JPS63734B2 - - Google Patents
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- Publication number
- JPS63734B2 JPS63734B2 JP52088569A JP8856977A JPS63734B2 JP S63734 B2 JPS63734 B2 JP S63734B2 JP 52088569 A JP52088569 A JP 52088569A JP 8856977 A JP8856977 A JP 8856977A JP S63734 B2 JPS63734 B2 JP S63734B2
- Authority
- JP
- Japan
- Prior art keywords
- sample
- container
- filling space
- container body
- fluorescent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
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- Analysing Materials By The Use Of Radiation (AREA)
- Optical Measuring Cells (AREA)
Description
【発明の詳細な説明】
本発明は螢光Ｘ線分析用微量試料容器に関す
る。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a microsample container for fluorescent X-ray analysis.
一般に、螢光Ｘ線分析は、試料に一次Ｘ線を照
射することにより、試料中の測定成分から発せら
れるその成分固有の波長を有する螢光Ｘ線（特性
Ｘ線ともいう）を測定して試料中の測定成分濃度
を知る分析方法である。 In general, fluorescent X-ray analysis measures fluorescent X-rays (also called characteristic X-rays) that are emitted from the component to be measured and have a wavelength specific to that component by irradiating the sample with primary X-rays. This is an analysis method that determines the concentration of a component to be measured in a sample.
例えばこの螢光Ｘ線分析方法により石油中のイ
オウ濃度を測定しようとする場合、その石油が例
えばタンク内に溜められている石油であれば必要
な試料の量は十分に確保することができる。しか
しながら、その石油が例えば海上流出油のように
少量しか手に入らないようなものについては入手
可能な試料の量は限られており、有効にその試料
を使用する必要がある。 For example, when measuring the sulfur concentration in petroleum using this fluorescent X-ray analysis method, if the petroleum is stored in a tank, a sufficient amount of sample can be secured. However, when the oil is available in small amounts, such as oil spilled on the sea, the amount of samples that can be obtained is limited, and it is necessary to use the samples effectively.
本発明はこのように入手可能な試料に量が限ら
れた場合に、特に有効な螢光Ｘ線分析用微量試料
容器に関するものである。 The present invention relates to a trace sample container for fluorescent X-ray analysis that is particularly effective when the amount of sample available is limited.
従来より使用されているこの種微量試料容器
は、例えば第１図に示すように、上部及び底部が
共に開口している筒状の容器本体１の底部に放射
線透過膜（例えばポリエステル膜等）２を張着す
ると共に、この放射線透過膜２の周縁部を固定具
（外枠或いはＯリング等）３によつて容器本体１
の外側に固定し、必要に応じて容器本体に蓋を取
り付けるようにしている。そして、試料４は底部
を放射線透過膜２で張着された容器本体１内に収
容されており、前記放射線透過膜２を通して試料
４に一次Ｘ線が照射され、この試料４より発生し
放射線透過膜２を通過して出てくる螢光Ｘ線を検
出するように構成されている。 For example, as shown in FIG. 1, this kind of microsample container that has been conventionally used has a cylindrical container body 1 with both the top and bottom open, and a radiation-transmitting film (such as a polyester film) 2 on the bottom of the container body 1. At the same time, the peripheral edge of the radiation-transparent film 2 is attached to the container body 1 using a fixing device (outer frame, O-ring, etc.) 3.
It is fixed to the outside of the container, and a lid can be attached to the container body as necessary. The sample 4 is housed in a container body 1 whose bottom is covered with a radiation-transparent membrane 2, and the sample 4 is irradiated with primary X-rays through the radiation-transparent membrane 2, and the radiation transmitted from the sample 4 is transmitted. It is configured to detect fluorescent X-rays passing through the membrane 2 and emerging.
この場合、一定以上の試料の厚み及び一定以上
の試料照射面積が要求されるが、照射面積に関し
ては実効的に一次Ｘ線の照射時間により補足する
ことができるが、試料の厚みに関しては測定精度
の点からある一定以上の厚み（有効厚み；例えば
石油製品中のイオウ測定においては約３mm）が要
求される。試料の量が十分に多い場合には前記試
料厚みは十分に確保し得るが、試料の量が少ない
場合には照射面積を多少犠性にしても所定の試料
厚みを確保する必要があり、そのため、試料容器
自体を小さくすることにより照射面積を小さく
し、試料厚みを確保しなければならなかつた。 In this case, a sample thickness of a certain value or more and a sample irradiation area of a certain value or more are required, but the irradiation area can be effectively supplemented by the primary X-ray irradiation time, but the measurement accuracy regarding the sample thickness is From this point of view, a thickness of at least a certain level (effective thickness; for example, approximately 3 mm in measuring sulfur in petroleum products) is required. If the amount of the sample is sufficiently large, the above-mentioned sample thickness can be ensured sufficiently, but if the amount of the sample is small, it is necessary to ensure the predetermined sample thickness even if the irradiation area is sacrificed to some extent. However, by making the sample container itself smaller, it was necessary to reduce the irradiation area and ensure the sample thickness.
しかしながら、試料の量が変わる毎に試料容器
自体の大きさを変えるという方法は、多くの試料
容器（それもそれぞれ大きさの異なるもの）を、
予め準備しておく必要があること、又、試料容器
の設定に関しては、試料容器の設置位置の微妙な
変化が測定する螢光Ｘ線の量に大きく影響するた
め、たえず一定の位置に置く必要があり、各試料
容器に応じたアダプタを別途製作し、分析部に取
り付ける等の改造が必要であつた。 However, the method of changing the size of the sample container itself each time the amount of sample changes requires the use of many sample containers (of different sizes).
It is necessary to prepare the sample container in advance, and the sample container must be kept in a constant position because subtle changes in its installation position greatly affect the amount of fluorescent X-rays to be measured. Therefore, it was necessary to make modifications such as separately manufacturing adapters for each sample container and attaching them to the analysis section.
本発明は上記の事柄に留意してなされたもの
で、試料の量が少ない場合でも所定の試料厚みを
確保することができる螢光Ｘ線分析用微量試料容
器を提供することを目的とする。 The present invention has been made with the above-mentioned considerations in mind, and it is an object of the present invention to provide a microsample container for fluorescent X-ray analysis that can ensure a predetermined sample thickness even when the amount of sample is small.
以下、本発明の実施例を図面を参照しながら説
明する。 Embodiments of the present invention will be described below with reference to the drawings.
第２図イ乃至ハは本発明に係る螢光Ｘ線分析用
微量試料容器の容器本体の種々の例を示す。 FIGS. 2A to 2C show various examples of container bodies of microsample containers for fluorescent X-ray analysis according to the present invention.
先ず、同図イにおいて、３１は容器本体で、そ
の略中央には上下に開口部を有する試料充填空間
部３５が形成してあり、その底面３１ａは試料充
填空間部３５の下部開口周端縁３２ａから外縁部
３１ｃにかけて上向きに傾斜したテーパ面に形成
されており、他方、上面３１ｂも試料充填空間部
３５の上部開口周端縁３２ｂから外縁部３１ｃに
かけて上向きに傾斜したテーパ面に形成されてい
る。そして、前記試料充填空間部３５はその内径
が容器本体３１の外径寸法の1/2〜1/3程度に設定
してあり、容器本体３１の外形寸法に相当する容
積に比して小さい容積を有する空間に形成されて
いる。 First, in A of the same figure, numeral 31 is a container main body, and a sample filling space 35 having upper and lower openings is formed approximately in the center of the container main body, and its bottom surface 31a is the peripheral edge of the lower opening of the sample filling space 35. The upper surface 31b is also formed as a tapered surface that slopes upward from the upper opening peripheral edge 32b of the sample filling space 35 to the outer edge 31c. There is. The sample filling space 35 has an inner diameter set to about 1/2 to 1/3 of the outer diameter of the container body 31, and has a smaller volume than the volume corresponding to the outer dimension of the container body 31. It is formed in a space with .
上記構成の容器本体３１においては、上面３１
ｂは試料充填空間部３５の上部開口周端縁３２ｂ
から外縁部３１ｃにかけて上向きに傾斜したテー
パ面に形成されており、つまり、該上面３１ｂは
開口部が形成されている中央部が外縁部３１ｃよ
りも低くなるように形成されているので、試料充
填空間部３５に対して試料を確実に充填すること
ができる。又、底面３１ａは試料充填空間部３５
の下部開口周端縁３２ａから外縁部３１ｃにかけ
て上向きに傾斜したテーパ面に形成されているの
で、該底面３１ａに沿わせて放射線透過膜を張設
したとき、底面３１ａとの間に隙間を生ずること
なく放射線透過膜を形成することができ、従つ
て、試料充填空間部３５内の試料が外部に漏れ出
ることがない。 In the container main body 31 having the above configuration, the upper surface 31
b is the upper opening peripheral edge 32b of the sample filling space 35
The upper surface 31b is formed into a tapered surface that slopes upward from the outer edge portion 31c to the outer edge portion 31c.In other words, the upper surface 31b is formed such that the central portion where the opening is formed is lower than the outer edge portion 31c, so that it is easy to fill the sample. The space 35 can be reliably filled with the sample. In addition, the bottom surface 31a is a sample filling space 35.
Since the tapered surface is formed upwardly from the lower opening peripheral edge 32a to the outer edge 31c, when the radiation-transmitting film is stretched along the bottom surface 31a, a gap is created between the bottom surface 31a and the bottom surface 31a. Therefore, the sample in the sample filling space 35 does not leak to the outside.
次に、同図ロにおいて、４１は容器本体で、そ
の底面４１ａ、上面４１ｂは前記容器本体３１と
同様に、それぞれ上向きに傾斜したテーパ面に形
成されている。４１ｃは外縁部である。そして、
この容器本体４１の下方（底面４１ａ側）には、
所定の試料厚みを形成し得る高さを有する試料充
填空間部４５が開設されている。この試料充填空
間部４５の内径も前記容器本体３１における試料
充填空間部３５と同様に、容器本体４１の外径寸
法の1/2〜1/3程度に設定してある。そして、前記
容器本体４１の中央部には試料充填空間部４５の
開口径よりも小径で、かつ、上面４１ｂから試料
充填空間部４５に通ずる試料注入孔４６が形成し
てある。 Next, in FIG. 4B, 41 is a container body, and its bottom surface 41a and top surface 41b are respectively formed into upwardly inclined tapered surfaces similarly to the container body 31. 41c is the outer edge. and,
Below this container body 41 (bottom surface 41a side),
A sample filling space 45 having a height that allows forming a predetermined sample thickness is provided. The inner diameter of this sample filling space 45 is also set to about 1/2 to 1/3 of the outer diameter of the container body 41, similarly to the sample filling space 35 in the container body 31. A sample injection hole 46 is formed in the center of the container body 41 and has a smaller diameter than the opening diameter of the sample filling space 45 and communicates with the sample filling space 45 from the top surface 41b.
上記構成の容器本体４１においては、上面４１
ｂが上向きの傾斜を有するテーパ面に形成してあ
るので、試料注入孔４６が細径であつても試料充
填空間部４５に対して確実に試料を充填すること
ができる。 In the container main body 41 having the above configuration, the upper surface 41
Since b is formed as a tapered surface having an upward slope, the sample filling space 45 can be reliably filled with the sample even if the sample injection hole 46 has a small diameter.
又、同図ハにおいて、５１は容器本体で、この
容器本体５１の外形は上記容器本体４１と殆ど同
じであるが、更に、上面５１ｂから試料充填空間
部５５に通ずる試料注入孔５６と平行に空気抜き
孔５７を設けてある。５１ａは底面、５１ｃは外
縁部である。 In addition, in the same figure C, 51 is a container main body, and the external shape of this container main body 51 is almost the same as the above-mentioned container main body 41. An air vent hole 57 is provided. 51a is the bottom surface, and 51c is the outer edge.
尚、上記各図において、６０は容器本体３１，
４１，５１のそれぞれ外縁部３１ｃ，４１ｃ，５
１ｃに周設された環状溝で、容器外枠又はＯリン
グ等を係止するためのものである。又、容器本体
３１，４１，５１は通常円筒形に形成され、従つ
て、その底３１ａ，４１ａ，５１ａ及び上面３１
ｂ，４１ｂ，５１ｂが上述のようにテーパ面をな
すとき、これらの底面３１ａ，４１ａ，５１ａ及
び上面３１ｂ，４１ｂ，５１ｂは略逆円錐形状を
呈し、更に、試料充填空間部３５，４５，５５及
び試料注入孔４６，５６の平面視形状は円形であ
る。 In each of the above figures, 60 indicates the container body 31,
Outer edge portions 31c, 41c, 5 of 41, 51, respectively
It is an annular groove provided around 1c, and is used to lock the outer frame of the container, an O-ring, etc. Further, the container bodies 31, 41, 51 are usually formed in a cylindrical shape, and therefore the bottoms 31a, 41a, 51a and the top surface 31
b, 41b, 51b form tapered surfaces as described above, the bottom surfaces 31a, 41a, 51a and the top surfaces 31b, 41b, 51b have a substantially inverted conical shape, and the sample filling spaces 35, 45, 55 The shape of the sample injection holes 46 and 56 in plan view is circular.
次に、第３図は第２図ロに示す容器本体４１を
用いた場合の螢光Ｘ線分析用微量試料容器の一例
を示し、ステンレス等の金属製（プラスチツク製
でもよい）の容器本体４１の底面４１ａ側に、例
えばポリエステルフイルムからなる放射線透過膜
４２を張設し、この放射線透過膜４２の周縁部を
プラスチツク製の筒状容器外枠又はＯリング等の
固定具４３により上方へ引き込んで容器本体４１
の外側面に固定することによつて螢光Ｘ線分析用
微量試料容器を形成する。そして、容器本体４１
の上面４１ｂ側から試料４４を流し込み、試料注
入孔４６を介して試料充填空間部４５に試料４４
を充填させている。４８はＸ線照射管、４９は検
出器である。 Next, FIG. 3 shows an example of a trace sample container for fluorescent X-ray analysis using the container body 41 shown in FIG. A radiation-transparent film 42 made of, for example, a polyester film is stretched over the bottom surface 41a of the container, and the peripheral edge of the radiation-transparent film 42 is pulled upward by a fixing device 43 such as a plastic cylindrical container outer frame or an O-ring. Container body 41
A trace sample container for fluorescent X-ray analysis is formed by fixing the sample to the outer surface of the sample. Then, the container body 41
The sample 44 is poured into the sample filling space 45 through the sample injection hole 46 from the upper surface 41b side.
is filled with. 48 is an X-ray irradiation tube, and 49 is a detector.
この場合、容器本体４１の底面４１ａは試料充
填空間部４５の下部開口周端縁４５′から外縁部
４１ｃにかけて上向きの傾斜を有するテーパ面に
形成されているから、放射線透過膜４２が試料充
填空間部４５の下部開口を密閉するように底面４
１ａに張設されることとなり、試料充填空間部４
５内に充填された試料４４の漏出又は滲出が効果
的に防止される。 In this case, the bottom surface 41a of the container body 41 is formed into a tapered surface having an upward slope from the lower opening peripheral edge 45' of the sample filling space 45 to the outer edge 41c. The bottom surface 4 is sealed so as to seal the lower opening of the portion 45.
1a, and the sample filling space 4
Leakage or seepage of the sample 44 filled in the sample 5 is effectively prevented.
尚、１c.c.程度の試料の量の場合、例えば上記容
器本体４１の外径d1を40mm、試料注入孔４６の内
径d2を５mm、試料充填空間部４５の内径Ｄを20
mm、試料充填空間部４５の高さ、即ち、分析に必
要な有効厚みＨを３mmとすればよい。 In the case of a sample amount of about 1 c.c., for example, the outer diameter d 1 of the container body 41 is 40 mm, the inner diameter d 2 of the sample injection hole 46 is 5 mm, and the inner diameter D of the sample filling space 45 is 20 mm.
mm, and the height of the sample filling space 45, that is, the effective thickness H required for analysis, may be 3 mm.
更に、上記容器本体３１，４１，５１は試料の
性質に応じてプラスチツク材その他の適当な材料
によつて作ることができる。又、容器本体３１，
４１，５１の上部には必要に応じて蓋を装着でき
るようにしてあつてもよい。 Furthermore, the container bodies 31, 41, 51 can be made of plastic or other suitable materials depending on the nature of the sample. Moreover, the container body 31,
A cover may be attached to the upper part of 41, 51 if necessary.
以上説明したように、本発明に係る螢光Ｘ線分
析用微量試料容器においては、容器本体には底面
の中央において下方に開口すると共に上面と連通
し、かつ、容器本体の外形寸法に相当する容積に
比して小さい容積を有する試料充填空間部が形成
してあるので、試料の量が少ない場合であつても
十分な試料厚みを確保することができる。そし
て、容器本体の上面には中央部から外縁部にかけ
て上向きに傾斜したテーパ面が形成してあるの
で、試料を試料充填空間部内に確実に充填するこ
とができ、更に、容器本体の下面にも中央部から
外縁部にかけて上向きに傾斜したテーパ面を形成
してあるので、試料充填空間部の下部開口側は放
射線透過膜によつて完全密封とすることができ、
従つて、試料が少ない場合であつてもこれを無駄
にすることなく、試料充填空間部内に保持するこ
とができるので、分析を確実に行うことができ
る。又、容器本体の形状は比較的簡単であるか
ら、安価に製作できるといつた利点がある。 As explained above, in the microsample container for fluorescent X-ray analysis according to the present invention, the container body has an opening downward at the center of the bottom surface, communicates with the top surface, and has a diameter corresponding to the external dimensions of the container body. Since a sample filling space having a volume smaller than the volume is formed, a sufficient sample thickness can be ensured even when the amount of sample is small. Since the upper surface of the container body is formed with a tapered surface that slopes upward from the center to the outer edge, the sample can be reliably filled into the sample filling space. Since a tapered surface is formed that slopes upward from the center to the outer edge, the lower opening side of the sample filling space can be completely sealed with the radiation-transparent film.
Therefore, even if there is a small amount of sample, it can be held in the sample filling space without wasting it, so that analysis can be performed reliably. Further, since the shape of the container body is relatively simple, there is an advantage that it can be manufactured at low cost.
第１図は従来の試料容器を示す断面図、第２図
イ，ロ，ハは本発明に係る螢光Ｘ線分析用微量試
料容器の容器本体の種々の例を示す断面図、第３
図は本発明に係る螢光Ｘ線分析用微量試料容器の
一例を示す断面図である。
３１，４１，５１…容器本体、３１ａ，４１
ａ，５１ａ…底面、３１ｂ，４１ｂ，５１ｂ…上
面、３１ｃ，４１ｃ，５１ｃ…外縁部３５，４
５，５５…試料充填空間部、４２…放射線透過
膜、４３…固定具、４４…試料、４６，５６…試
料注入孔、５７…空気抜き孔。
FIG. 1 is a sectional view showing a conventional sample container, FIGS.
The figure is a sectional view showing an example of a microsample container for fluorescent X-ray analysis according to the present invention. 31, 41, 51... Container body, 31a, 41
a, 51a...Bottom surface, 31b, 41b, 51b...Top surface, 31c, 41c, 51c...Outer edge portion 35, 4
5, 55... Sample filling space, 42... Radiation transmitting membrane, 43... Fixture, 44... Sample, 46, 56... Sample injection hole, 57... Air vent hole.
Claims (1)
テーパ面をそれぞれ有する上面及び底面と、該底
面の中央において下方に開口すると共に前記上面
と連通する試料充填空間部とを備えてなる容器本
体と、前記底面に張設され前記試料充填空間部の
下部開口側を閉塞する放射線透過膜と、該放射線
透過膜を固定するための固定具とからなり、前記
試料充填空間部が容器本体の外径寸法に対応する
容積に比して十分小さい容積を有するように構成
したことを特徴とする螢光Ｘ線分析用微量試料容
器。 ２ 容器本体の中央部に、試料充填空間部の開口
径よりも小径であつて、容器本体の上面から前記
試料充填空間部に通ずる試料注入孔を設けてなる
特許請求の範囲第１項に記載の螢光Ｘ線分析用微
量試料容器。 ３ 容器本体の上面から試料充填空間部に通じて
いる空気抜き孔を設けてなる特許請求の範囲第１
項または第２項に記載の螢光Ｘ線分析用微量試料
容器。[Scope of Claims] 1. A top surface and a bottom surface each having an upwardly inclined tapered surface from the center to the outer edge, and a sample filling space that opens downward at the center of the bottom surface and communicates with the top surface. a container body, a radiation-transparent film stretched over the bottom surface and closing the lower opening side of the sample filling space, and a fixture for fixing the radiation-transparent film, and the sample filling space is 1. A trace sample container for fluorescent X-ray analysis, characterized in that the container is configured to have a volume that is sufficiently smaller than the volume corresponding to the outer diameter of the main body. 2. Claim 1, wherein a sample injection hole is provided in the center of the container body, the diameter of which is smaller than the opening diameter of the sample filling space, and which communicates from the top surface of the container body to the sample filling space. Micro sample container for fluorescent X-ray analysis. 3. Claim 1, comprising an air vent hole communicating from the top surface of the container body to the sample filling space.
The micro sample container for fluorescent X-ray analysis according to item 1 or 2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8856977A JPS5423593A (en) | 1977-07-22 | 1977-07-22 | Microsample container |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8856977A JPS5423593A (en) | 1977-07-22 | 1977-07-22 | Microsample container |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5423593A JPS5423593A (en) | 1979-02-22 |
| JPS63734B2 true JPS63734B2 (en) | 1988-01-08 |
Family
ID=13946486
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP8856977A Granted JPS5423593A (en) | 1977-07-22 | 1977-07-22 | Microsample container |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5423593A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001255289A (en) * | 2000-03-08 | 2001-09-21 | Horiba Ltd | Liquid sample cell, upper surface irradiation type x-ray analysis method using it, and apparatus therefor |
| US9402426B2 (en) | 2008-04-10 | 2016-08-02 | Asics Corporation | Upper garment |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3791384B2 (en) * | 2001-10-11 | 2006-06-28 | 株式会社島津製作所 | Multiple cell for optical analysis |
| US7222406B2 (en) | 2002-04-26 | 2007-05-29 | Battelle Memorial Institute | Methods for making a multi-layer seal for electrochemical devices |
| JP4873188B2 (en) * | 2008-08-04 | 2012-02-08 | 株式会社島津製作所 | Spectrophotometer |
| JP2024001708A (en) * | 2022-06-22 | 2024-01-10 | 株式会社日立ハイテクサイエンス | Sample cell for fluid sample, fluorescent X-ray analyzer using the same, and fluorescent X-ray analysis method |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1232765B (en) * | 1964-12-28 | 1967-01-19 | Bodenseewerk Perkin Elmer Co | Liquid cuvette for polarimeter |
| US3847777A (en) * | 1972-05-08 | 1974-11-12 | Instrumentation Labor Inc | Electrochemical analyzer |
| JPS49134196U (en) * | 1973-03-20 | 1974-11-18 |
-
1977
- 1977-07-22 JP JP8856977A patent/JPS5423593A/en active Granted
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001255289A (en) * | 2000-03-08 | 2001-09-21 | Horiba Ltd | Liquid sample cell, upper surface irradiation type x-ray analysis method using it, and apparatus therefor |
| US9402426B2 (en) | 2008-04-10 | 2016-08-02 | Asics Corporation | Upper garment |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5423593A (en) | 1979-02-22 |
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