JPS6352699B2 - - Google Patents
Info
- Publication number
- JPS6352699B2 JPS6352699B2 JP56101724A JP10172481A JPS6352699B2 JP S6352699 B2 JPS6352699 B2 JP S6352699B2 JP 56101724 A JP56101724 A JP 56101724A JP 10172481 A JP10172481 A JP 10172481A JP S6352699 B2 JPS6352699 B2 JP S6352699B2
- Authority
- JP
- Japan
- Prior art keywords
- sample
- liquid
- rays
- powder
- observation
- 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
Links
- 239000007788 liquid Substances 0.000 claims description 29
- 238000005259 measurement Methods 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- 230000005855 radiation Effects 0.000 claims 1
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 239000003208 petroleum Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 239000004794 expanded polystyrene Substances 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000004441 surface measurement Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/076—X-ray fluorescence
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Description
【発明の詳細な説明】
本発明は、液体試料の螢光Ｘ線分析に適した試
料面決定方法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a sample surface determination method suitable for fluorescent X-ray analysis of liquid samples.
試料にＸ線を照射し、試料の成分元素から放出
される螢光Ｘ線を単線晶の回析作用を利用して、
元素の定性、定量分析を行なう螢光Ｘ線分析が知
られている。 The sample is irradiated with X-rays, and the fluorescent X-rays emitted from the component elements of the sample are analyzed using the diffraction effect of single-line crystals.
Fluorescent X-ray analysis for qualitative and quantitative analysis of elements is known.
螢光Ｘ線分析では、第１図に示すようにＸ線管
４ａから発生するＸ線は測定基準面A1に照射さ
れ、試料から放出される螢光Ｘ線を検出する検出
器４ｂが配置されているが、試料面がA2，A3の
ように測定基準面にないときには、螢光Ｘ線は検
出器４ｂの光軸からはずれるため螢光Ｘ線の強度
は変動してしまう。そこで、試料面の決定は、精
度のよい分析のためには必須の要件となつてい
る。 In fluorescent X-ray analysis, as shown in Fig. 1, X-rays generated from an X-ray tube 4a are irradiated onto a measurement reference surface A1 , and a detector 4b is arranged to detect fluorescent X-rays emitted from the sample. However, when the sample surface is not on the measurement reference plane as in A 2 and A 3 , the intensity of the fluorescent X-rays fluctuates because the fluorescent X-rays are deviated from the optical axis of the detector 4b. Therefore, determining the sample surface is an essential requirement for accurate analysis.
液体試料の元素分析、例えば石油中のイオウ分
を分析する場合は、試料の石油は底部に窓のある
容器に入れ、下方から分析している。これは、窓
つまり測定面の上下位置あわせが簡単なためであ
る。しかし、窓の材質によつては螢光Ｘ線が吸収
され、強度が低下したり、窓の材質あるいは厚さ
の異いにより強度が変化し測定精度を悪くしてい
た。また、試料によつては、窓材が変質変形して
しまうなどの不都合も生じていた。 For elemental analysis of a liquid sample, for example, when analyzing the sulfur content in petroleum, the petroleum sample is placed in a container with a window at the bottom and analyzed from below. This is because it is easy to vertically align the window, that is, the measurement surface. However, depending on the material of the window, the fluorescent X-rays are absorbed and the intensity decreases, and the intensity changes depending on the material or thickness of the window, resulting in poor measurement accuracy. Further, depending on the sample, problems such as deterioration and deformation of the window material occurred.
本件発明者は、すでに特願昭55―30920号によ
り、試料（一般には固体）の測定面を定める方
法、つまり焦点深度の浅いレンズを用いた観察系
により、試料表面の像の焦点があうように試料を
上下することにより、±0.1mm以内まで測定面の上
下位置の精度を保持する方法を提案している。 The inventor of the present invention has already proposed in Japanese Patent Application No. 55-30920 a method of determining the measurement surface of a sample (generally a solid), that is, an observation system using a lens with a shallow depth of focus, so that the image of the sample surface is brought into focus. We propose a method that maintains the accuracy of the vertical position of the measurement surface to within ±0.1 mm by raising and lowering the sample.
この方法は、試料表面の像が目視できる限りあ
らゆる試料に対して有効であるが、前述のような
液体試料の場合ほとんど像を認めることができ
ず、前記方法だけでは液体試料の分析は行なえな
かつた。 This method is effective for all kinds of samples as long as the image of the sample surface can be visually observed, but in the case of liquid samples such as those mentioned above, an image is hardly visible, and liquid samples cannot be analyzed using this method alone. Ta.
本発明の目的は、液体試料を螢光Ｘ線分析でき
る試料面決定方法を提供することにある。 An object of the present invention is to provide a method for determining a sample surface by which a liquid sample can be analyzed by fluorescent X-rays.
前記目的を達成するために、本発明による液体
螢光Ｘ線分析装置における試料面決定方法は、液
体表面にＸ線を照射し、表面からの螢光Ｘ線を分
析する液体螢光Ｘ線分析装置において、液体試料
が充填され前記Ｘ線で照射される領域とは液表面
で分離された領域をもつ開放形の試料容器と、前
記試料容器の高さ位置調節をする上下機構と、焦
点深度の浅いレンズを用い前記試料液面が測定基
準面にあるときに液体表面を観察面に結像する観
察系とを設け、前記Ｘ線で照射される領域とは液
表面で分離された領域に粉体を浮遊させ、前記観
察面に前記粉体を結像させるように前記上下機構
で容器位置を調節し、測定面を決定するように構
成されている。 In order to achieve the above object, a method for determining a sample surface in a liquid fluorescence X-ray analyzer according to the present invention is a liquid fluorescence X-ray analysis method in which the liquid surface is irradiated with X-rays and the fluorescence X-rays from the surface are analyzed. The apparatus includes an open sample container having a region filled with a liquid sample and separated from the region to be irradiated with the X-rays by a liquid surface, a vertical mechanism for adjusting the height position of the sample container, and a depth of focus. An observation system is provided that uses a shallow lens to form an image of the liquid surface on the observation surface when the sample liquid surface is on the measurement reference plane, and the area irradiated with the X-rays is an area separated by the liquid surface. The container position is adjusted by the vertical mechanism so that the powder is suspended and an image of the powder is formed on the observation surface, and the measurement surface is determined.
前記構成によれば、浮遊粉体を観察面に結像さ
せるだけで測定基準面が決定でき、本発明の目的
は完全に達成できる。 According to the above configuration, the measurement reference plane can be determined simply by imaging the floating powder on the observation plane, and the object of the present invention can be completely achieved.
以下図面等を参照して本発明をさらに詳しく説
明する。 The present invention will be described in more detail below with reference to the drawings and the like.
第２図は、本発明方法を実施する装置の実施例
を示した正面図、第３図は同側面図である。 FIG. 2 is a front view showing an embodiment of an apparatus for implementing the method of the present invention, and FIG. 3 is a side view of the same.
試料容器１は膜等の窓がない上面開放形の容器
であり、石油等の液体試料２が充填されており、
この液面を２分する分離部材１ａが設けられてい
る。これにより液の表面の粉体６の浮遊領域と測
定領域が分離され、粉体６は分析領域から隔離さ
れる。試料容器１は、上下機構３に載置されてい
る。 The sample container 1 is an open-top container with no window such as a membrane, and is filled with a liquid sample 2 such as petroleum.
A separating member 1a is provided to divide this liquid level into two. As a result, the floating region of the powder 6 on the surface of the liquid and the measurement region are separated, and the powder 6 is isolated from the analysis region. The sample container 1 is placed on a vertical mechanism 3.
螢光Ｘ線分析装置４は、Ｘ線管４ａ、検出器４
ｂとからなり、Ｘ線管４ａから発生するＸ線は試
料容器４の分割された一方側に照射され、試料表
面から発生する螢光Ｘ線は検出器４ｂで検出され
る。観察系５は焦点深度の浅いレンズ５ａ、ミラ
ー５ｂ、観察面であるピントグラス５ｃとからな
り、試料容器４の分割された他方側の試料液面に
対向して設けられており、液面が測定基準面に達
したとき、結像するように配置されている。 The fluorescent X-ray analyzer 4 includes an X-ray tube 4a and a detector 4.
The X-rays generated from the X-ray tube 4a are irradiated onto one side of the divided sample container 4, and the fluorescent X-rays generated from the sample surface are detected by the detector 4b. The observation system 5 consists of a lens 5a with a shallow depth of focus, a mirror 5b, and a focusing glass 5c serving as an observation surface, and is provided facing the sample liquid surface on the other divided side of the sample container 4. It is arranged to form an image when it reaches the measurement reference plane.
観察系５が配置された前記他方側の試料液面に
は、試料液に浮く物質の粉末、例えば発泡ポリス
チロール等の粉末である浮遊粉体６を浮遊させ、
上下機構３で容器位置を上下に調節することによ
り、浮遊粉体６を観察面であるピントグラス５ｃ
に結像させて、容器内で連通している測定面の位
置を正確に決定するようにしてある。 On the sample liquid surface on the other side where the observation system 5 is arranged, suspended powder 6, which is a powder of a substance that floats on the sample liquid, for example, a powder of expanded polystyrene, is suspended;
By adjusting the container position up and down with the up and down mechanism 3, the floating powder 6 can be seen in the focusing glass 5c which is the observation surface.
is imaged to accurately determine the position of the communicating measurement surface within the container.
以上説明したように、本発明によれば測定面を
決定する窓を設けなくとも正確に試料面を決定で
き、精度のよい液体試料の分析が可能となつた。 As explained above, according to the present invention, the sample surface can be determined accurately without providing a window for determining the measurement surface, and a liquid sample can be analyzed with high precision.
第１図は螢光Ｘ線分析装置の原理を示す略図、
第２図は本発明方法を実施する装置の実施例を示
した正面図、第３図は同側面図である。
１…試料容器、２…液体試料、３…上下機構、
４…螢光Ｘ線分析装置、５…観察系、６…浮遊粉
体。
Figure 1 is a schematic diagram showing the principle of a fluorescent X-ray analyzer;
FIG. 2 is a front view showing an embodiment of the apparatus for carrying out the method of the present invention, and FIG. 3 is a side view of the same. 1...sample container, 2...liquid sample, 3...vertical mechanism,
4... Fluorescence X-ray analyzer, 5... Observation system, 6... Floating powder.
Claims (1)
線を分析する液体螢光Ｘ線分析装置において、液
体試料が充填され前記Ｘ線で照射される領域とは
液表面で分離された領域をもつ開放形の試料容器
と、前記試料容器の高さ位置調節をする上下機構
と、焦点深度の浅いレンズを用い前記試料液面が
測定基準面にあるときに液体表面を観察面に結像
する観察系とを設け、前記Ｘ線で照射される領域
とは液表面で分離された領域に粉体を浮遊させ、
前記観察面に前記粉体を結像させるように前記上
下機構で容器位置を調節し、測定面を決定するよ
うに構成したことを特徴とする液体螢光Ｘ線分析
装置における試料面決定方法。1 Irradiate the liquid surface with X-rays to detect fluorescent light from the surface
A liquid fluorescence X-ray analyzer for analyzing radiation includes an open sample container filled with a liquid sample and having a region separated by a liquid surface from the region irradiated with the X-rays, and a height of the sample container. A region irradiated with the X-rays is provided with a vertical mechanism for position adjustment and an observation system that uses a lens with a shallow depth of focus to image the liquid surface on an observation surface when the sample liquid surface is on the measurement reference surface. is a method in which powder is suspended in a separated area on the liquid surface,
A method for determining a sample surface in a liquid fluorescence X-ray analyzer, characterized in that the container position is adjusted by the vertical mechanism so as to image the powder on the observation surface, and the measurement surface is determined.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10172481A JPS582726A (en) | 1981-06-30 | 1981-06-30 | Sample surface determining method in analyzing device for liquid fluorescent x ray |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10172481A JPS582726A (en) | 1981-06-30 | 1981-06-30 | Sample surface determining method in analyzing device for liquid fluorescent x ray |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS582726A JPS582726A (en) | 1983-01-08 |
| JPS6352699B2 true JPS6352699B2 (en) | 1988-10-19 |
Family
ID=14308236
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10172481A Granted JPS582726A (en) | 1981-06-30 | 1981-06-30 | Sample surface determining method in analyzing device for liquid fluorescent x ray |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS582726A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5339868A (en) * | 1987-01-07 | 1994-08-23 | Nippon Steel Corporation | Bent pipe having sectional form of high strength |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5114812B2 (en) * | 1972-08-30 | 1976-05-12 | ||
| JPS5440132B2 (en) * | 1974-05-27 | 1979-12-01 |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5439705Y2 (en) * | 1974-07-18 | 1979-11-24 | ||
| JPS6126921Y2 (en) * | 1977-08-25 | 1986-08-12 |
-
1981
- 1981-06-30 JP JP10172481A patent/JPS582726A/en active Granted
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5114812B2 (en) * | 1972-08-30 | 1976-05-12 | ||
| JPS5440132B2 (en) * | 1974-05-27 | 1979-12-01 |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS582726A (en) | 1983-01-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| RU2012872C1 (en) | Method for obtaining image of object internal structure | |
| Schachman et al. | Ultracentrifuge studies with absorption optics. IV. Molecular weight determinations at the microgram level | |
| US4154669A (en) | Automatic electrophoresis apparatus | |
| US5468359A (en) | Method of determining presence of an analyte by isoelectric focusing | |
| US4688938A (en) | Method and apparatus for determining the contact angle of a drop of liquid placed on a solid or liquid horizontal substrate | |
| US4351709A (en) | Method of obtaining the mean electrophoretic mobility of particles | |
| US5784154A (en) | Electrophoresis separation in a capillary passage | |
| US4402612A (en) | Apparatus for detecting foreign particles in a liquid | |
| SU1386049A3 (en) | Infrared analyser for relative determination of quantities of some substances in sample of food products,mainly,in flour | |
| JPS5992330A (en) | Centrifugal analyzer | |
| EP0039701B1 (en) | Liquid flow photometer | |
| JPS6352699B2 (en) | ||
| FR2497399B1 (en) | DEVICE FOR DETECTING THE FOCUSING OF AN ELECTRON BEAM IN AN IMAGE TUBE AND METHOD FOR DETECTING AND ADJUSTING THIS FOCUS | |
| JPH0346777B2 (en) | ||
| JP4763868B2 (en) | Nephelometric detection unit with optical in-process control | |
| AU4336893A (en) | Detecting diamonds in a rock sample | |
| US4239612A (en) | Automatic electrophoresis apparatus | |
| Staudinger et al. | Quick optical measurement of particle distribution in a sedimentation apparatus | |
| US7262843B2 (en) | Method and device for correcting for the size and/or shape of a measuring volume in a chemical and/or biological sample | |
| US20070190661A1 (en) | Method and device for recording microscopic images | |
| RU197194U1 (en) | SCANNING DEVICE EXPRESS ANALYSIS OF CORES | |
| JP2000055842A (en) | X-ray image pick-up analysis method and device | |
| Longsworth | Improved electrophoresis apparatus for small volumes | |
| JP2746852B2 (en) | Transmitted light measurement device | |
| US3226556A (en) | Photosensitive liquid examining means for electrophoresis apparatus |