JP4398901B2 - Sample holder for fluorescent X-ray analysis and fluorescent X-ray analysis method and apparatus using the same - Google Patents

Sample holder for fluorescent X-ray analysis and fluorescent X-ray analysis method and apparatus using the same Download PDF

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JP4398901B2
JP4398901B2 JP2005136884A JP2005136884A JP4398901B2 JP 4398901 B2 JP4398901 B2 JP 4398901B2 JP 2005136884 A JP2005136884 A JP 2005136884A JP 2005136884 A JP2005136884 A JP 2005136884A JP 4398901 B2 JP4398901 B2 JP 4398901B2
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sample
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frame
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正道 森
未知子 井上
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Rigaku Corp
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Description

本発明は、分析試料の含有成分を蛍光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 components contained in an analysis sample, and a fluorescent X-ray analysis method and apparatus using the same.

従来、分析試料の含有成分を蛍光X線分析するための技術として、液体試料を保持するためのフィルムを用いる蛍光X線分析用試料容器を利用する分析方法がある(特許文献1参照)。このような蛍光X線分析方法では、フィルムを用いる液体試料容器90(図8)が用いられている。図9に示すように、この容器は内外二重の筒状セルのうち内側セル91の一端面にフィルム93の中央部を宛がい、その周囲を内側セル91の周囲に沿わせたうえ、フィルム93で包まれた内側セル91の先端を外側セル92の一端から挿入し、内側セル91の先端が外側セル92の突条(クランプ部)88に達すると、この突条88が内側セル91を包むようになっているフィルム93を内側セル91の外周面との間に挟みつけ、フィルム93は内側セル91の一端側に所定の張力で張られた状態となる。フィルム93が張られた端面を底にして、上方より液体試料94がホルダ90に注がれ保持される。この状態で下側から1次X線が照射され蛍光X線分析がなされる。   Conventionally, as a technique for X-ray fluorescence analysis of components contained in an analysis sample, there is an analysis method using a sample container for X-ray fluorescence analysis using a film for holding a liquid sample (see Patent Document 1). In such a fluorescent X-ray analysis method, a liquid sample container 90 (FIG. 8) using a film is used. As shown in FIG. 9, the container has a central portion of the film 93 that is directed to one end surface of the inner cell 91 among the inner and outer double cylindrical cells, and the periphery of the container is aligned with the periphery of the inner cell 91. 93, the tip of the inner cell 91 is inserted from one end of the outer cell 92, and when the tip of the inner cell 91 reaches the protrusion (clamp portion) 88 of the outer cell 92, the protrusion 88 The film 93 that is to be wrapped is sandwiched between the outer peripheral surface of the inner cell 91 and the film 93 is stretched to one end side of the inner cell 91 with a predetermined tension. The liquid sample 94 is poured into the holder 90 and held from above with the end face on which the film 93 is stretched as the bottom. In this state, primary X-rays are irradiated from the lower side, and fluorescent X-ray analysis is performed.

このような試料保持方法では液体試料94を直接、ホルダ90に入れるため容器の内面に液体試料94が付着し、他の試料を分析する場合には、必ずホルダ90を洗浄しなければならず手間がかかる。フィルムをホルダに張る際にフィルムに皺が寄ったり、不均一な張力になったりすることにより、液体試料が漏れ、測定装置、ホルダ、測定装置の周辺、測定者の手などを汚染させる不具合が生じる。測定面が皺になったり、不均一な張力による弛みになったりすると試料毎の測定面の高さ位置が異なり分析精度が悪なる。特に、この作業に慣れていない測定者の場合には、このような不具合が起こり易い。   In such a sample holding method, since the liquid sample 94 is directly put into the holder 90, the liquid sample 94 adheres to the inner surface of the container, and when analyzing other samples, the holder 90 must be washed. It takes. When the film is stretched on the holder, the film may be wrinkled or uneven tension may cause the liquid sample to leak, contaminating the measuring device, the holder, the periphery of the measuring device, the operator's hand, etc. Arise. If the measurement surface becomes wrinkled or becomes slack due to non-uniform tension, the height of the measurement surface varies from sample to sample, resulting in poor analysis accuracy. In particular, in the case of a measurer who is not used to this work, such a problem is likely to occur.

上記の試料保持方法を改良したものとして、液体試料を保持するための2枚のフィルムを用いる蛍光X線分析用液体試料容器(図10)を利用する分析方法がある。図11(A)に示すように、この試料容器80は以下のような手順で組み立てられる。内側セル81の一端を上向きに立てその上方に1枚目のフィルム83を被せ、1枚目のフィルム83を内側セル81の開口部82の内部へ押し込み窪み部84を形成する。次に図11(B)のように、窪み部84に液体試料85を注入する。図11(C)のように液体試料85が入った窪み部84の開口を覆うように、上から2枚目のフィルム86を被せ、さらにその上から一端側を下にした外側セル87を被せるようにして、1枚目のフィルム83で包まれた内側セル81を外側セル87に挿入する。図11(D)に示すように、挿入に伴って内側セル81の先端が外側セル87の突条(クランプ部)88に達すると、この突条88が内側セル81を包むようになっている二重のフィルムを内側セル81の外周面との間に挟みつけ、外側のフィルム86は内側セル81の一端側に所定の張力で張られた状態となる。これにより、窪み部84が密閉され、ホルダ80が組み立てられる。   As an improvement of the above-described sample holding method, there is an analysis method using a liquid sample container for fluorescent X-ray analysis (FIG. 10) using two films for holding a liquid sample. As shown in FIG. 11A, the sample container 80 is assembled in the following procedure. One end of the inner cell 81 is faced upward, and a first film 83 is placed thereon, and the first film 83 is pushed into the opening 82 of the inner cell 81 to form a recess 84. Next, as shown in FIG. 11B, a liquid sample 85 is injected into the recess 84. As shown in FIG. 11 (C), a second film 86 is covered from the top so as to cover the opening of the recess 84 containing the liquid sample 85, and an outer cell 87 with one end side down from above is covered. In this manner, the inner cell 81 wrapped with the first film 83 is inserted into the outer cell 87. As shown in FIG. 11 (D), when the tip of the inner cell 81 reaches the protrusion (clamping portion) 88 of the outer cell 87 with the insertion, the protrusion 88 wraps the inner cell 81. A heavy film is sandwiched between the outer peripheral surface of the inner cell 81 and the outer film 86 is stretched to one end side of the inner cell 81 with a predetermined tension. Thereby, the hollow part 84 is sealed and the holder 80 is assembled.

このようにしてホルダが組み立てられたら、このホルダを上下ひっくり返し、フィルムが張られた側を下向きにし、下側からX線を照射し蛍光X線分析を行う。
特開平7−134082号公報
When the holder is assembled in this manner, the holder is turned upside down, the side on which the film is stretched is directed downward, and X-rays are irradiated from the lower side to perform fluorescent X-ray analysis.
Japanese Patent Laid-Open No. 7-134082

しかし、前記のような1枚または2枚のフィルムを用いて液体試料容器に測定者自らがフィルムを張る試料保持具では、X線が照射される測定面のフィルムを皺なく均一に引っ張られた状態に組み上げるには熟練を要する。図11(B)に示されているように、液体試料85を最初に保持する1枚目のフィルム83は内側セルの開口部の内部へ押し込み窪み部84を作るときに、内側セル81の全周にわたって皺が形成される。そのため、2枚目のフィルム86を内側セル81に被せて外側セル87を挿入すると内側セル81の全周にわたって形成された皺により、2枚目のフィルム86に皺が寄ったり、不均一な張力になったりすることがある(図11(D))。特に、この作業に慣れていない非熟練者の場合には、このような不具合が起こり易い。2枚目のフィルム86に皺が寄っていると液体試料が漏れるなどの不具合が生じる。   However, in the sample holder in which the measurer himself stretches the film on the liquid sample container using one or two films as described above, the film on the measurement surface irradiated with X-rays was pulled evenly. It takes skill to assemble into a state. As shown in FIG. 11 (B), the first film 83 that initially holds the liquid sample 85 is pushed into the opening of the inner cell to form the depression 84, and the entire inner cell 81 is completely removed. A wrinkle is formed over the circumference. Therefore, when the second film 86 is put on the inner cell 81 and the outer cell 87 is inserted, wrinkles formed over the entire circumference of the inner cell 81 may cause wrinkles on the second film 86 or uneven tension. (FIG. 11D). In particular, such an inconvenience is likely to occur in the case of a non-expert who is not used to this work. If the second film 86 is wrinkled, problems such as leakage of the liquid sample occur.

従来の試料保持具では、測定者自らが試料容器に1枚または2枚のフィルムを液体試料85、94が漏れないように張らなければならない。また、試料容器80,90に液体試料85、94を注ぎ込んだ後、図8、10に示した状態で装置にセットされる。そうすると、1次X線が照射される測定面89には、液体試料85、94の液面高さに応じた圧力が加わる。その結果、フィルム83,86,93に皺ができることによってフィルム93と内側セル91との間や1枚目のフィルム83と2枚目のフィルム86との間に僅かな間隙がクランプ位置にでき、液体試料の液面高さがフィルムのクランプ位置よりも高くなっていると、液体試料圧力とクランプ位置にできた僅かな間隙の圧力との差圧作用により、クランプ位置にできた僅かな間隙から液体試料85,94が漏れ出す。   In the conventional sample holder, the measurer himself must stretch one or two films into the sample container so that the liquid samples 85 and 94 do not leak. Moreover, after pouring the liquid samples 85 and 94 into the sample containers 80 and 90, they are set in the apparatus in the state shown in FIGS. Then, a pressure corresponding to the liquid surface height of the liquid samples 85 and 94 is applied to the measurement surface 89 irradiated with the primary X-rays. As a result, by forming wrinkles on the films 83, 86, 93, a slight gap can be formed between the film 93 and the inner cell 91 or between the first film 83 and the second film 86 at the clamp position. If the liquid level of the liquid sample is higher than the clamp position of the film, the differential pressure action between the liquid sample pressure and the slight gap pressure at the clamp position will cause a slight gap at the clamp position. Liquid samples 85 and 94 leak out.

そのため、測定装置、試料容器、測定装置の周辺、測定者の手などを汚染させる不具合が生じる。測定面が皺になったり、不均一な張力による弛みになったりすると試料毎の測定面の高さが異なり分析精度が悪化する。   For this reason, there arises a problem that the measuring device, the sample container, the periphery of the measuring device, the hand of the measurer, etc. are contaminated. If the measurement surface becomes wrinkled or becomes slack due to non-uniform tension, the height of the measurement surface varies from sample to sample and the analysis accuracy deteriorates.

測定後、試料を回収し試料容器を再度利用するためにフィルムを試料容器から取り除く作業を行う必要がある。しかし、従来の試料容器では突条(クランプ部)を有しているため、フィルムを試料容器から取り除く時に、試料容器に傷を付けたり、2枚のフィルムを使用する場合でも、試料容器を試料で汚染させるなどして、再度、試料容器を使用できなくなる場合がある。   After the measurement, it is necessary to remove the film from the sample container in order to collect the sample and reuse the sample container. However, since the conventional sample container has a protrusion (clamp part), even when the film is removed from the sample container, even if the sample container is damaged or two films are used, the sample container is In some cases, the sample container cannot be used again due to contamination.

本発明は前記従来の問題に鑑みてなされたもので、試料の含有成分を蛍光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、液体だけでなく粉体や固体試料の分析作業の効率化と簡易化を図るとともに、試料毎の測定面の高さ位置を測定面全面にわたって同一にすることにより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 component contained in a sample, and a fluorescent X-ray analysis method and apparatus using the same, The purpose is to improve the analysis accuracy by making the measurement surface of each sample not only the liquid but also the efficiency and simplification of the analysis work of the powder and solid sample, and making the height of the measurement surface for each sample the same over the entire measurement surface. To do.

前記目的を達成するために、本発明の第1構成にかかる蛍光X線分析用試料保持具は、試料に下方から1次X線を照射して蛍光X線分析するために用いられるものであって、枠体と、その枠体に付着された付着部、前記枠体の外周よりも外側の外周部および前記枠体の内周よりも内側でX線を透過させるための透過部を有するフィルムとを備え試料を保持する。   In order to achieve the above object, the sample holder for fluorescent X-ray analysis according to the first configuration of the present invention is used for fluorescent X-ray analysis by irradiating a sample with primary X-rays from below. And a film having a frame, an attachment portion attached to the frame, an outer peripheral portion outside the outer periphery of the frame body, and a transmission portion for transmitting X-rays inside the inner periphery of the frame body And hold the sample.

本発明の第1構成によれば、試料測定面を構成するフィルムが枠体に皺のない状態で均一な張力で張られているので、測定者自らがフィルムを張ることなく試料毎の測定面の高さ位置を測定面全面にわたって同一にすることにより分析精度を向上させることができる。したがって、測定試料の準備に熟練度を必要としない。また、本発明の第1構成によれば、試料は1枚のフィルム、または1枚のフィルムとフィルムに付着された枠体のみに接触するので、従来技術のようにフィルムとホルダとの間や2枚のフィルムの間に間隙が形成されることはなく、クランプ部に液体試料の圧力がかからず、液体試料圧力とクランプ位置にできた僅かな間隙の圧力との差圧作用により、クランプ位置にできた僅かな間隙から液体試料が漏れ出すことはない。   According to the first configuration of the present invention, since the film constituting the sample measurement surface is stretched with a uniform tension without any wrinkles on the frame, the measurement surface for each sample is not stretched by the measurer himself. The analysis accuracy can be improved by making the height position of the same over the entire measurement surface. Therefore, skill is not required for the preparation of the measurement sample. In addition, according to the first configuration of the present invention, the sample contacts only one film or one film and a frame attached to the film. A gap is not formed between the two films, and the pressure of the liquid sample is not applied to the clamp part, and the pressure difference between the liquid sample pressure and the slight gap pressure formed at the clamp position causes the clamp. The liquid sample does not leak from the slight gap formed at the position.

本発明の第1構成においては、枠体は1mm程度の厚みを有するポリプロピレン、ポリエチレンテレフタレート(PET)を用いるのが好ましく、枠体が付着されるフィルムには、ポリエステル(例えばポリエチレンテレフタレート)、ポリプロピレンまたはポリイミドを用いるのが好ましい。枠体とフィルムの付着部との付着にはプラスチックフィルムを接着できる接着剤を用いる方法や熱溶着や超音波溶着などの付着方法であればよく、特に方法を問わない。   In the first configuration of the present invention, it is preferable to use polypropylene and polyethylene terephthalate (PET) having a thickness of about 1 mm for the frame, and for the film to which the frame is attached, polyester (for example, polyethylene terephthalate), polypropylene or It is preferable to use polyimide. The attachment of the frame and the attachment portion of the film is not particularly limited as long as it is a method using an adhesive capable of adhering a plastic film, or an attachment method such as thermal welding or ultrasonic welding.

本発明の第2構成にかかる蛍光X線分析方法は、前記第1構成の蛍光X線分析用試料保持具と下部にX線を通過させるための開口を有する筒状のホルダとを用いるものであって、前記透過部が前記ホルダの開口を覆い、前記外周部が前記ホルダの側部の内面を覆うように、前記蛍光X線分析用試料保持具を前記ホルダに装着し、上方から液体または粉体試料を注いで、前記透過部を介して前記試料に下方から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 according to the second configuration of the present invention uses the fluorescent X-ray analysis sample holder of the first configuration and a cylindrical holder having an opening for allowing X-rays to pass therethrough. The fluorescent X-ray analysis sample holder is mounted on the holder so that the transmission part covers the opening of the holder and the outer peripheral part covers the inner surface of the side part of the holder, and the liquid or A powder sample is poured, and the sample is irradiated with primary X-rays from below through the transmission part, and the intensity of the generated secondary X-rays is measured.

本発明の第3構成にかかる蛍光X線分析装置は、前記第1構成の蛍光X線分析用試料保持具を用いるものであって、試料を保持した前記蛍光X線分析用試料保持具の透過部を介して、前記試料に下方から1次X線を照射するX線源と、前記試料から発生する2次X線の強度を測定する検出手段とを備える。   A fluorescent X-ray analysis apparatus according to a third configuration of the present invention uses the fluorescent X-ray analysis sample holder of the first configuration, and is transmitted through the fluorescent X-ray analysis sample holder holding a sample. And an X-ray source for irradiating the sample with primary X-rays from below and a detecting means for measuring the intensity of secondary X-rays generated from the sample.

本発明の第2、第3構成によれば、前記第1構成の蛍光X線分析用試料保持具を用いるので、第1構成と同様の作用効果が得られる。   According to the second and third configurations of the present invention, since the sample holder for fluorescent X-ray analysis of the first configuration is used, the same effects as the first configuration can be obtained.

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。この試料保持具は、試料の含有成分を蛍光X線分析するために用いられるものであって、図1に示すように、試料を保持するX線透過性フィルムを安定に保持するための例えば、ポリプロピレン、ポリエチレンテレフタレート(PET)などの樹脂材料からなる輪状の枠体2と、その枠体にプラスチック用接着剤で付着された付着部1a、その枠体2の外周よりも外側の外周部1cおよび前記枠体の内周よりも内側でX線を透過させるための透過部1bを有する厚さ10μm未満の例えばポリエステル(例えばポリエチレンテレフタレート)、ポリプロピレンまたはポリイミドなどの樹脂材料からなるフィルム1を備え、下部にX線を通過させるための開口7を有する円筒状のホルダ6に、透過部1bがホルダ6の開口7を覆い、外周部1cがホルダ6の側部の内面を覆うように装着されることにより、上方から注がれた液体試料9を保持する。   Hereinafter, the sample holder for fluorescent X-ray analysis which is 1st Embodiment of this invention is demonstrated. This sample holder is used for fluorescent X-ray analysis of the components contained in the sample, and as shown in FIG. 1, for example, for stably holding an X-ray transmissive film for holding a sample, An annular frame 2 made of a resin material such as polypropylene or polyethylene terephthalate (PET), an attachment portion 1a attached to the frame with an adhesive for plastic, an outer peripheral portion 1c outside the outer periphery of the frame 2, and Provided with a film 1 made of a resin material such as polyester (for example, polyethylene terephthalate), polypropylene, or polyimide having a thickness of less than 10 μm and having a transmission part 1b for transmitting X-rays inside the inner periphery of the frame, A transparent holder 1b covers the opening 7 of the holder 6 on the cylindrical holder 6 having an opening 7 for allowing X-rays to pass through the outer periphery 1c. By being mounted so as to cover the inner surface of the side of the holder 6, for holding a liquid sample 9 which was poured from above.

本実施形態の試料保持具5は、輪状の枠体2の内外周と円筒状のホルダ6の側部の内径とが同心状に装着して使用されるものであるので、輪状の枠体2の外周の直径は使用される円筒状のホルダ6の側部の内径より少し小さいことが望ましく、輪状の枠体2の内周の直径は試料を測定するのに充分なX線が透過できる径であることが望ましいので、枠体2の外内周の直径は所定のホルダ6の側部の内径と開口7の直径に適合した所定の寸法のものであればよい。試料9を保持するX線透過性フィルム1を安定に保持するため枠体2は、耐薬品性および使用後の廃棄処理を考慮すると、例えばポリプロピレン、ポリエチレンテレフタレート(PET)などの樹脂材料がよい。また、フィルムを安定に保持するための厚みは0.5mm以上、2mm以下の厚みを有することが望ましく、1mm程度がより望ましい。   Since the sample holder 5 of the present embodiment is used in such a manner that the inner and outer circumferences of the ring-shaped frame 2 and the inner diameter of the side portion of the cylindrical holder 6 are mounted concentrically, the ring-shaped frame 2 is used. The diameter of the outer circumference of the cylindrical holder 6 is preferably slightly smaller than the inner diameter of the side of the cylindrical holder 6 to be used, and the diameter of the inner circumference of the ring-shaped frame 2 is a diameter that can transmit X-rays sufficient to measure the sample. Therefore, the outer diameter of the outer periphery of the frame body 2 may be of a predetermined size that matches the inner diameter of the side of the predetermined holder 6 and the diameter of the opening 7. In order to stably hold the X-ray transmissive film 1 holding the sample 9, the frame 2 is preferably made of a resin material such as polypropylene or polyethylene terephthalate (PET) in consideration of chemical resistance and disposal after use. The thickness for stably holding the film is preferably 0.5 mm or more and 2 mm or less, more preferably about 1 mm.

図2に試料保持具5の上面図を示すように、枠体2は外周の直径d2が40mm、内周の直径d1が30mm、厚みが1mmであるポリプロピレンであり、枠体2の内周の中心位置が厚さ6μm、直径(図2のd3)90mmの円形のポリエチレンテレフタレートフィルム1の中心部に位置するようにプラスチック用付着剤でフィルム1の付着部1aに付着され枠体2の外周よりも外側の外周部1cおよび枠体2の内周よりも内側でX線を透過させるための透過部1bが構成されている。   As shown in the top view of the sample holder 5 in FIG. 2, the frame 2 is polypropylene having an outer diameter d2 of 40 mm, an inner diameter d1 of 30 mm, and a thickness of 1 mm. From the outer periphery of the frame 2 and attached to the attachment part 1a of the film 1 with an adhesive for plastic so that the center position is located in the center of the circular polyethylene terephthalate film 1 having a thickness of 6 μm and a diameter (d3 in FIG. 2) of 90 mm. In addition, a transmission portion 1b for transmitting X-rays is formed inside the outer peripheral portion 1c and the inner periphery of the frame 2 inside.

フィルム1と枠体2の付着には、例えば、スプレーのり(成分はアクリルゴム(10%)、有機溶剤(54%)およびイソヘキサンガス(36%)で、噴射用高圧ガスはジメチルエーテル)を枠体の裏に吹き付けて、フィルム1の中央部に貼付されている。貼付に用いる接着剤は、このスプレーのりに限らず、分析の障害とならないものであればよい。図3に示すように、枠体2の下部全面がフィルム1に付着され付着部1aを構成している。なお、図示と理解の容易のため、図で表した各部の厚さは実際の寸法とは異なる。   For attachment of the film 1 and the frame 2, for example, spray paste (components are acrylic rubber (10%), organic solvent (54%) and isohexane gas (36%), high-pressure gas for injection is dimethyl ether) It is sprayed on the back of the body and stuck to the center of the film 1. The adhesive used for sticking is not limited to this spray paste, and any adhesive that does not hinder analysis can be used. As shown in FIG. 3, the entire lower surface of the frame 2 is attached to the film 1 to form an attachment portion 1 a. For ease of illustration and understanding, the thickness of each part shown in the figure is different from the actual dimension.

図1に示すように、この試料保持具5は下部にX線を通過させるための開口7を有する円筒状のホルダ6、例えば、従来から蛍光X線分析に使用されている底部6aを有する下面照射用液体ホルダ6に、枠体2がフィルム1の下方に位置して、透過部1bが枠体2の内周部とともにホルダの開口7を覆い、外周部1cがホルダ6の側部の内面を覆うように装着されることにより、上方から注がれた液体試料9を保持する。   As shown in FIG. 1, the sample holder 5 has a cylindrical holder 6 having an opening 7 for allowing X-rays to pass therethrough, for example, a lower surface having a bottom 6a conventionally used for fluorescent X-ray analysis. In the irradiation liquid holder 6, the frame 2 is positioned below the film 1, the transmission part 1 b covers the opening 7 of the holder together with the inner peripheral part of the frame 2, and the outer peripheral part 1 c is the inner surface of the side part of the holder 6. The liquid sample 9 poured from above is held.

上記例では試料保持具の枠体2を輪状のものについて説明したが、輪状のものに限らず試料を安定に保持でき、試料を測定するのに充分なX線が透過できる透過部1bを有する構造であれば多角形や楕円形などの枠体でもよく、枠体の内外周の大きさや厚みなどについても輪状のものと同程度のものであればよい。   In the above example, the frame body 2 of the sample holder has been described as having a ring shape. As long as it has a structure, it may be a frame such as a polygon or an ellipse, and the size and thickness of the inner and outer peripheries of the frame may be the same as those of a ring.

上記例では試料保持具の外周部1cを円形のものを図示したが、試料保持具の外周部1cの外縁部をホルダの上部の開放部8に固定できればよいものであるので、円形である必要はなく、例えば楕円や多角形などのものであってもよい。また、試料保持具の円形の直径を90mmとしたが、試料保持具の外周部1cは試料の保持作業が容易にできる大きさのものであればよい。   In the above example, the outer peripheral portion 1c of the sample holder is shown in a circular shape, but it is only necessary to fix the outer edge portion of the outer peripheral portion 1c of the sample holder to the open portion 8 at the upper part of the holder, and therefore it needs to be circular. For example, it may be an ellipse or a polygon. In addition, although the circular diameter of the sample holder is 90 mm, the outer peripheral portion 1c of the sample holder may be of a size that can easily hold the sample.

上記例ではホルダ6に底部6aを有するものを図示したが、試料保持具5の透過部1aが底部を有さない筒状のホルダの開口を覆い、試料保持具5の外周部1cが底部を有さない筒状のホルダの側部の内面を覆うように、試料保持具5の底部を有さない筒状のホルダに装着し試料を保持してもよい。本実施形態では、円筒状のホルダ6について説明したが、楕円筒や角筒などの筒状のものでもよく、試料保持具5の枠体2の形状に適合した形状のホルダを用いるのが望ましい。   In the above example, the holder 6 having the bottom 6a is illustrated, but the transmission part 1a of the sample holder 5 covers the opening of the cylindrical holder that does not have the bottom, and the outer peripheral part 1c of the sample holder 5 covers the bottom. The sample may be held by attaching it to a cylindrical holder that does not have the bottom of the sample holder 5 so as to cover the inner surface of the side of the cylindrical holder that does not have. In the present embodiment, the cylindrical holder 6 has been described. However, a cylindrical holder such as an elliptic cylinder or a rectangular cylinder may be used, and it is desirable to use a holder having a shape that matches the shape of the frame 2 of the sample holder 5. .

上記では、円筒状のホルダ6に、枠体2がフィルム1の下方に位置して、透過部1bが枠体2の内周部とともにホルダの開口7を覆い、外周部1cがホルダ6の側部の内面を覆うように装着した例を示したが、図4に示すように、ホルダ6に、枠体2がフィルム1の上方に位置して、透過部1bがホルダの開口7を覆い、外周部1cがホルダ6の側部の内面を覆うように装着した例について以下に説明する。   In the above, the frame 2 is positioned below the film 1 on the cylindrical holder 6, the transmission part 1 b covers the opening 7 of the holder together with the inner peripheral part of the frame 2, and the outer peripheral part 1 c is on the holder 6 side. As shown in FIG. 4, the frame 2 is positioned above the film 1 and the transmission part 1b covers the opening 7 of the holder, as shown in FIG. An example in which the outer peripheral portion 1c is mounted so as to cover the inner surface of the side portion of the holder 6 will be described below.

枠体2がフィルム1の上方に位置するように装着すると、枠体2がフィルム1の下方に位置するように装着した場合に比べ、試料9の測定面である透過部1bと1次X線21との距離が枠体2の厚みの距離だけ近づき試料9から発生する2次X線22の強度が増大し、分析感度が向上する。より高感度の分析を望む場合に適した例である。   When the frame 2 is mounted so as to be positioned above the film 1, the transmission portion 1 b that is the measurement surface of the sample 9 and the primary X-ray are compared with the case where the frame 2 is mounted so as to be positioned below the film 1. The intensity of the secondary X-rays 22 generated from the sample 9 increases as the distance from 21 approaches the distance of the thickness of the frame 2, and the analysis sensitivity is improved. This is an example suitable for a case where higher sensitivity analysis is desired.

その反面、枠体2をフィルム1の上方に位置するように装着した場合は、枠体2が液体試料9と接触する。また、付着部1aを接着剤で付着した場合には、測定する液体試料の種類によっては液体試料9が付着部1aと枠体2の間に浸透し接着剤中の成分を溶出させ、その成分が測定対象元素に影響を与えることが考えられる。したがって、この場合には分析開始前に測定する試料の内容や測定対象元素を検討する必要がある。特に、測定対象元素に影響を与える可能性の低い水溶液性の試料の分析に用いるのが好ましい。枠体を接着剤を用いず熱溶着や超音波溶着で付着させた場合には、上記のような配慮は不要となる。   On the other hand, when the frame 2 is mounted so as to be positioned above the film 1, the frame 2 comes into contact with the liquid sample 9. When the adhering portion 1a is adhered with an adhesive, depending on the type of liquid sample to be measured, the liquid sample 9 permeates between the adhering portion 1a and the frame 2 and elutes the components in the adhesive. May affect the element to be measured. Therefore, in this case, it is necessary to examine the content of the sample and the element to be measured before starting the analysis. In particular, it is preferably used for analysis of an aqueous sample having a low possibility of affecting the measurement target element. When the frame is attached by thermal welding or ultrasonic welding without using an adhesive, the above consideration is not necessary.

試料9が気化し易い試料であったり、試料の気化ガスによって測定装置が汚染されたり、腐食されたりする場合や液体試料を注ぎ込んだホルダ6の搬送時に液体試料を溢すなどの心配がある場合には、試料の気化ガスや液体試料がこぼれないようにホルダ上部の開放部8に図5に示すように、ガス抜きキャップや多孔質膜14などの通気性のある材料などを保持した蓋16でホルダ上部の開放部8を覆うことが望ましい。より確実に試料保持具の外周部1cをホルダ6の側部上面で固定する必要がある場合には、第2実施形態で説明する膜押さえ37(図7参照)を蓋16と共に用いてもよい。蓋16が不要な場合には、膜押さえ37のみを用いてより確実に外周部1cを固定してもよい。   When the sample 9 is an easily vaporized sample, the measurement device is contaminated or corroded by the vaporized gas of the sample, or the liquid sample overflows when the holder 6 into which the liquid sample is poured is transported As shown in FIG. 5, a lid 16 holding a gas permeable material such as a gas vent cap or a porous membrane 14 in the opening 8 at the top of the holder so that the vaporized gas or liquid sample of the sample does not spill. It is desirable to cover the opening 8 at the top of the holder. When it is necessary to more securely fix the outer peripheral portion 1c of the sample holder on the side surface of the holder 6, the film presser 37 (see FIG. 7) described in the second embodiment may be used together with the lid 16. . When the lid 16 is not necessary, the outer peripheral portion 1c may be more securely fixed using only the film presser 37.

上記では、試料保持具5では筒状のホルダを用いて試料を保持することについて説明したが、筒状のホルダを用いず試料保持具のみで試料を保持してもよい。試料保持具5の透過部1bに微量の液体や少量のゲル状物や粉体の試料などを載せ、試料を包み込むように試料の上方で試料保持具5の外周部1cをクリップ等で止め試料を保持する。また、蛍光X線分析装置の試料ターレットや試料測定部の試料を載置する凹状の窪みの底部に試料保持具5の枠体2を上方より合わせ、試料保持具5の外周部1cが試料を載置する凹状の窪みの側部の内面を覆うように、試料保持具5を装着し、上方より液体や粉体の試料を注ぎ込み試料の上方で試料保持具5の外周部1cをクリップ等で止め試料を保持してもよい。上記したように本発明の試料保持具は液体試料だけではなく、ゲル状体、粉体、固体などの試料を保持するものである。   In the above description, the sample holder 5 holds the sample using the cylindrical holder. However, the sample holder may be held only by the sample holder without using the cylindrical holder. A small amount of liquid, a small amount of gel or powder sample is placed on the transmission part 1b of the sample holder 5, and the outer peripheral part 1c of the sample holder 5 is stopped with a clip or the like above the sample so as to wrap the sample. Hold. In addition, the frame 2 of the sample holder 5 is aligned with the bottom of the concave recess on which the sample turret of the fluorescent X-ray analyzer or the sample of the sample measurement unit is placed, and the outer peripheral portion 1c of the sample holder 5 holds the sample. A sample holder 5 is mounted so as to cover the inner surface of the side of the concave recess to be placed, a liquid or powder sample is poured from above, and the outer peripheral portion 1c of the sample holder 5 is clipped or the like above the sample. A stop sample may be held. As described above, the sample holder of the present invention holds not only a liquid sample but also a sample such as a gel-like body, powder, or solid.

本発明の試料保持具5の透過部1bでは試料測定面を構成するフィルム1が枠体2に皺のない状態で、均一な張力で張られているので、従来技術のように試料容器の透過部としてフィルムを測定者自らが皺のない状態で張ったり、均一な張力で張るという作業をすることなく、試料保持具5を円筒状のホルダ6に装着し、ホルダ6の上方から試料9を注ぎ込みホルダ6の上下をひっくり返すことなく、そのまま蛍光X線分析装置にセットすれば測定を行うことができ、分析作業の簡易化が図れる。試料測定面を構成する透過部1bのフィルム1が枠体2に皺のない状態で、均一な張力で張られており、試料毎の測定面の高さ位置を測定面全面にわたって同一にすることができ、測定者は熟練を要さずに高精度の分析を行うことができる。   In the transmission part 1b of the sample holder 5 of the present invention, the film 1 constituting the sample measurement surface is stretched with a uniform tension without any wrinkles on the frame body 2, so that the transmission of the sample container is performed as in the prior art. The sample holder 5 is attached to the cylindrical holder 6 and the sample 9 is attached from the upper side of the holder 6 without performing the work of stretching the film by the measurer himself without any wrinkles or even tension. The measurement can be performed by setting it in the fluorescent X-ray analyzer as it is without turning the pouring holder 6 upside down, and the analysis work can be simplified. The film 1 of the transmission part 1b constituting the sample measurement surface is stretched with a uniform tension in a state where there is no wrinkle on the frame 2, and the height position of the measurement surface for each sample is made the same over the entire measurement surface. Therefore, the measurer can perform highly accurate analysis without requiring skill.

また、従来技術のように液体試料を保持する場合に起こる液体試料の漏れについても、本発明の試料保持具5は、液体試料と1枚のフィルム、または1枚のフィルムとフィルムに付着された枠体のみに接触するので、従来技術のようにフィルムとホルダとの間や2枚のフィルムの間に間隙が形成されることはなく、クランプ部に液体試料の圧力がかからず、液体試料圧力とクランプ位置にできた僅かな間隙の圧力との圧力差により、クランプ位置にできた僅かな間隙から液体試料が漏れることはない。上記したように筒状のホルダを用いず試料保持具のみで試料を保持できるので、分析作業の簡易化が図れる。また、本発明の試料保持具は液体試料だけではなく、ゲル状体、粉体、固体などの試料も保持することができる。   In addition, regarding the leakage of the liquid sample that occurs when the liquid sample is held as in the prior art, the sample holder 5 of the present invention is attached to the liquid sample and one film, or one film and film. Since only the frame is contacted, no gap is formed between the film and the holder or between the two films as in the prior art, and the pressure of the liquid sample is not applied to the clamp part. Due to the pressure difference between the pressure and the pressure in the slight gap at the clamping position, the liquid sample does not leak from the slight gap at the clamping position. Since the sample can be held only by the sample holder without using the cylindrical holder as described above, the analysis work can be simplified. Moreover, the sample holder of the present invention can hold not only a liquid sample but also a sample such as a gel-like body, a powder, and a solid.

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40は、本発明の第3実施形態であり、図6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5を用いる装置であって、試料保持具5が直接またはホルダ6を介して載置される試料台である試料ステージ25と、下部にX線を通過させるための開口7を有し、試料保持具の透過部1bが開口7を覆い、試料保持具の外周部1cが円筒状の側部の内面を覆うように装着された円筒状のホルダ6と、円筒状のホルダ6の内部に装着され、上方から注がれた液体試料を保持した試料保持具の透過部1bの部位に1次X線14を照射するX線管などのX線源23と、試料保持具の透過部1bの部位の試料から発生する蛍光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24と、を備えている。   Next, a fluorescent X-ray analysis method according to the second embodiment of the present invention will be described. An X-ray fluorescence analyzer 40 used in this analysis method is the third embodiment of the present invention, and as shown in FIG. 6, is an apparatus using the sample holder 5 for X-ray fluorescence analysis of the first embodiment. The sample holder 5 has a sample stage 25 which is a sample stage placed directly or via the holder 6, and an opening 7 for allowing X-rays to pass therethrough, and the transmission part 1b of the sample holder. Covers the opening 7, and the cylindrical holder 6 mounted so that the outer peripheral portion 1c of the sample holder covers the inner surface of the cylindrical side portion is mounted inside the cylindrical holder 6, and poured from above. Generated from an X-ray source 23 such as an X-ray tube that irradiates a primary X-ray 14 to a portion of the transmission part 1b of the sample holder holding the liquid sample and a sample of the part of the transmission part 1b of the sample holder Detection means 24 such as an X-ray detector for measuring the intensity of secondary X-rays 15 such as fluorescent X-rays; It is equipped with a.

この装置40を使用する第2実施形態の蛍光X線分析方法は、第1実施形態の蛍光X線分析用試料保持具5を用いる方法であって、試料保持具5を散乱X線の発生が少ない樹脂製やアルミニウムまたはチタン等の金属製の円筒状のホルダの開口7を試料保持具5の透過部1bが覆い、試料保持具の外周部1cが円筒状のホルダ6の側部の内面を覆うように装着し、液体や粉体試料を注ぐ作業を容易にするために試料保持具の外周部1cの外縁部をホルダ6の開放部8を構成する側部の上端部で外側に折り曲げ、液体または粉体試料9をホルダ6の上方より注ぎ込み試料保持具5に液体または粉体試料9を保持させ、そのホルダ6を試料ステージ25に載置し、試料保持具の透過部1bを介して試料に下方から1次X線14を照射し、試料から発生する2次X線15の強度を測定する。   The fluorescent X-ray analysis method of the second embodiment using this apparatus 40 is a method using the sample holder 5 for fluorescent X-ray analysis of the first embodiment, and the sample holder 5 generates scattered X-rays. The transparent portion 1b of the sample holder 5 covers the opening 7 of a cylindrical holder made of a small amount of resin or metal such as aluminum or titanium, and the outer peripheral portion 1c of the sample holder covers the inner surface of the side portion of the cylindrical holder 6. In order to facilitate the work of pouring the liquid or powder sample, the outer edge of the outer peripheral portion 1c of the sample holder is folded outward at the upper end of the side portion constituting the open portion 8 of the holder 6, A liquid or powder sample 9 is poured from above the holder 6 to hold the liquid or powder sample 9 in the sample holder 5, and the holder 6 is placed on the sample stage 25, via the transmission part 1 b of the sample holder. Irradiate the sample with primary X-rays 14 from below, Measuring the intensity of green for secondary X-rays 15.

本実施形態では、試料保持具の枠体2を輪状のものについて説明したが、第1実施形態と同様に試料を安定に保持でき、試料を測定するのに充分なX線が透過できる透過部1bを有する構造であれば多角形や楕円形などの枠体でもよく、枠体の内外周の大きさや厚みなどについては輪状のものと同程度のものであればよい。   In the present embodiment, the frame 2 of the sample holder has been described as having a ring shape. However, similarly to the first embodiment, the sample can be stably held, and a transmissive portion that can transmit X-rays sufficient to measure the sample. As long as the structure has 1b, it may be a frame such as a polygon or an ellipse, and the size and thickness of the inner and outer peripheries of the frame may be the same as those of a ring.

本実施形態では、試料保持具の外周部1cを円形のものについて説明したが、第1実施形態と同様に円形である必要はなく、例えば楕円や四角形、多角形などのものであってもよいし、試料保持具の外周部1cは試料の保持作業が容易にできる大きさのものであればよい。   In the present embodiment, the outer peripheral portion 1c of the sample holder has been described as being circular, but it is not necessary to be circular as in the first embodiment, and may be, for example, an ellipse, a rectangle, or a polygon. The outer peripheral portion 1c of the sample holder may be of a size that can easily hold the sample.

第1実施形態と同様に、試料が気化し易い試料であったり、試料の気化ガスによって測定装置が汚染されたり、腐食されたりする場合や液体試料を注ぎ込んだホルダの搬送時に液体試料を溢すなどの心配がある場合には、ホルダ上部の開放部8に図5に示すように、ガス抜きキャップや多孔質膜14などの通気性のある材料などを保持した蓋16でホルダ上部の開放部8を覆うことが望ましい。より確実に試料保持具の外周部1cをホルダ6の側部上面で固定する必要がある場合には、下記する膜押さえ37(図7参照)を蓋16と共に用いてもよい。蓋16が不要な場合には、膜押さえ37のみを用いてより確実に外周部1cを固定してもよい。   Similar to the first embodiment, when the sample is easily vaporized, the measuring device is contaminated or corroded by the vaporized gas of the sample, or the liquid sample overflows when the holder into which the liquid sample is poured is transported When there is a concern, as shown in FIG. 5, the open portion 8 at the top of the holder is covered with a lid 16 that holds a gas-permeable cap or a porous material such as the porous membrane 14. It is desirable to cover 8. When it is necessary to more securely fix the outer peripheral portion 1 c of the sample holder on the side surface of the holder 6, a film presser 37 (see FIG. 7) described below may be used together with the lid 16. When the lid 16 is not necessary, the outer peripheral portion 1c may be more securely fixed using only the film presser 37.

上記例ではホルダ6に底部6aを有するものを図示したが、試料保持具5の透過部1aが底部を有さない筒状のホルダ36(図7参照)の開口を覆い、試料保持具の外周部1cが底部を有さない筒状のホルダ36の側部の内面を覆うように、底部を有さない筒状のホルダ36に試料保持具5を装着し試料9を保持してもよい。底部を有さない筒状のホルダ36に試料保持具5を装着し試料9を保持する方法の一例について以下に説明する。   In the above example, the holder 6 having the bottom 6a is illustrated. However, the transmission part 1a of the sample holder 5 covers the opening of the cylindrical holder 36 (see FIG. 7) that does not have the bottom, and the outer periphery of the sample holder The sample holder 5 may be attached to the cylindrical holder 36 having no bottom so that the sample 9 is held so that the part 1c covers the inner surface of the side of the cylindrical holder 36 having no bottom. An example of a method for attaching the sample holder 5 to the cylindrical holder 36 having no bottom and holding the sample 9 will be described below.

図7(A)に示すように、試料保持具5の輪状の枠体2が下方に位置するように台上(図示していない)に置き、外周部1cを透過部1b方向に折り込み、折り込まれた外周部1cであって付着部1aに隣接する周辺部を輪状の枠体2と試料保持具5の輪状の枠体2の内外周径とほぼ同径の内外周径を有する円筒状のホルダ36の側部下面36aとでサンドイッチ状に挟み込む。挟み込まれていない外周部の部分を円筒状のホルダ36の側部の内面を覆うように試料保持具5を円筒状のホルダ36に装着し、図7(B)に示すように、外周部1cの外縁部をリング状のフィルム押さえ37と円筒状のホルダ36の側部上面36bとで固定し、図7(C)に示すように、液体または粉体試料9をホルダ36の上方より注ぎ込む。その後、空気孔を有するキャップ38でフィルム押さえ37を上方より固定することにより試料保持具5に液体または粉体試料9が保持される。そのホルダ36を試料ステージ25に載置し、試料保持具の透過部1bを介して試料9に下方から1次X線14を照射し、試料9から発生する2次X線15の強度を測定する(図6参照)。   As shown in FIG. 7 (A), the ring-shaped frame 2 of the sample holder 5 is placed on a table (not shown) so as to be positioned below, and the outer peripheral portion 1c is folded in the direction of the transmitting portion 1b. The outer peripheral portion 1c that is adjacent to the adhering portion 1a has a cylindrical shape having an inner and outer peripheral diameter that is substantially the same as the inner and outer peripheral diameters of the annular frame 2 and the annular frame 2 of the sample holder 5. The holder 36 is sandwiched between the side lower surfaces 36a. The sample holder 5 is mounted on the cylindrical holder 36 so that the outer peripheral portion not sandwiched covers the inner surface of the side portion of the cylindrical holder 36, and as shown in FIG. 7B, the outer peripheral portion 1c. The outer edge portion is fixed by the ring-shaped film presser 37 and the side upper surface 36b of the cylindrical holder 36, and the liquid or powder sample 9 is poured from above the holder 36 as shown in FIG. Then, the liquid or powder sample 9 is held by the sample holder 5 by fixing the film presser 37 from above with a cap 38 having air holes. The holder 36 is placed on the sample stage 25, the sample 9 is irradiated with the primary X-ray 14 from below through the transmission part 1b of the sample holder, and the intensity of the secondary X-ray 15 generated from the sample 9 is measured. (See FIG. 6).

本実施形態では、リング状のフィルム押さえ37や空気孔を有するキャップ38の両方を用いたが、キャップ38を用いずにフィルム押さえ37のみを用いてもよいし、キャップ38のみを用いてもよい。   In the present embodiment, both the ring-shaped film press 37 and the cap 38 having air holes are used. However, only the film press 37 may be used without using the cap 38, or only the cap 38 may be used. .

本実施形態では、円筒状のホルダ6、36について説明したが、第1実施形態と同様に楕円筒や角筒などの筒状のものでもよく、試料保持具5の枠体2の形状に適合した筒状のホルダを用いるのが望ましい。   In the present embodiment, the cylindrical holders 6 and 36 have been described. However, similarly to the first embodiment, a cylindrical shape such as an elliptical cylinder or a rectangular cylinder may be used, and the shape of the frame 2 of the sample holder 5 is adapted. It is desirable to use a cylindrical holder.

第1実施形態と同様に、試料保持具5の枠体2がフィルム1の下方に位置するようにホルダ6、36に装着してもよいし、試料保持具5の枠体2がフィルム1の上方に位置するようにホルダ6、36に装着してもよい。   Similarly to the first embodiment, the frame 2 of the sample holder 5 may be attached to the holders 6 and 36 so that the frame 2 of the sample holder 5 is positioned below the film 1. You may mount | wear with the holders 6 and 36 so that it may be located upwards.

以上のように試料ステージ25に載置した試料保持具5またはホルダ6、36に装着されている試料保持具5の透過部1bの部位に1次X線14を照射して、試料9から発生する2次X線15の強度を測定し蛍光X線分析を行う。蛍光X線分析装置40はエネルギー分散型でも波長分散型のどちらの装置であってもよい。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5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。   As described above, the primary X-ray 14 is irradiated to the part of the transmission part 1b of the sample holder 5 mounted on the sample stage 25 or the sample holder 5 mounted on the holders 6 and 36, and generated from the sample 9. The intensity of the secondary X-ray 15 is measured and the fluorescent X-ray analysis is performed. The X-ray fluorescence analyzer 40 may be either an energy dispersion type or a wavelength dispersion type apparatus. According to the method and apparatus of the second and third embodiments, since the fluorescent X-ray analysis sample holder 5 of the first embodiment is used, the same operational effects as those of the first embodiment 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とホルダの断面図である。It is sectional drawing of the sample holder for fluorescent X-ray analysis which is 1st Embodiment of this invention, and a holder. 同試料保持具の上面図である。It is a top view of the sample holder. 同試料保持具の断面図である。It is sectional drawing of the sample holder. 同試料保持具をホルダに装着する変形例を示す断面図である。It is sectional drawing which shows the modification which equips the holder with the sample holder. 同試料保持具、ホルダおよび蓋の断面図である。It is sectional drawing of the sample holder, a holder, and a lid | cover. 本発明の第2実施形態の蛍光X線分析方法に使用される、本発明の第3実施形態の蛍光X線分析装置を示す概略図である。It is the schematic which shows the X-ray fluorescence analyzer of 3rd Embodiment of this invention used for the X-ray fluorescence analysis method of 2nd Embodiment of this invention. (A),(B),(C)は、第2実施形態の試料を保持する方法の各手順を示す断面図である。(A), (B), (C) is sectional drawing which shows each procedure of the method of hold | maintaining the sample of 2nd Embodiment. 第1の従来例の断面図である。It is sectional drawing of the 1st prior art example. 前記図8の従来例の分解斜視図である。FIG. 9 is an exploded perspective view of the conventional example of FIG. 8. 第2の従来例の断面図である。It is sectional drawing of the 2nd prior art example. (A),(B),(C)は、前記図10の従来例の試料を保持する方法の各手順を示す斜視図である。(A), (B), (C) is a perspective view which shows each procedure of the method of hold | maintaining the sample of the prior art example of the said FIG.

符号の説明Explanation of symbols

1 フィルム
1a 付着部
1b 透過部
1c 外周部
2 枠体
5 試料保持具
6、36 筒状のホルダ
7 筒状のホルダの開口
9 試料
14 1次X線
15 2次X線
23 X線源
24 検出手段
40 蛍光X線分析装置
DESCRIPTION OF SYMBOLS 1 Film 1a Adhering part 1b Permeation | transmission part 1c Outer peripheral part 2 Frame 5 Sample holder 6, 36 Cylindrical holder 7 Opening of cylindrical holder 9 Sample 14 Primary X-ray 15 Secondary X-ray 23 X-ray source 24 Detection Means 40 X-ray fluorescence analyzer

Claims (3)

液体、ゲル状体または粉体試料に下方から1次X線を照射して蛍光X線分析するために用いられる蛍光X線分析用試料ホルダであって、
枠体と、その枠体に付着された付着部、前記枠体の外周よりも外側の外周部および前記枠体の内周よりも内側でX線を透過させるための透過部を有するフィルムとを備えた蛍光X線分析用試料保持具と、
下部にX線を通過させるための開口を有する筒状のホルダと、
を備え、
前記枠体が前記フィルムの下方に位置して、前記透過部が前記枠体の内周部とともに前記筒状のホルダの開口を覆い、前記外周部が前記筒状のホルダの側部の内面を覆うように配置され、前記透過部の上に前記試料を保持する蛍光X線分析用試料ホルダ
A sample holder for X-ray fluorescence analysis used for X-ray fluorescence analysis by irradiating a liquid, gel or powder sample with primary X-rays from below ;
A film having a frame, an attachment portion attached to the frame, an outer periphery outside the outer periphery of the frame, and a transmission portion for transmitting X-rays inside the inner periphery of the frame A sample holder for fluorescent X-ray analysis provided ,
A cylindrical holder having an opening for passing X-rays at the bottom;
With
The frame is located below the film, the transmission part covers the opening of the cylindrical holder together with the inner peripheral part of the frame, and the outer peripheral part covers the inner surface of the side part of the cylindrical holder. A sample holder for fluorescent X-ray analysis that is arranged so as to cover and holds the sample on the transmission part .
請求項1に記載の蛍光X線分析用試料ホルダを用いる蛍光X線分析方法であって、
蛍光X線分析用試料ホルダの上方から前記試料を注いで、
前記透過部を介して前記試料に下方から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,
Pour the sample from above the sample holder for X-ray fluorescence analysis,
A fluorescent X-ray analysis method for measuring the intensity of secondary X-rays generated by irradiating the sample with primary X-rays from below through the transmission part.
請求項1に記載の蛍光X線分析用試料ホルダを用いる蛍光X線分析装置であって、
前記試料を保持した前記蛍光X線分析用試料ホルダの透過部を介して、前記試料に下方から1次X線を照射するX線源と、
前記試料から発生する2次X線の強度を測定する検出手段とを備えた蛍光X線分析装置。
A fluorescent X-ray analyzer using the fluorescent X-ray analysis sample holder according to claim 1,
Through the transmission portion of the fluorescent X-ray analytical sample holder holding the sample, the X-ray source for irradiating primary X-rays from below the sample,
A fluorescent X-ray analyzer comprising: a detecting unit that measures the intensity of secondary X-rays generated from the sample.
JP2005136884A 2005-05-10 2005-05-10 Sample holder for fluorescent X-ray analysis and fluorescent X-ray analysis method and apparatus using the same Expired - Fee Related JP4398901B2 (en)

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