by the lead-out unit 123 communicating with the introduction unit 122 via the sample chamber 1a.

したがって、例えば、各試料を分析するたびに個別のセルを準備する必要がないため、分析ごとにセルを廃棄することがなく、また、各試料を同一のセル１にて分析することができるため、個別のセルにより発生する測定誤差（弾性膜の平面状態等により発生する測定誤差）が生じるのを防止できる。   Therefore, for example, since it is not necessary to prepare a separate cell for each analysis of each sample, the cell is not discarded for each analysis, and each sample can be analyzed in the same cell 1. It is possible to prevent the occurrence of measurement errors (measurement errors caused by the flat state of the elastic film) caused by individual cells.

また、本実施形態に係る蛍光Ｘ線分析装置は、導入部１２２の入口部１２２ａが注出手段５の先端部と嵌合しているため、入口部１２２ａから外気を侵入させることなく試料を試料室１ａ内に導入することができる。したがって、試料中に気泡が発生するのを防止できるため、分析精度を向上させることができる。   Further, in the X-ray fluorescence analyzer according to the present embodiment, since the inlet 122a of the introduction part 122 is fitted with the tip of the extraction means 5, the sample is sampled without intruding outside air from the inlet 122a. It can be introduced into the chamber 1a. Therefore, since it is possible to prevent bubbles from being generated in the sample, analysis accuracy can be improved.

また、本実施形態に係る蛍光Ｘ線分析装置は、注出手段５により、試料室１ａ内の試料の流れを停止させた状態で分析することができる。したがって、試料室１ａの内圧、即ち、試料が弾性膜１１に与える圧力を一定の状態にて何度も分析することができるため、弾性膜１１の変形（伸び）状態が同じ状態にて分析でき、その結果、分析精度を向上させることができる。   Further, the X-ray fluorescence analyzer according to the present embodiment can perform analysis with the extraction means 5 in a state where the flow of the sample in the sample chamber 1a is stopped. Therefore, since the internal pressure of the sample chamber 1a, that is, the pressure applied to the elastic film 11 by the sample can be analyzed many times in a constant state, the deformation (elongation) state of the elastic film 11 can be analyzed in the same state. As a result, the analysis accuracy can be improved.

なお、本発明に係る蛍光Ｘ線分析装置のセル及び蛍光Ｘ線分析装置は、上記した実施の形態に限定されるものではなく、本発明の要旨を逸脱しない範囲内において種々変更を加え得ることは勿論である。   The cell of the fluorescent X-ray analyzer and the fluorescent X-ray analyzer according to the present invention are not limited to the above-described embodiments, and various modifications can be made without departing from the scope of the present invention. Of course.

例えば、本発明に係る蛍光Ｘ線分析装置のセルは、図８に示すように、セル１’の内部を流れる試料の流速を一定とするように構成される場合でもよい。かかる構成を採用すべく、具体的には、セル１’は、導入部１２２’及び試料室１ａ’並びに導出部１２３’の内空間の断面積が一定となるように構成される。   For example, the cell of the fluorescent X-ray analyzer according to the present invention may be configured so that the flow rate of the sample flowing inside the cell 1 'is constant as shown in FIG. Specifically, the cell 1 ′ is configured so that the cross-sectional areas of the inner spaces of the introduction part 122 ′, the sample chamber 1 a ′, and the lead-out part 123 ′ are constant so as to adopt such a configuration.

より具体的には、セル１’は、試料室１ａ’を形成するセル本体１２’の凹部１２１ａ’を備え、凹部１２１ａ’は、湾曲状に形成される湾曲面と、該湾曲面の外縁に連設される環状の側面とを備える。かかる構成によれば、例えば、導入部１２２’及び試料室１ａ’並びに導出部１２３’内に、試料を円滑に流すことができる（液溜まりする箇所が発生するのを防止できる）。   More specifically, the cell 1 ′ includes a concave portion 121a ′ of the cell body 12 ′ that forms the sample chamber 1a ′. The concave portion 121a ′ is formed on a curved surface that is formed in a curved shape and an outer edge of the curved surface. An annular side surface provided continuously. According to such a configuration, for example, the sample can flow smoothly into the introduction part 122 ′, the sample chamber 1 a ′, and the lead-out part 123 ′ (a place where a liquid pool is generated can be prevented).

また、本発明に係る蛍光Ｘ線分析装置のセルは、試料室１ａ内の試料の流れを停止させるべく、弁を備える場合や、導入部１２２や導出部１２３に弁（逆止弁）の機能が設けられる場合でもよい。   Moreover, the cell of the fluorescent X-ray analysis apparatus according to the present invention includes a valve in order to stop the flow of the sample in the sample chamber 1a, or a function of a valve (check valve) in the introduction part 122 or the lead-out part 123. May be provided.

また、本発明に係るＸ線分析装置は、導出部１２３（例えば出口部１２３ａ）に、試料を検出する検出手段（センサ）を備える場合でもよい。かかる構成によれば、試料が試料室１ａ内に満たされていることを確認することができる。   The X-ray analysis apparatus according to the present invention may include a detection unit (sensor) for detecting a sample in the derivation unit 123 (for example, the outlet unit 123a). According to this configuration, it can be confirmed that the sample is filled in the sample chamber 1a.

また、上記実施形態に係る蛍光Ｘ線分析装置のセル１においては、膜固定体１３（嵌合部１３１の内周部１３１ｂ）が弾性膜１１の外周部をセル本体１２（被嵌合部１２１の外周部１２１ｄ）に向けて押圧することにより、弾性膜１１の外周部がセル本体１２に係止される場合を説明したが、かかる場合に限られず、例えば、セル本体に弾性膜の外周部を固定（係止）させべく、セル本体との間に弾性膜の外周部を挟むように構成される環状の固定部材をさらに備える場合でもよい。さらには、接着剤により、弾性膜１１の外周部をセル本体１２に係止（止着）させる場合でもよい。   Further, in the cell 1 of the X-ray fluorescence spectrometer according to the above embodiment, the membrane fixing body 13 (the inner peripheral portion 131b of the fitting portion 131) is connected to the outer peripheral portion of the elastic membrane 11 as the cell main body 12 (the fitted portion 121). In this case, the outer peripheral portion of the elastic film 11 is locked to the cell main body 12 by pressing toward the outer peripheral portion 121d). In order to fix (lock), an annular fixing member configured to sandwich the outer peripheral portion of the elastic membrane between the cell body and the cell body may be further provided. Furthermore, the outer peripheral part of the elastic film 11 may be locked (fixed) to the cell body 12 by an adhesive.

また、上記実施形態に係る蛍光Ｘ線分析装置のセル１においては、セル本体１２の支持部１２１ｂが連続した凸状で且つ円環状に形成される場合を説明したが、かかる場合に限られず、例えば、支持部は、断続的な凸状に形成される場合でもよく、また、角環状に形成される場合でもよい。要するに、支持部は、弾性膜における支持する部位より内方の部位が平面状となるように支持可能に形成されていればよい。   Further, in the cell 1 of the fluorescent X-ray analyzer according to the above-described embodiment, the case where the support portion 121b of the cell body 12 is formed in a continuous convex shape and an annular shape has been described. For example, the support part may be formed in an intermittent convex shape, or may be formed in a square ring shape. In short, the support part should just be formed so that it can support so that the site | part inside from the site | part to support in an elastic film may become planar shape.

また、上記実施形態に係る蛍光Ｘ線分析装置のセル１においては、膜固定体１３の押圧部１３１ｃが連続した凸状で且つ円環状に形成される場合を説明したが、かかる場合に限られず、例えば、押圧部は、断続的な凸状に形成される場合でもよく、また、角環状に形成される場合でもよい。要するに、押圧部は、平面状に支持された弾性膜における支持部よりも内方且つ開口部よりも外方の部位を押圧し、弾性膜における窓部（試料室を形成する部位）が平面状となるように形成されていればよい。   Moreover, in the cell 1 of the fluorescent X-ray analyzer according to the above embodiment, the case where the pressing portion 131c of the membrane fixing body 13 is formed in a continuous convex shape and an annular shape has been described, but the present invention is not limited to this case. For example, the pressing part may be formed in an intermittent convex shape, or may be formed in an annular shape. In short, the pressing portion presses the inner portion of the elastic film supported in a flat shape and the outer portion of the opening, and the window portion (the portion forming the sample chamber) in the elastic film is flat. What is necessary is just to be formed.

また、上記実施形態に係る蛍光Ｘ線分析装置のセル１においては、導入部１２２及び導出部１２３を備える、即ち、フローセルの場合を説明したが、かかる場合に限られず、例えば、試料を内部に密閉する容器形状のセルの場合でもよい。   Moreover, in the cell 1 of the fluorescent X-ray analysis apparatus according to the above-described embodiment, the introduction unit 122 and the derivation unit 123 are provided, that is, the case of the flow cell has been described. However, the present invention is not limited to this case. It may be a container-shaped cell to be sealed.

また、上記実施形態に係るセル１においては、シール部材１４がＯリングである場合を説明したが、かかる場合に限られない。例えば、上記実施形態のセル１においては、シール部材１４と試料室１ａとの間には、セル本体１２の部位が存在しているのに対して、当該部位を省略すべく、シール部材は、シート状で且つ環状のパッキン（環状平パッキン）とし、シール部材の内周部により、試料室の一部を形成させる場合でもよい。   Moreover, in the cell 1 which concerns on the said embodiment, although the case where the sealing member 14 was an O-ring was demonstrated, it is not restricted to such a case. For example, in the cell 1 of the above embodiment, the part of the cell main body 12 exists between the seal member 14 and the sample chamber 1a, but in order to omit the part, the seal member is A sheet-like and annular packing (annular flat packing) may be used, and a part of the sample chamber may be formed by the inner peripheral portion of the seal member.

また、上記実施形態に係る蛍光Ｘ線分析装置は、セル１が装置本体９１に対して着脱可能な構成である場合を説明したが、かかる場合に限られない。例えば、セルのうち、膜固定体が装置本体と一体的に形成される場合でもよい。   In addition, although the fluorescent X-ray analysis apparatus according to the above embodiment has been described with respect to the case where the cell 1 is configured to be detachable from the apparatus main body 91, the present invention is not limited thereto. For example, in the cell, the membrane fixing body may be formed integrally with the apparatus main body.

また、上記実施形態に係る蛍光Ｘ線分析装置は、試料室１ａに試料を導入するために注出手段５として注射器を採用した場合を説明したが、かかる場合に限られない。例えば、導入部１２２の入口部１２２ａに吐出ポンプを取り付ける場合でもよく、また、導出部１２３の出口部１２３ａに吸引ポンプを取り付ける場合でもよい。さらには、試料を収容する容器をセル１より高い位置に配置し、当該容器と導入部１２２の入口部１２２ａとをホースで接続することにより、試料の重力を用いて試料を試料室１ａ内に導入する場合でもよい。   Moreover, although the fluorescence X-ray-analysis apparatus based on the said embodiment demonstrated the case where a syringe was employ | adopted as the extraction means 5 in order to introduce a sample into the sample chamber 1a, it is not restricted to this. For example, a discharge pump may be attached to the inlet portion 122a of the introducing portion 122, or a suction pump may be attached to the outlet portion 123a of the outlet portion 123. Furthermore, the sample is placed in the sample chamber 1a using the gravity of the sample by arranging a container for storing the sample at a position higher than the cell 1 and connecting the container and the inlet 122a of the introduction unit 122 with a hose. It may be introduced.

本発明の一実施形態に係る蛍光Ｘ線分析装置の全体斜視図を示す。1 is an overall perspective view of a fluorescent X-ray analyzer according to an embodiment of the present invention. 同実施形態に係る蛍光Ｘ線分析装置の要部概略断面図を示す。The principal part schematic sectional drawing of the fluorescent X ray analyzer which concerns on the same embodiment is shown. 同実施形態に係る蛍光Ｘ線分析装置の要部概略斜視図を示す。The principal part schematic perspective view of the fluorescent X ray analysis apparatus which concerns on the same embodiment is shown. 同実施形態に係る蛍光Ｘ線分析装置のセルの分解斜視図を示す。The disassembled perspective view of the cell of the fluorescent X-ray analyzer which concerns on the same embodiment is shown. 同実施形態に係る蛍光Ｘ線分析装置のセルの組み立て方法を説明する断面図であって、（ａ）は全体概略図、（ｂ）はＥ領域の拡大図を示す。It is sectional drawing explaining the assembly method of the cell of the fluorescent X-ray analyzer which concerns on the embodiment, Comprising: (a) is a whole schematic diagram, (b) shows the enlarged view of E area | region. 同実施形態に係る蛍光Ｘ線分析装置のセルの組み立て方法を説明する断面図であって、（ａ）は全体概略図、（ｂ）はＦ領域の拡大図を示す。It is sectional drawing explaining the assembly method of the cell of the fluorescent X-ray-analysis apparatus which concerns on the same embodiment, Comprising: (a) is a whole schematic diagram, (b) shows the enlarged view of F area | region. 同実施形態に係る蛍光Ｘ線分析装置のセルの組み立て方法を説明する断面図であって、（ａ）は全体概略図、（ｂ）はＧ領域の拡大図を示す。It is sectional drawing explaining the assembly method of the cell of the fluorescent X-ray-analysis apparatus based on the embodiment, Comprising: (a) is a whole schematic diagram, (b) shows the enlarged view of G area | region. 本発明の他の実施形態に係る蛍光Ｘ線分析装置のセルの断面図であって、（ａ）は全体概略図、（ｂ）はＨ領域の拡大図を示す。It is sectional drawing of the cell of the fluorescent-X-ray-analysis apparatus which concerns on other embodiment of this invention, Comprising: (a) is a whole schematic diagram, (b) shows the enlarged view of H area | region.

符号の説明Explanation of symbols

１…セル、１ａ…試料室、２…Ｘ線源、３…検出部、１１…弾性膜、１２…セル本体、１３…膜固定体、１２１…被嵌合部、１２１ａ…凹部、１２１ｂ…支持部、１２２…導入部、１２２ａ…入口部、１２３…導出部、１３１…嵌合部、１３１ｃ…押圧部、１３２…開口部   DESCRIPTION OF SYMBOLS 1 ... Cell, 1a ... Sample chamber, 2 ... X-ray source, 3 ... Detection part, 11 ... Elastic film, 12 ... Cell main body, 13 ... Membrane fixing body, 121 ... Fit part, 121a ... Recessed part, 121b ... Support , 122 ... introduction part, 122 a ... inlet part, 123 ... derivation part, 131 ... fitting part, 131 c ... pressing part, 132 ... opening part

Claims (4)

Ｘ線透過性を有する弾性膜と、弾性膜に覆われることにより試料を収容するための試料室となる凹部を有するセル本体と、弾性膜をセル本体との間に介在させて固定すると共に、弾性膜を介して試料室内の試料にＸ線を照射させるための開口部を有する膜固定体とを備え、弾性膜がセル本体と膜固定体との間に固定される際に、弾性膜の外周部がセル本体に係止されるように構成される蛍光Ｘ線分析装置のセルにおいて、
セル本体は、外周部が係止された弾性膜を平面状にして支持すべく、凹部の周りに環状の支持部を備え、膜固定体は、平面状にして支持された弾性膜における支持部よりも内方且つ開口部よりも外方の部位を押圧すべく、環状の押圧部を備えることを特徴とする蛍光Ｘ線分析装置のセル。 An elastic membrane having X-ray permeability, a cell main body having a recess serving as a sample chamber for receiving a sample by being covered with the elastic membrane, and an elastic membrane interposed between the cell main body and fixing, A membrane fixing member having an opening for irradiating the sample in the sample chamber with X-rays through the elastic membrane, and when the elastic membrane is fixed between the cell body and the membrane fixing member, In the cell of the fluorescent X-ray analyzer configured so that the outer peripheral portion is locked to the cell body,
The cell body is provided with an annular support portion around the recess to support the elastic membrane with the outer peripheral portion held in a flat shape, and the membrane fixing body is a support portion in the elastic membrane supported in a flat shape. A fluorescent X-ray analyzer cell comprising an annular pressing portion so as to press a portion inside and outside the opening. 支持部は、押圧部を内嵌するように構成され、弾性膜は、支持部の内周部と押圧部の外周部とに挟まれて固定される請求項１に記載の蛍光Ｘ線分析装置のセル。   The fluorescent X-ray analyzer according to claim 1, wherein the support portion is configured to fit the pressing portion, and the elastic film is sandwiched and fixed between the inner peripheral portion of the support portion and the outer peripheral portion of the pressing portion. Cell. 請求項１又は２に記載のセルと、試料室内の試料にＸ線を照射するＸ線源と、試料から発生する蛍光Ｘ線を検出する検出部とを備えることを特徴とする蛍光Ｘ線分析装置。   3. A fluorescent X-ray analysis comprising: the cell according to claim 1; an X-ray source that irradiates a sample in the sample chamber with X-rays; and a detection unit that detects fluorescent X-rays generated from the sample. apparatus. 内部に収容する試料を先端部から注出する注出手段をさらに備え、セルは、試料を試料室へ導入するための導入部と、試料室を介して導入部と連通し、試料を試料室から導出するための導出部とを備え、導入部は、注出手段の先端部と嵌合する入口部を備える請求項３に記載の蛍光Ｘ線分析装置。   The cell further includes an extraction means for extracting the sample accommodated in the tip from the tip portion, the cell communicates with the introduction portion through the sample chamber, an introduction portion for introducing the sample into the sample chamber, and the sample is placed in the sample chamber The fluorescent X-ray analysis apparatus according to claim 3, further comprising: a lead-out portion for lead-out from the lead-out portion, wherein the introduction portion includes an inlet portion that fits with a tip portion of the extraction means.
JP2008231754A 2008-09-10 2008-09-10 Cell of fluorescent x-ray analyzer and fluorescent x-ray analyzer Pending JP2010066085A (en)

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