JP2011089794A - Sample holder for fluorescent x-ray analysis, and method and device of fluorescent x-ray analysis using the same - Google Patents

Sample holder for fluorescent x-ray analysis, and method and device of fluorescent x-ray analysis using the same Download PDF

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JP2011089794A
JP2011089794A JP2009241519A JP2009241519A JP2011089794A JP 2011089794 A JP2011089794 A JP 2011089794A JP 2009241519 A JP2009241519 A JP 2009241519A JP 2009241519 A JP2009241519 A JP 2009241519A JP 2011089794 A JP2011089794 A JP 2011089794A
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cylindrical
sample
holder
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Kenji Watanabe
健二 渡邉
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Rigaku Denki Co Ltd
Rigaku Corp
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Rigaku Corp
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a sample holder for fluorescent X-ray analysis which enhances the analytical sensitivity and analysis accuracy, by holding a large amount of sample dripped and dried in a constant height position, at all times. <P>SOLUTION: The sample holder 1 for fluorescent X-ray analysis includes a tubular fastener 3; a polymeric film 2 having a slack 2a for forming a cavity 2c of a prescribed size, inside the tubular fastener 3 and a periphery 2b locked along one end 3a of the tubular fastener; and a tubular holder 4 for pushing up the slack 2a of the polymeric film in the vicinity of an inner circumference of the tubular holder 4 by being upward slid along the inner circumference of the tubular holder 4. The liquid sample S is immersed and dried in the cavity 2c formed by the slack 2a of the polymeric film being pushed downward. The tubular holder 4 is slid upward, to make one end 4a of the tubular holder flatten the slack 2a, and holds the dried sample. <P>COPYRIGHT: (C)2011,JPO&INPIT

Description

本発明は、液体試料を蛍光X線分析するために用いられる蛍光X線分析用試料保持具ならびにそれを用いる蛍光X線分析方法および装置に関する。   The present invention relates to a fluorescent X-ray analysis sample holder used for fluorescent X-ray analysis of a liquid sample, and a fluorescent X-ray analysis method and apparatus using the same.

従来、液体試料を蛍光X線分析するための技術として、極薄のポリマーフィルムに直径2mmの窪みを成形した試料保持具がMOXTEK社から販売されている。また、図13に示すように液体試料Sを蛍光X線分析するために用いられる蛍光X線分析用試料保持具1であって、輪状の台座2と、台座2に所定の張力で保持される周辺部3aおよびX線を透過させるための透過部3bを有する厚さ12μm以下の熱収縮性フィルム3とを備え、透過部3bに窪み3cが形成されており、透過部の窪み3cに液体試料Sが滴下されて乾燥されることにより、透過部3bが平坦になるとともに、乾燥された試料を保持する蛍光X線分析用試料保持具1がある(特許文献1)。   Conventionally, as a technique for fluorescent X-ray analysis of a liquid sample, a sample holder in which a recess having a diameter of 2 mm is formed in an extremely thin polymer film is sold by MOTTEK. 13 is a fluorescent X-ray analysis sample holder 1 used for fluorescent X-ray analysis of a liquid sample S as shown in FIG. 13, and is held by a ring-shaped base 2 and the base 2 with a predetermined tension. A heat-shrinkable film 3 having a thickness of 12 μm or less having a peripheral portion 3a and a transmissive portion 3b for transmitting X-rays. A dent 3c is formed in the transmissive portion 3b, and a liquid sample is formed in the dent 3c of the transmissive portion. When S is dropped and dried, there is a fluorescent X-ray analysis sample holder 1 that holds the dried sample while the transmission part 3b becomes flat (Patent Document 1).

特開2009−222615号公報JP 2009-222615 A

しかし、MOXTEK社の試料保持具は、ポリマーフィルムを成形して製作されているので、点滴された液体試料Sの乾燥前の試料保持具50の状態を示す断面図である図14および点滴された液体試料Sの乾燥後の試料保持具50の状態を示す断面図である図15に示すように、液体試料Sが点滴される窪み54は、液体試料Sの乾燥後であっても乾燥前と同様に窪んでいるが、液体試料Sの乾燥段階においてポリマーフィルム53に少し変形が生じ、個々の試料保持具50によって窪み54に保持されている乾燥された試料Sの高さが変動し、検出される蛍光X線強度が変動する。そのため、精度よく分析することができない。   However, since the sample holder of MOXTEK is manufactured by molding a polymer film, FIG. 14 which is a cross-sectional view showing the state of the sample holder 50 before drying the instilled liquid sample S and the instilled liquid sample S. As shown in FIG. 15, which is a cross-sectional view showing the state of the sample holder 50 after the liquid sample S is dried, the depression 54 into which the liquid sample S is instilled is not dried even after the liquid sample S is dried. Similarly, the polymer film 53 is slightly deformed in the drying stage of the liquid sample S, and the height of the dried sample S held in the depression 54 by the individual sample holders 50 varies and is detected. The intensity of the fluorescent X-rays to be changed varies. Therefore, it cannot be analyzed with high accuracy.

特許文献1に記載の蛍光X線分析用試料保持具1は、室温において熱収縮性フィルム3を輪状の台座2に所定の張力でぴんと張った状態に伸張し、この伸張した状態で押圧冶具によって押圧して窪み3cを形成する。したがって、室温ではこの窪み3cは平坦な元の状態に戻らない。この窪み3cに液体試料が滴下乾燥される。この液体試料が乾燥されるときの熱量によって熱収縮性フィルム3が収縮して平坦になるとともに、乾燥された試料を保持する。このように、この蛍光X線分析用試料保持具1では、熱収縮性フィルム3が液体試料の乾燥時の熱量によって平坦な状態に戻ることができる窪み3cでなければならないので、その窪み3cの径は小さく深さは浅く、窪み3cが液体試料を保持できる容量は小さい。液体試料を保持できる容量が小さいために試料の濃縮度が低く、高感度の蛍光X線分析を行うことができない。   The sample holder 1 for fluorescent X-ray analysis described in Patent Document 1 is such that a heat-shrinkable film 3 is stretched to a ring-shaped pedestal 2 with a predetermined tension at room temperature, and in this stretched state, a pressing jig is used. The depression 3c is formed by pressing. Therefore, the depression 3c does not return to a flat original state at room temperature. A liquid sample is dropped and dried in the recess 3c. The heat-shrinkable film 3 is shrunk and flattened by the amount of heat when the liquid sample is dried, and the dried sample is held. Thus, in this fluorescent X-ray analysis sample holder 1, the heat-shrinkable film 3 must be a recess 3c that can return to a flat state by the amount of heat when the liquid sample is dried. The diameter is small and the depth is shallow, and the capacity that the recess 3c can hold the liquid sample is small. Since the volume that can hold the liquid sample is small, the concentration of the sample is low, and high-sensitivity X-ray fluorescence analysis cannot be performed.

この浅い窪み3cに液体試料を滴下すると、窪み3cの周辺壁に沿って液体試料が這い上がり、液体試料が窪み3cの外側に広がることがある。特に、有機溶媒溶液の試料ではこの這い上がり現象が起こり易く、液体試料の一部が窪み3cの外で乾燥することがある。そのため、試料によって乾燥された試料の保持位置が異なるため、蛍光X線分析の感度が変動する。また、熱収縮性フィルム3が液体試料の乾燥時に均一な平坦面に戻らず、一部波状になることがある。熱収縮性フィルム3が波状になると、滴下乾燥された試料の高さ位置が変動するため、蛍光X線分析の感度が変動する。   When a liquid sample is dropped into the shallow depression 3c, the liquid sample may creep up along the peripheral wall of the depression 3c, and the liquid sample may spread outside the depression 3c. In particular, this scooping phenomenon is likely to occur in the sample of the organic solvent solution, and a part of the liquid sample may be dried outside the recess 3c. For this reason, since the holding position of the dried sample differs depending on the sample, the sensitivity of the fluorescent X-ray analysis varies. Further, the heat-shrinkable film 3 may not be returned to a uniform flat surface when the liquid sample is dried, and may be partially wavy. When the heat-shrinkable film 3 becomes wavy, the sensitivity of the fluorescent X-ray analysis varies because the height position of the dropped and dried sample varies.

本発明は前記従来の問題に鑑みてなされたもので、液体試料を蛍光X線分析するために用いられる蛍光X線分析用試料保持具ならびにそれを用いる蛍光X線分析方法および装置において、多量の点滴乾燥された試料を常に一定の高さ位置に保持することができる蛍光X線分析用試料保持具を提供することによって分析感度を向上させるとともに分析精度を向上させることを目的とする。   The present invention has been made in view of the above-mentioned conventional problems, and in a fluorescent X-ray analysis sample holder used for fluorescent X-ray analysis of a liquid sample, and a fluorescent X-ray analysis method and apparatus using the same, An object of the present invention is to improve analysis sensitivity and improve analysis accuracy by providing a sample holder for fluorescent X-ray analysis that can always hold a drip-dried sample at a certain height position.

前記目的を達成するために、本発明の蛍光X線分析用試料保持具は、液体試料を蛍光X線分析するために用いられる蛍光X線分析用試料保持具であって、筒状固着具と、その筒状固着具の内側に所定の大きさの窪み部を形成するためのたるみ部および前記筒状固着具の一方の端部に沿って固着される周辺部を有する高分子フィルムと、前記筒状固着具の内径よりも小さい外径を有し、前記筒状固着具の内周に沿ってスライド可能な筒状保持具であって、前記筒状固着具の一方の端部から前記筒状固着具の内側に挿入されて、前記筒状固着具の内周に沿って上方にスライドされて前記高分子フィルムのたるみ部の、前記筒状固着具の内周近傍を押し上げる筒状保持具とを備え、前記高分子フィルムのたるみ部が下方に押し下げられることにより形成される窪み部に液体試料が滴下乾燥され、前記筒状保持具が前記筒状固着具の内周に沿って上方にスライドされ、前記筒状保持具の一方の端部によって前記たるみ部が平坦にされる位置で支持されるとともに乾燥された試料を保持する。   In order to achieve the above object, a sample holder for fluorescent X-ray analysis of the present invention is a sample holder for fluorescent X-ray analysis used for fluorescent X-ray analysis of a liquid sample, and includes a cylindrical fixing tool and A polymer film having a slack portion for forming a hollow portion of a predetermined size inside the cylindrical fixing tool and a peripheral portion fixed along one end of the cylindrical fixing tool, and A cylindrical holder having an outer diameter smaller than an inner diameter of the cylindrical fastener and slidable along an inner periphery of the cylindrical fastener, wherein the cylinder is inserted from one end of the cylindrical fastener. A cylindrical holder inserted inside the cylindrical fastener and slid upward along the inner periphery of the cylindrical fastener to push up the slack portion of the polymer film near the inner periphery of the cylindrical fastener And the slack portion of the polymer film is pushed downward A liquid sample is dripped and dried in the formed recess, the cylindrical holder is slid upward along the inner periphery of the cylindrical fastener, and the slack portion is formed by one end of the cylindrical holder. Hold the dried and supported sample in a flattened position.

本発明の蛍光X線分析用試料保持具によれば、多量の点滴乾燥された試料を常に一定の高さ位置に保持することができるので、高感度および高精度の分析を行うことができる。   According to the sample holder for fluorescent X-ray analysis of the present invention, a large amount of drip-dried sample can always be held at a certain height position, so that highly sensitive and highly accurate analysis can be performed.

本発明の蛍光X線分析装置は、本発明の蛍光X線分析用試料保持具を備える蛍光X線分析装置であって、前記窪み部に液体試料が滴下乾燥され、前記筒状保持具によって前記たるみ部が平坦にされて試料を保持した前記窪み部であった部位に1次X線を照射するX線源と、前記窪み部であった部位から発生する2次X線の強度を測定する検出手段とを備える。   The fluorescent X-ray analyzer of the present invention is a fluorescent X-ray analyzer provided with the fluorescent X-ray analysis sample holder of the present invention, wherein a liquid sample is dropped and dried in the recess, and the cylindrical holder An X-ray source that irradiates primary X-rays to a portion that was the hollow portion where the slack portion was flattened and held the sample, and the intensity of secondary X-rays generated from the portion that was the hollow portion are measured Detecting means.

本発明の蛍光X線分析用試料保持具の作製方法は、蛍光X線分析用試料保持具の作製方法であって、筒状固着具と高分子フィルムを準備し、前記筒状固着具の内側に所定の大きさの窪み部を形成するためのたるみ部が生じるように前記筒状固着具の一方の端部に沿って前記高分子フィルムの周辺部を固着し、前記筒状固着具の内径よりも小さい外径を有し、前記筒状固着具の内周に沿ってスライド可能な筒状保持具を準備し、前記筒状保持具を前記筒状固着具の一方の端部より内側に挿入し、前記筒状固着具の内周に沿って上方にスライドさせて前記高分子フィルムのたるみ部の、前記筒状固着具の内周近傍を押し上げて前記筒状保持具の一方の端部によって前記たるみ部を平坦にし、前記筒状保持具を下方にスライドさせ、再度前記高分子フィルムのたるみ部を形成してこのたるみ部を下方に押し下げることにより、滴下される液体試料を保持する窪み部を形成する。   The method for producing a sample holder for fluorescent X-ray analysis of the present invention is a method for producing a sample holder for fluorescent X-ray analysis, comprising a cylindrical fixing tool and a polymer film, and an inner side of the cylindrical fixing tool. The peripheral part of the polymer film is fixed along one end of the cylindrical fixing tool so that a slack part for forming a hollow part of a predetermined size is formed on the inner diameter of the cylindrical fixing tool. A cylindrical holder that has a smaller outer diameter and is slidable along the inner periphery of the cylindrical fastener, and the cylindrical holder is located inside one end of the cylindrical fastener. Insert and slide upward along the inner periphery of the cylindrical fastener to push up the slack portion of the polymer film in the vicinity of the inner periphery of the cylindrical fastener to one end of the cylindrical holder The slack portion is flattened by sliding the cylindrical holder downward and again the polymer. To form a slack portion of Irumu by depressing the slack portion downwardly to form a recess portion for holding a liquid sample is dropped.

本発明の蛍光X線分析用試料保持具の作製方法によれば、多量の点滴乾燥された試料を常に一定の高さ位置に保持することができる蛍光X線分析用試料保持具を作製することができるので、高感度および高精度の分析を行うことができる。   According to the method for producing a sample holder for fluorescent X-ray analysis of the present invention, a sample holder for fluorescent X-ray analysis that can always hold a large amount of drip-dried sample at a certain height position is produced. Therefore, highly sensitive and highly accurate analysis can be performed.

本発明の蛍光X線分析方法は、本発明の蛍光X線分析用試料保持具を用いる蛍光X線分析方法であって、前記窪み部に液体試料を滴下乾燥させ、前記筒状保持具によって前記たるみ部を平坦にする位置で支持するとともに、前記窪み部であった部位に乾燥された試料を保持させ、前記窪み部であった部位に1次X線を照射して、発生する2次X線の強度を測定する。   The fluorescent X-ray analysis method of the present invention is a fluorescent X-ray analysis method using the fluorescent X-ray analysis sample holder of the present invention, in which a liquid sample is dropped and dried in the recess, and the cylindrical holder is used to While supporting the slack portion at a flattened position, the dried sample is held in the portion that was the depression, and the secondary X generated by irradiating the portion that was the depression with primary X-rays. Measure the line strength.

本発明の蛍光X線分析方法および装置によれば、本発明の蛍光X線分析用試料保持具を用いるので、本発明の蛍光X線分析用試料保持具と同様の作用効果が得られる。   According to the fluorescent X-ray analysis method and apparatus of the present invention, since the fluorescent X-ray analysis sample holder of the present invention is used, the same effects as the fluorescent X-ray analysis sample holder of the present invention can be obtained.

本発明の第1実施形態である蛍光X線分析用試料保持具の筒状固着具の縦断面図である。It is a longitudinal cross-sectional view of the cylindrical fixing tool of the sample holder for fluorescent X-ray analysis which is 1st Embodiment of this invention. 同試料保持具の筒状固着具に筒状保持具が挿入された状態を示す縦断面図である。It is a longitudinal cross-sectional view which shows the state by which the cylindrical holder was inserted in the cylindrical fixing tool of the sample holder. 同試料保持具のたるみ部が平坦になっている状態を示す縦断面図である。It is a longitudinal cross-sectional view which shows the state in which the slack part of the sample holder is flat. 同試料保持具の窪み部が押圧冶具によって形成される状態を示す縦断面図である。It is a longitudinal cross-sectional view which shows the state in which the hollow part of the sample holder is formed with a pressing jig. 同試料保持具による液体試料の保持状態を示す縦断面図である。It is a longitudinal cross-sectional view which shows the holding state of the liquid sample by the sample holder. 同試料保持具のたるみ部が平坦になり乾燥された試料を保持する状態を示す縦断面図である。It is a longitudinal cross-sectional view which shows the state which hold | maintains the sample which the slack part of the sample holder became flat and was dried. Siの検量線である。It is a calibration curve of Si. 本発明の第3実施形態である上面照射型蛍光X線分析装置の概略図である。It is the schematic of the top surface irradiation type | mold fluorescence X-ray-analysis apparatus which is 3rd Embodiment of this invention. 本発明の第3実施形態の変形である下面照射型蛍光X線分析装置の概略図である。It is the schematic of the bottom surface irradiation type | mold fluorescence X-ray-analysis apparatus which is a deformation | transformation of 3rd Embodiment of this invention. Naの測定データである。It is measurement data of Na. Mgの測定データである。It is the measurement data of Mg. Alの測定データである。It is the measurement data of Al. 従来の試料保持具の斜視図である。It is a perspective view of the conventional sample holder. 従来の他の試料保持具が液体試料を保持する状態を示す縦断面図である。It is a longitudinal cross-sectional view which shows the state in which the other conventional sample holder hold | maintains a liquid sample. 同試料保持具が乾燥された試料を保持する状態を示す縦断面図である。It is a longitudinal section showing the state where the sample holder holds the dried sample.

以下、本発明の第1実施形態である蛍光X線分析用試料保持具について説明する。筒状固着具3と高分子フィルム2を準備し、図1に示すように筒状固着具3の内側に所定の大きさの窪み部を形成するためのたるみ部2aを形成するように、筒状固着具3の一方の端部3aに沿って高分子フィルムの周辺部2bを固着する。このたるみ部2aは所定の半径を有する円形である。高分子フィルムの周辺部2bを固着する方法については後述する。筒状固着具3は、他の内周部位よりも大きい滑り摩擦力を有する係止部、例えば3列の円周スリット3cを、他方の端部3bの内周に備えている。例えば、筒状固着具3は外径43.5mm、内径40.5mm、高さ23mmの筒状であり、ポリエチレン、ポリスチレンなどの樹脂材料からなる。例えば、高分子フィルム2は厚さ12μm以下、好ましくは2〜8μmのポリエステル、ポリプロピレン、ポリイミドなどからなり、材質としてはポリイミドがより好ましい。   Hereinafter, the sample holder for fluorescent X-ray analysis which is 1st Embodiment of this invention is demonstrated. A cylindrical fixing tool 3 and a polymer film 2 are prepared, and as shown in FIG. 1, a cylindrical part is formed so as to form a slack part 2a for forming a recessed part of a predetermined size inside the cylindrical fixing tool 3. The peripheral portion 2b of the polymer film is fixed along one end 3a of the shaped fixing tool 3. The slack portion 2a is a circle having a predetermined radius. A method for fixing the peripheral portion 2b of the polymer film will be described later. The cylindrical fixing tool 3 includes a locking portion having a sliding friction force larger than that of other inner peripheral portions, for example, three rows of circumferential slits 3c on the inner periphery of the other end portion 3b. For example, the cylindrical fixture 3 has a cylindrical shape with an outer diameter of 43.5 mm, an inner diameter of 40.5 mm, and a height of 23 mm, and is made of a resin material such as polyethylene or polystyrene. For example, the polymer film 2 is made of polyester, polypropylene, polyimide or the like having a thickness of 12 μm or less, preferably 2 to 8 μm, and the material is more preferably polyimide.

筒状固着具3の内径よりも小さい外径を有し、筒状固着具3の内周に沿ってスライド可能な筒状保持具4を準備する。例えば、筒状保持具4は外径40.0mm、内径38mm、高さ24.5mmの筒状であり、ポリエチレン、ポリスチレンなどの合成樹脂材料からなる。   A cylindrical holder 4 having an outer diameter smaller than the inner diameter of the cylindrical fastener 3 and slidable along the inner periphery of the cylindrical fastener 3 is prepared. For example, the cylindrical holder 4 has a cylindrical shape with an outer diameter of 40.0 mm, an inner diameter of 38 mm, and a height of 24.5 mm, and is made of a synthetic resin material such as polyethylene or polystyrene.

図2に示すように筒状保持具4を筒状固着具3の他方の端部3bより内側に挿入し、筒状固着具3の内周に沿って上方にスライドする。筒状固着具3を上方にスライドする方法としては、筒状保持具4の他方の端部4bを机上に置いて、筒状保持具4の外径よりも僅かに大きい内径と十分な深さを持つ釣鐘型の押し込み冶具(図示なし)を用いて、筒状固着具3を筒状保持具4の外周に沿って下方にスライドさせてもよい。   As shown in FIG. 2, the cylindrical holder 4 is inserted inside the other end 3 b of the cylindrical fixing tool 3 and is slid upward along the inner periphery of the cylindrical fixing tool 3. As a method of sliding the cylindrical fixing tool 3 upward, the other end 4b of the cylindrical holder 4 is placed on a desk, and an inner diameter slightly larger than the outer diameter of the cylindrical holder 4 and a sufficient depth. The cylindrical fixing tool 3 may be slid downward along the outer periphery of the cylindrical holder 4 using a bell-shaped pushing jig (not shown) having

筒状固着具3の内周に沿って上方にスライドさせると、図3に示すように筒状保持具4の一方の端部4aによってたるみ部2aが平坦にされる位置で支持される。このとき、筒状保持具4の一方の端部の端面4dと筒状固着具3の他方の端部の端面3dが面一になった位置で、筒状固着具3の係止部3cによってたるみ部2aが支持され、ぴんと張った平坦な状態に伸張される。   When it is slid upward along the inner periphery of the cylindrical fixture 3, the slack portion 2a is supported at a position where the slack portion 2a is flattened by one end 4a of the cylindrical holder 4 as shown in FIG. At this time, at the position where the end surface 4d of one end of the cylindrical holder 4 and the end surface 3d of the other end of the cylindrical fastener 3 are flush with each other, the locking portion 3c of the cylindrical fastener 3 The slack portion 2a is supported and stretched to a tight flat state.

ぴんと張った平坦な状態への伸張は、筒状保持具4の一方の端部の端面4dが筒状固着具3の他方の端部の端面3dよりも数mm出っ張った位置で、たるみ部2aが支持されてもよい。本発明の第1実施形態の試料保持具1では、端面4dと端面3dが面一、または端面4dが端面3dよりも数mm出っ張った位置でたるみ部2aが支持されるように、筒状保持具4の高さが筒状固着具3の高さよりも1.5mm高く形成されている。   The tensioned flat state is extended at a position where the end surface 4d of one end of the cylindrical holder 4 protrudes several millimeters from the end surface 3d of the other end of the cylindrical fixing member 3 and the slack portion 2a. May be supported. In the sample holder 1 according to the first embodiment of the present invention, the cylindrical holding is performed so that the slack portion 2a is supported at a position where the end surface 4d and the end surface 3d are flush with each other, or the end surface 4d protrudes several mm from the end surface 3d. The height of the tool 4 is 1.5 mm higher than the height of the cylindrical fixing tool 3.

図3から分かるように、筒状保持具4の一方の端部の端面4dと筒状固着具3の他方の端部の端面3dが面一の状態で支持されている高分子フィルム2のたるみ部2aは、その全体が平面上に伸張されると、筒状保持具4の高さと同外径の1/2とが加算された長さの半径を有する円形である。   As can be seen from FIG. 3, the sagging of the polymer film 2 in which the end surface 4d at one end of the cylindrical holder 4 and the end surface 3d at the other end of the cylindrical fixture 3 are supported in a flush state. When the entire portion 2a is extended on a plane, the portion 2a has a circular shape having a radius of a length obtained by adding the height of the cylindrical holder 4 and 1/2 of the same outer diameter.

筒状保持具4を下方にスライドさせ、再度前記高分子フィルムのたるみ部2aを形成してこのたるみ部2aを下方に押し下げることにより、滴下される液体試料Sを保持する窪み部2cを形成する。図4に示すように例えば直径15mm、長さ100mmの円柱である、ポリエチレンやテフロン(登録商標)などの合成樹脂製、または高分子フィルム2を損傷させないように端面が処理されたガラス管などの押圧冶具5を用いて、たるみ部2aを下方に押し下げることによって窪み2cを形成する。形成される窪み部2cは、例えば深さが約20mm、平面視で直径が約15mmの円形である。窪み2cの形状は上記に限らず、平面視で楕円形、矩形など点滴された液体試料が保持できる窪んだ形状であればよい。また、寸法も上記に限らず筒状保持具4を下方にスライドさせる距離を変えることによって、深さ2〜20mm、平面視での最大長さ5〜35mmなど点滴する液体試料量に適した大きさに形成すればよい。   The cylindrical holder 4 is slid downward, the slack portion 2a of the polymer film is formed again, and the slack portion 2a is pushed downward to form the hollow portion 2c that holds the liquid sample S to be dropped. . As shown in FIG. 4, for example, a cylinder having a diameter of 15 mm and a length of 100 mm, made of a synthetic resin such as polyethylene or Teflon (registered trademark), or a glass tube whose end face is treated so as not to damage the polymer film 2 The depression 2c is formed by pressing the slack portion 2a downward using the pressing jig 5. The formed recess 2c is, for example, a circle having a depth of about 20 mm and a diameter of about 15 mm in plan view. The shape of the dent 2c is not limited to the above, and may be any shape that can hold an instilled liquid sample such as an ellipse or a rectangle in plan view. Also, the dimensions are not limited to the above, and the size suitable for the amount of liquid sample to be instilled, such as a depth of 2 to 20 mm and a maximum length of 5 to 35 mm in plan view, by changing the distance by which the cylindrical holder 4 is slid downward. What is necessary is just to form.

高分子フィルム2を筒状固着具3に固着する方法について説明する。前記したようにたるみ部2aの円形の所定の半径は筒状保持具4の高さと同外径によって算出することができるので、この所定の半径を有する円の外周に、筒状固着具3の一方の端部3aに沿って固着するためののりしろとなる周辺部2bを有する高分子フィルム2を準備する。例えば、前記した外径40.0mm、内径38mm、高さ24.5mmの筒状保持具4を用い、周辺部2bの幅を20mmにすると、たるみ部2aの半径は44.5mmであるので、半径64.5mmの高分子フィルム2を準備する。高分子フィルム2の試料が接触しない面にたるみ部2aと周辺部2bとの境界に線を表示するなどして、のりしろとなる周辺部2bの領域を明確にして、筒状固着具3の一方の端部3a、例えば端部3aの外周に沿って周辺部2bを固着する。固着する個所は端部3aの外周に限らず、端部3aの端面であってもよい。高分子フィルム2を固着する方法は溶着、接着剤による接着、粘着テープによる貼付などによるのが好ましいが、リング等によって固定されていてもよい。   A method for fixing the polymer film 2 to the cylindrical fixing tool 3 will be described. As described above, the circular predetermined radius of the slack portion 2a can be calculated from the same outer diameter as the height of the cylindrical holder 4, so that the cylindrical fastener 3 is placed on the outer periphery of the circle having the predetermined radius. A polymer film 2 having a peripheral portion 2b serving as a margin for adhering along one end portion 3a is prepared. For example, if the cylindrical holder 4 having an outer diameter of 40.0 mm, an inner diameter of 38 mm, and a height of 24.5 mm is used and the width of the peripheral portion 2b is 20 mm, the radius of the slack portion 2a is 44.5 mm. A polymer film 2 having a radius of 64.5 mm is prepared. The region of the peripheral portion 2b that becomes a margin is clarified by displaying a line on the boundary between the slack portion 2a and the peripheral portion 2b on the surface of the polymer film 2 that is not in contact with the sample. The peripheral portion 2b is fixed along the outer periphery of the end portion 3a, for example, the end portion 3a. The part to be fixed is not limited to the outer periphery of the end 3a, but may be the end face of the end 3a. The polymer film 2 is preferably fixed by welding, bonding with an adhesive, sticking with an adhesive tape, or the like, but it may be fixed with a ring or the like.

なお、第1実施形態の試料保持具1の作製方法も本発明の実施形態である。   In addition, the manufacturing method of the sample holder 1 of 1st Embodiment is also embodiment of this invention.

この試料保持具1を用いる蛍光X線分析においては、図5に示すように、窪み2cに液体試料Sを滴下する。ここで、窪み2cはその周囲よりも窪んでいるので、液体試料Sは窪み2cから周囲に転がることがなく、窪み2cで安定に保持される。そして、滴下した液体試料Sを適切な加熱乾燥器具により40〜60℃に加熱乾燥させると、窪み2cの液体試料Sが乾燥されて保持される。   In the fluorescent X-ray analysis using the sample holder 1, the liquid sample S is dropped into the recess 2c as shown in FIG. Here, since the recess 2c is recessed from the periphery thereof, the liquid sample S does not roll from the recess 2c to the periphery, and is stably held in the recess 2c. And if the dripped liquid sample S is heat-dried at 40-60 degreeC with a suitable heat-drying instrument, the liquid sample S of the hollow 2c will be dried and hold | maintained.

筒状保持具4を筒状固着具3の内周に沿って上方にスライドさせると、図6に示すようにたるみ部2aがぴんと張った平坦になる位置で係止部3cによって支持され、その位置で乾燥された試料Sが保持される。   When the cylindrical holder 4 is slid upward along the inner periphery of the cylindrical fixture 3, the slack portion 2a is supported by the locking portion 3c at a flattened position as shown in FIG. The sample S dried in position is held.

試料保持具1を蛍光X線分析装置の試料台へ載置して、液体試料Sの含有成分Sを保持した窪み2cであった部位に1次X線を照射して蛍光X線分析を行う。試料保持具1を蛍光X線分析装置の試料台へ載置する方法については、後述する。   The sample holder 1 is placed on the sample stage of the fluorescent X-ray analyzer, and the X-ray fluorescence analysis is performed by irradiating the primary X-rays onto the portion that was the recess 2c holding the component S of the liquid sample S. . A method for placing the sample holder 1 on the sample stage of the X-ray fluorescence analyzer will be described later.

第1実施形態の試料保持具1を用いて、微量のSiを含んだエーテル類溶液試料1を100μl(マイクロリットル)点滴乾燥して1次X線出力2.4KWで測定したときの検量線を図7に示す。この検量線は横軸がSiの濃度、縦軸が蛍光X線強度であり、4ppm以下の範囲で良い直線性を示している。蛍光X線強度の測定時間が120秒間であるこの検量線から検出限界LLDを算出すると30ppbとなる。この測定結果によれば、今迄測定することができなかった有機溶媒中の微量のSiの測定が可能となった。   Using the sample holder 1 of the first embodiment, a calibration curve is obtained when the ether solution sample 1 containing a trace amount of Si is drip-dried 100 μl (microliter) and measured with a primary X-ray output of 2.4 KW. As shown in FIG. In this calibration curve, the horizontal axis represents the concentration of Si, the vertical axis represents the fluorescent X-ray intensity, and shows good linearity in the range of 4 ppm or less. When the detection limit LLD is calculated from this calibration curve in which the measurement time of the fluorescent X-ray intensity is 120 seconds, it becomes 30 ppb. According to this measurement result, it was possible to measure a trace amount of Si in an organic solvent that could not be measured until now.

以上のように、第1実施形態の蛍光X線分析用試料保持具1によれば、高分子フィルムのたるみ部2aを下方に押し下げることにより深い大きな窪み部2cが形成されるので、多量の液体試料を1度に滴下・乾燥でき、高い濃縮度によって高感度の分析を高精度で行うことができる。従来技術のように多量の液体試料を点滴するために、複数回点滴すると、点滴量の誤差が複数回累積し、点滴量誤差が大きくなり分析精度が悪くなる。例えば、10回点滴したら誤差は10倍になる。さらに、乾燥された試料Sがぴんと張った平坦に伸張された高分子フィルム2に保持されるので、測定時の試料高さは常に一定の高さになり、精度のよい分析を行うことができる。特に表面張力が弱く、液体試料が這い上がり窪みの外側に広がり易い有機溶媒溶液の試料であっても深い大きな窪み部2cの一定位置に保持されるため、再現性のよい分析を行なうことができ、その効果は顕著である。さらに、点滴乾燥された試料Sの保持担体として高分子フィルム2を用いているので、保持担体からの散乱X線を減少させてバックグラウンドを抑制することができる。   As described above, according to the sample holder 1 for X-ray fluorescence analysis of the first embodiment, the deep large depression 2c is formed by pushing down the slack portion 2a of the polymer film downward, so that a large amount of liquid The sample can be dropped and dried at a time, and high sensitivity analysis can be performed with high accuracy due to high concentration. If a plurality of infusions are performed to instill a large amount of liquid sample as in the prior art, the infusion amount error accumulates a plurality of times, the infusion amount error increases, and the analysis accuracy deteriorates. For example, if drip is performed 10 times, the error becomes 10 times. Furthermore, since the dried sample S is held by the tightly stretched and flat polymer film 2, the sample height at the time of measurement is always a constant height, and an accurate analysis can be performed. . In particular, even a sample of an organic solvent solution whose surface tension is weak and the liquid sample crawls up and easily spreads outside the depression is held at a fixed position in the deep large depression 2c, so that a reproducible analysis can be performed. The effect is remarkable. Furthermore, since the polymer film 2 is used as the holding carrier for the drip-dried sample S, the background can be suppressed by reducing scattered X-rays from the holding carrier.

次に、本発明の第2実施形態の蛍光X線分析方法について説明する。この分析方法に使用される蛍光X線分析装置10は、本発明の第3実施形態であり、図8に示すように、第1実施形態の蛍光X線分析用試料保持具1を備える装置であって、試料保持具1が直接または試料ホルダ18を介して載置される試料台である試料ステージ17と、液体試料Sが滴下されて乾燥されることにより、乾燥された試料Sを保持した窪み2cであった部位2dに1次X線12を照射するX線管などのX線源11と、窪み2cであった部位2dから発生する蛍光X線などの2次X線15の強度を測定するX線検出器などの検出手段16とを備えている。試料ホルダ18からの散乱線の影響を低減するため、また、高さ調整のための適切な素材のスペーサー19を備えてもよい。   Next, a fluorescent X-ray analysis method according to the second embodiment of the present invention will be described. An X-ray fluorescence analyzer 10 used in this analysis method is a third embodiment of the present invention, and as shown in FIG. 8, is an apparatus including the sample holder 1 for X-ray fluorescence analysis of the first embodiment. The sample holder 1 is a sample stage 17 that is placed directly or via the sample holder 18, and the liquid sample S is dropped and dried to hold the dried sample S. The intensity of the secondary X-ray 15 such as an X-ray source 11 such as an X-ray tube that irradiates the primary X-ray 12 to the part 2d that was the depression 2c, and the fluorescent X-ray generated from the part 2d that was the depression 2c. And a detecting means 16 such as an X-ray detector for measurement. In order to reduce the influence of scattered radiation from the sample holder 18, a spacer 19 made of an appropriate material for height adjustment may be provided.

この装置を使用する第2実施形態の蛍光X線分析方法では、第1実施形態の蛍光X線分析用試料保持具1の窪み2cに液体試料Sを滴下して乾燥させた後、筒状保持具4を筒状固着具3の内周に沿って上方にスライドさせ、図6に示すようにたるみ部2aがぴんと張った平坦になる位置で係止部3cによって支持され、その位置で乾燥された試料Sが保持される。乾燥された試料Sが保持された試料保持具1全体を、底付き円筒状の試料ホルダ18の開口部に載置して、その試料ホルダ18を試料ステージ17に載置する。   In the fluorescent X-ray analysis method of the second embodiment using this apparatus, the liquid sample S is dropped into the recess 2c of the fluorescent X-ray analysis sample holder 1 of the first embodiment and dried, and then held in a cylindrical shape. The tool 4 is slid upward along the inner periphery of the cylindrical fixing tool 3, and is supported by the locking part 3c at a flattened position where the slack part 2a is tight as shown in FIG. 6, and is dried at that position. Sample S is held. The entire sample holder 1 holding the dried sample S is placed in the opening of the bottomed cylindrical sample holder 18, and the sample holder 18 is placed on the sample stage 17.

試料ホルダ18を用いず、試料保持具1を直接試料ステージ17に載置してもよい。   The sample holder 1 may be placed directly on the sample stage 17 without using the sample holder 18.

以上のように試料ステージ17に載置した試料保持具1の乾燥された試料Sを保持した窪み2cであった部位2dに1次X線12を照射して、発生する2次X線15の強度を測定する。   As described above, the primary X-ray 12 is irradiated to the portion 2d which is the depression 2c holding the dried sample S of the sample holder 1 placed on the sample stage 17, and the secondary X-ray 15 generated is generated. Measure strength.

元素Na、Mg、Alがそれぞれ5000ppm含有されているオイルを芳香族系有機溶媒で200倍に希釈し、その芳香族系溶液を、本実施形態の分析方法によって、窪み2cに30μl点滴して1次X線出力50Wで120秒間測定したデータを図10〜12に示す。この測定データは、横軸が蛍光X線分析装置のゴニオの走査角度である2θ、縦軸が蛍光X線強度である。この測定結果は、検出限界LLDが、Na3.3ppm、Mg2.3ppm、Al0.68ppmという高感度なデータである。したがって、高倍率に希釈しても試料中の微量成分の測定をすることができる。さらに重油などのオイル試料を高倍率に希釈することによって共存元素の影響を充分に抑制することができ、高精度の分析ができる。なお、図10〜12に示す測定データの採取には、液体試料を保持する高分子フィルム2として厚さ12μmのポリプロピレンフィルムを用いた。   An oil containing 5000 ppm of each of the elements Na, Mg, and Al is diluted 200 times with an aromatic organic solvent, and the aromatic solution is instilled into the depression 2c by 30 μl by the analysis method of this embodiment. Data measured for 120 seconds at the next X-ray output of 50 W are shown in FIGS. In this measurement data, the horizontal axis represents 2θ which is the gonio scanning angle of the fluorescent X-ray analyzer, and the vertical axis represents the fluorescent X-ray intensity. This measurement result is highly sensitive data with a detection limit LLD of Na 3.3 ppm, Mg 2.3 ppm, and Al 0.68 ppm. Therefore, even when diluted at a high magnification, it is possible to measure trace components in the sample. Furthermore, by diluting an oil sample such as heavy oil at a high magnification, the influence of coexisting elements can be sufficiently suppressed, and high-precision analysis can be performed. In collecting the measurement data shown in FIGS. 10 to 12, a polypropylene film having a thickness of 12 μm was used as the polymer film 2 holding the liquid sample.

以上は、乾燥された試料Sの上方から1次X線12を照射するいわゆる上面照射の場合であるが、図9に示すように、乾燥された試料Sの下方から1次X線を照射するいわゆる下面照射の場合にも、試料保持具1を用いることができる。   The above is the case of so-called top surface irradiation in which the primary X-ray 12 is irradiated from above the dried sample S. As shown in FIG. 9, the primary X-ray is irradiated from below the dried sample S. The sample holder 1 can also be used in the case of so-called bottom irradiation.

第2、第3実施形態の方法、装置によれば、第1実施形態の蛍光X線分析用試料保持具1を用いるので、第1実施形態と同様の作用効果が得られる。   According to the method and apparatus of the second and third embodiments, since the fluorescent X-ray analysis sample holder 1 of the first embodiment is used, the same operational effects as those of the first embodiment can be obtained.

前記した実施形態においては、高分子フィルム2を筒状固着具3の一方の端部3aに沿って固着した蛍光X線分析用試料保持具1について説明したが、筒状固着具3を用いずに、筒状保持具の一方の端部に沿って脱着可能なスナップリング(図示なし)によって、筒状保持具4に高分子フィルム2を支持してもよい。例えば、ポリエチレン製のスナップリングは、筒状保持具の一方の端部の外周において凹凸の嵌合によって結合され、その嵌合を外すことによって筒状保持具から取外すことができる。   In the embodiment described above, the sample holder 1 for fluorescent X-ray analysis in which the polymer film 2 is fixed along the one end 3a of the cylindrical fixture 3 has been described, but the cylindrical fixture 3 is not used. In addition, the polymer film 2 may be supported on the cylindrical holder 4 by a snap ring (not shown) that is detachable along one end of the cylindrical holder. For example, a snap ring made of polyethylene is coupled by an uneven fitting on the outer periphery of one end of the cylindrical holder, and can be removed from the cylindrical holder by removing the fitting.

このスナップリングを用いる蛍光X線分析用試料保持具においては、高分子フィルム2をスナップリングと筒状保持具4の一方の端部4aとの間に挟み、押圧冶具5によって所望の大きさの窪み部2cを形成した後、スナップリングで高分子フィルム2を筒状保持具4の一方の端部4aに支持する。この窪み2cに液体試料Sを滴下して乾燥させる。液体試料Sが乾燥すると、スナップリングを筒状保持具4から取外し、高分子フィルム2を筒状保持具の一方の端部4aの端面においてぴんと張った平坦になるように伸張して、スナップリングで高分子フィルム2を筒状保持具の一方の端部4aに支持する。窪み2cであった部位2dに乾燥された試料Sが保持されているので、第2実施形態の分析方法と同様に試料保持具1全体を、試料ホルダ18の開口部に載置して、その試料ホルダ18を試料ステージ17に載置して分析する。   In the sample holder for fluorescent X-ray analysis using this snap ring, the polymer film 2 is sandwiched between the snap ring and one end portion 4a of the cylindrical holder 4, and the pressing jig 5 has a desired size. After forming the recess 2c, the polymer film 2 is supported on one end 4a of the cylindrical holder 4 with a snap ring. The liquid sample S is dropped into the recess 2c and dried. When the liquid sample S is dried, the snap ring is removed from the cylindrical holder 4, and the polymer film 2 is stretched so as to be tight and flat on the end surface of one end portion 4a of the cylindrical holder. The polymer film 2 is supported by one end 4a of the cylindrical holder. Since the dried sample S is held in the portion 2d that is the depression 2c, the entire sample holder 1 is placed on the opening of the sample holder 18 in the same manner as the analysis method of the second embodiment. The sample holder 18 is placed on the sample stage 17 and analyzed.

この分析方法は、所望の大きな窪み部2cが形成されるので、多量の液体試料を1回の操作で滴下・乾燥でき、高い濃縮度によって高感度かつ高精度の分析をすることができる。従来技術のように多量の液体試料を点滴するために、複数回点滴すると、点滴量の誤差が複数回累積し、点滴量誤差が大きくなり分析精度が悪くなる。例えば、10回点滴したら誤差は10倍になる。さらに、乾燥された試料Sがぴんと張った平坦に伸張された高分子フィルム2に保持されるので、測定時の試料高さは常に一定の高さになり、精度のよい分析を行うことができる。特に、表面張力が弱く液体試料が這い上がり窪みの外側に広がり易い有機溶媒溶液の試料であっても深い大きな窪み部2cの一定位置に保持されるため、再現性のよい分析を行なうことができ、その効果は顕著である。   In this analysis method, since a desired large depression 2c is formed, a large amount of liquid sample can be dropped and dried by one operation, and high sensitivity and high accuracy analysis can be performed with high concentration. If a plurality of infusions are performed to instill a large amount of liquid sample as in the prior art, the infusion amount error accumulates a plurality of times, the infusion amount error increases, and the analysis accuracy deteriorates. For example, if drip is performed 10 times, the error becomes 10 times. Furthermore, since the dried sample S is held by the tightly stretched and flat polymer film 2, the sample height at the time of measurement is always a constant height, and an accurate analysis can be performed. . In particular, even a sample of an organic solvent solution whose surface tension is weak and the liquid sample tends to spread and spread outside the depression is held at a fixed position in the deep large depression 2c, so that a reproducible analysis can be performed. The effect is remarkable.

1 蛍光X線分析用試料保持具
2 高分子フィルム
2a たるみ部
2b 周辺部
2c 窪み部
2d 窪みであった部位
3 筒状固着具
3a 筒状固着具の一方の端部
4 筒状保持具
4a 筒状保持具の一方の端部
10 蛍光X線分析装置
11 X線源
12 1次X線
15 2次X線
16 検出手段
S 液体試料
DESCRIPTION OF SYMBOLS 1 Sample holder 2 for fluorescent X-ray analysis Polymer film 2a Slack part 2b Peripheral part 2c Indented part 2d The part which was a hollow 3 Cylindrical fixing tool 3a One end part 4 of a cylindrical fixing tool Cylindrical holding tool 4a One end 10 of the cylindrical holder X-ray fluorescence analyzer 11 X-ray source 12 Primary X-ray 15 Secondary X-ray 16 Detection means S Liquid sample

Claims (4)

液体試料を蛍光X線分析するために用いられる蛍光X線分析用試料保持具であって、
筒状固着具と、
その筒状固着具の内側に所定の大きさの窪み部を形成するためのたるみ部および前記筒状固着具の一方の端部に沿って固着される周辺部を有する高分子フィルムと、
前記筒状固着具の内径よりも小さい外径を有し、前記筒状固着具の内周に沿ってスライド可能な筒状保持具であって、前記筒状固着具の一方の端部から前記筒状固着具の内側に挿入されて、前記筒状固着具の内周に沿って上方にスライドされて前記高分子フィルムのたるみ部の、前記筒状固着具の内周近傍を押し上げる筒状保持具とを備え、
前記高分子フィルムのたるみ部が下方に押し下げられることにより形成される窪み部に液体試料が滴下乾燥され、前記筒状保持具が前記筒状固着具の内周に沿って上方にスライドされ、前記筒状保持具の一方の端部によって前記たるみ部が平坦にされる位置で支持されるとともに乾燥された試料を保持する蛍光X線分析用試料保持具。
A sample holder for X-ray fluorescence analysis used for X-ray fluorescence analysis of a liquid sample,
A cylindrical fastener,
A polymer film having a slack portion for forming a recessed portion of a predetermined size inside the cylindrical fixing tool and a peripheral portion fixed along one end of the cylindrical fixing tool;
A cylindrical holder having an outer diameter smaller than an inner diameter of the cylindrical fastener, and slidable along an inner periphery of the cylindrical fastener, wherein the cylindrical fastener is disposed from one end of the cylindrical fastener. A cylindrical holder that is inserted inside the cylindrical fixing tool and is slid upward along the inner periphery of the cylindrical fixing tool to push up the slack portion of the polymer film near the inner periphery of the cylindrical fixing tool. With tools,
The liquid sample is dripped and dried into a recess formed by the downward slack of the polymer film being pushed down, and the cylindrical holder is slid upward along the inner periphery of the cylindrical fastener, A sample holder for fluorescent X-ray analysis which holds a dried sample while being supported at a position where the slack portion is flattened by one end of a cylindrical holder.
請求項1に記載の蛍光X線分析用試料保持具を備える蛍光X線分析装置であって、
前記窪み部に液体試料が滴下乾燥され、前記筒状保持具によって前記たるみ部が平坦にされて試料を保持した前記窪み部であった部位に1次X線を照射するX線源と、
前記窪み部であった部位から発生する2次X線の強度を測定する検出手段とを備える蛍光X線分析装置。
A fluorescent X-ray analyzer comprising the fluorescent X-ray analysis sample holder according to claim 1,
An X-ray source that irradiates primary X-rays onto a portion of the hollow portion where the liquid sample is dropped and dried in the hollow portion, the slack portion is flattened by the cylindrical holder and the sample is held;
A fluorescent X-ray analyzer comprising: detection means for measuring the intensity of secondary X-rays generated from the portion that was the depression.
蛍光X線分析用試料保持具の作製方法であって、
筒状固着具と高分子フィルムを準備し、
前記筒状固着具の内側に所定の大きさの窪み部を形成するためのたるみ部が生じるように前記筒状固着具の一方の端部に沿って前記高分子フィルムの周辺部を固着し、
前記筒状固着具の内径よりも小さい外径を有し、前記筒状固着具の内周に沿ってスライド可能な筒状保持具を準備し、
前記筒状保持具を前記筒状固着具の一方の端部より内側に挿入し、前記筒状固着具の内周に沿って上方にスライドさせて前記高分子フィルムのたるみ部の、前記筒状固着具の内周近傍を押し上げて前記筒状保持具の一方の端部によって前記たるみ部を平坦にし、
前記筒状保持具を下方にスライドさせ、再度前記高分子フィルムのたるみ部を形成してこのたるみ部を下方に押し下げることにより、滴下される液体試料を保持する窪み部を形成する蛍光X線分析用試料保持具の作製方法。
A method for producing a sample holder for fluorescent X-ray analysis,
Prepare a cylindrical fastener and a polymer film,
The peripheral portion of the polymer film is fixed along one end of the cylindrical fixing tool so that a slack portion for forming a hollow portion of a predetermined size is formed inside the cylindrical fixing tool,
A cylindrical holder having an outer diameter smaller than an inner diameter of the cylindrical fastener, and being slidable along an inner periphery of the cylindrical fastener;
The cylindrical holder is inserted inside one end of the cylindrical fixing tool, and is slid upward along the inner periphery of the cylindrical fixing tool, so that the cylindrical portion of the slack portion of the polymer film is Pushing up the vicinity of the inner periphery of the fastener to flatten the slack portion by one end of the cylindrical holder,
Fluorescent X-ray analysis that slides down the cylindrical holder, forms a sagging portion of the polymer film again, and pushes the sagging portion downward to form a hollow portion that holds the dropped liquid sample. Method for preparing a sample holder.
請求項1に記載の蛍光X線分析用試料保持具を用いる蛍光X線分析方法であって、
前記窪み部に液体試料を滴下乾燥させ、
前記筒状保持具によって前記たるみ部を平坦にする位置で支持するとともに、前記窪み部であった部位に乾燥された試料を保持させ、
前記窪み部であった部位に1次X線を照射して、発生する2次X線の強度を測定する蛍光X線分析方法。
A fluorescent X-ray analysis method using the fluorescent X-ray analysis sample holder according to claim 1,
A liquid sample is dropped and dried in the recess,
While supporting the slack portion at a position flattened by the cylindrical holder, and holding the dried sample in the portion that was the depression,
A fluorescent X-ray analysis method for measuring the intensity of secondary X-rays generated by irradiating primary X-rays to the portion that was the depression.
JP2009241519A 2009-10-20 2009-10-20 Sample holder for fluorescent x-ray analysis, and method and device of fluorescent x-ray analysis using the same Pending JP2011089794A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2021001778A (en) * 2019-06-20 2021-01-07 住友金属鉱山株式会社 Filter paper pedestal
WO2022003850A1 (en) * 2020-07-01 2022-01-06 株式会社島津製作所 X-ray analysis apparatus

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2021001778A (en) * 2019-06-20 2021-01-07 住友金属鉱山株式会社 Filter paper pedestal
JP7188288B2 (en) 2019-06-20 2022-12-13 住友金属鉱山株式会社 filter paper tray
WO2022003850A1 (en) * 2020-07-01 2022-01-06 株式会社島津製作所 X-ray analysis apparatus
TWI787821B (en) * 2020-07-01 2022-12-21 日商島津製作所股份有限公司 X-ray analysis device

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