DE19806168A1 - X-ray measuring cell capable of direct flow - Google Patents
X-ray measuring cell capable of direct flowInfo
- Publication number
- DE19806168A1 DE19806168A1 DE1998106168 DE19806168A DE19806168A1 DE 19806168 A1 DE19806168 A1 DE 19806168A1 DE 1998106168 DE1998106168 DE 1998106168 DE 19806168 A DE19806168 A DE 19806168A DE 19806168 A1 DE19806168 A1 DE 19806168A1
- Authority
- DE
- Germany
- Prior art keywords
- measuring cell
- ray
- samples
- cell
- cell according
- 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.)
- Withdrawn
Links
- 210000004027 cell Anatomy 0.000 claims description 32
- 239000007788 liquid Substances 0.000 claims description 9
- 238000005259 measurement Methods 0.000 claims description 7
- 229920000642 polymer Polymers 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 239000000919 ceramic Substances 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 3
- 239000012876 carrier material Substances 0.000 claims description 3
- 210000005056 cell body Anatomy 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims description 2
- 230000001419 dependent effect Effects 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 5
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000011835 investigation Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000004094 surface-active agent Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000011514 reflex Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000011144 upstream manufacturing 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
- G01N23/20—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 using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
-
- 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
- G01N23/02—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 transmitting the radiation through the material
Landscapes
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
Description
Die Erfindung betrifft eine frei durchströmbare Meßzelle, mit der Röntgeninten sitäten winkelabhängig von in gasförmigen oder flüssigen Trägermaterialien enthaltenen Proben gemessen werden können.The invention relates to a freely flowable measuring cell with the X-ray ink depending on the angle of in gaseous or liquid carrier materials contained samples can be measured.
In modernen Röntgendiffraktometern werden für die Vermessung von polykristal linen Proben (Pulvern) die verschiedensten Probenaufnahmen und Meßzellen eingesetzt. Die gängigsten Probenaufnahmen für Messungen in Transmission sind ein- oder zweiseitig abgeschmolzene Kapillarröhrchen oder Folien, zwischen denen das Pulver fixiert wird. Für Reflexionsmessungen werden die Proben in der Regel auf flachen Probenträgern, z. B. aus Edelstahl, Quarz, Polymer, Glas etc., aufgestreut oder als Flachpräparat in Vertiefungen im Probenträger präpariert.In modern X-ray diffractometers are used for the measurement of polycrystals Linen samples (powders) a wide variety of sample holders and measuring cells used. The most common sample recordings for measurements in transmission are capillary tubes or foils melted off on one or both sides, between which the powder is fixed. The samples are usually used for reflection measurements on flat sample carriers, e.g. B. made of stainless steel, quartz, polymer, glass etc., sprinkled on or prepared as a flat preparation in wells in the sample holder.
Einige Hersteller, z. B. Johanna Otto (Johanna Otto GmbH, Rottenburger Straße 3, D-72411 Bodelshausen, Deutschland), Anton Paar (Anton Paar KG, Kärntner Straße 322, A-8054 Graz, Österreich) oder Stoe (Stoe & Cie GmbH, Hilpert straße 10, D-64295 Darmstadt, Deutschland) bieten kommerziell Zellen in Form von Tieftemperatur- und Hochtemperaturkammern bzw. -aufsätzen an, in denen Proben thermisch behandelt werden können, wobei die Proben in situ vermessen werden können. Weiterhin ist die Zuführung von Reaktionsgasen möglich, so daß Reaktionen an Feststoffen in situ bei entsprechenden Temperaturen möglich sind. Die Probe liegt dabei stationär auf dem Probenträger und wird einer Reaktivgas atmosphäre, Temperatur, Licht, etc. oder einem Gradienten dieser physikalisch chemischen Parameter ausgesetzt. Neben den kommerziell erhältlichen Zellen wurden auch von einzelnen Forschungsgruppen und von Firmen Reaktionszellen entwickelt, in denen Feststoff in situ unter Reaktionsbedingungen und/oder auch in einem Reaktivgas- oder Flüssigkeitsstrom röntgenographisch untersucht werden können (B.S. Clausen, G. Steffensen, B. Fabius, J. Villadsen, R. Feidenhansl, H. Topsoe, J. Catal 132 (2) (1991) 524; L. Grabaek, B.S. Clausen, G. Steffensen, H. Some manufacturers, e.g. B. Johanna Otto (Johanna Otto GmbH, Rottenburger Straße 3, D-72411 Bodelshausen, Germany), Anton Paar (Anton Paar KG, Carinthia Straße 322, A-8054 Graz, Austria) or Stoe (Stoe & Cie GmbH, Hilpert Strasse 10, D-64295 Darmstadt, Germany) commercially offer cells in the form of low-temperature and high-temperature chambers or attachments in which Samples can be treated thermally, the samples being measured in situ can be. Furthermore, the supply of reaction gases is possible, so that Reactions to solids are possible in situ at appropriate temperatures. The sample is stationary on the sample holder and becomes a reactive gas atmosphere, temperature, light, etc. or a gradient of these physically exposed to chemical parameters. In addition to the commercially available cells have also been used by individual research groups and companies' reaction cells developed in which solid in situ under reaction conditions and / or in a reactive gas or liquid flow can be examined by X-ray analysis (B.S. Clausen, G. Steffensen, B. Fabius, J. Villadsen, R. Feidenhansl, H. Topsoe, J. Catal 132 (2) (1991) 524; L. Grabaek, B.S. Clausen, G. Steffensen, H.
Topsoe, Mater. Sci. Forum 133-136 (1993) 255; I.J. Shannon, T. Maschmeyer, G. Sankar, J.M. Thomas, R.D. Oldroyd, M. Sheehy, D. Madill, A.M. Waller, R.P. Townsend, Catal. Lett. 44 (1, 2) (1997) 23; T. Fawcett, Chemtech 17 (9) (1987) 564; D. Cunningham, R.J. Davey, K.J. Roberts, J.N. Sherwood, T. Shripathi, J. Crystal Growth 99 (1990) 1065; K.J. Roberts, J. Crystal Growth 130 (1993) 657). Gemeinsam ist allen diesen Zellen, daß die Feststoffprobe im Gegensatz zu der hier beschriebenen Erfindung fest in der Zelle fixiert wird und lediglich von einem Fluid umspült wird.Topsoe, Mater. Sci. Forum 133-136 (1993) 255; I.J. Shannon, T. Maschmeyer, G. Sankar, J.M. Thomas, R.D. Oldroyd, M. Sheehy, D. Madill, A.M. Waller, R.P. Townsend, Catal. Lett. 44 (1, 2) (1997) 23; T. Fawcett, Chemtech 17 (9) (1987) 564; D. Cunningham, R.J. Davey, K.J. Roberts, J.N. Sherwood, T. Shripathi, J. Crystal Growth 99 (1990) 1065; K.J. Roberts, J. Crystal Growth 130 (1993) 657). Common to all these cells is that the solid sample is in contrast to the one here described invention is firmly fixed in the cell and only by a fluid is washed around.
Es besteht jedoch ein Bedarf, Proben nicht nur als stationäre Feststoffe zu untersuchen, sondern auch in gasförmiger oder flüssiger Matrix während des Durchströmens einer Meßzelle.However, there is a need to add samples not only as stationary solids investigate, but also in gaseous or liquid matrix during the Flowing through a measuring cell.
Es ist uns gelungen, eine Probenzelle zu konstruieren, mit der es möglich ist,
flüssige oder gasförmige Proben im Durchfluß durch die Probenzelle zu
untersuchen. Damit können insbesondere auch die folgenden Substanzen
untersucht werden:
We have succeeded in constructing a sample cell with which it is possible to examine liquid or gaseous samples as they flow through the sample cell. The following substances can be examined in particular:
- a) Substanzen, die außerhalb einer flüssigen oder gasförmigen Matrix keine für eine Messung ausreichend lange Lebensdauer haben, da ihre Struktur ohne das umgebende Lösungsmittel oder Gas verändert wird.a) Substances that do not exist outside of a liquid or gaseous matrix have a measurement long enough lifespan, because their structure without the surrounding solvent or gas is changed.
- b) Substanzen, die sehr kurze Lebensdauern an sich haben. Dies ist durch einen kontinuierlichen Flußbetrieb mit festen Verweilzeiten möglich (Prinzip eines kontinuierlichen Rohrreaktors), da hierdurch für jede gewünschte Akkumula tionszeit eines beliebigen Umsatzpunktes der Reaktion Daten gesammelt werden können. Durch Variation der Länge und/oder der Strömungsgeschwindigkeit eines der Meßzelle vorgeschalteten Rohrrektors können zu jedem beliebigen Zeitpunkt der Reaktion unabhängig von der Reaktionsgeschwindigkeit über lange Zeiträume vom selben Reaktionspunkt Daten aufgenommen werden. b) Substances that have very short lifetimes. This is through one continuous river operation with fixed dwell times possible (principle of one continuous tube reactor), as this means that for every desired accumulator data of any reaction point of the reaction can. By varying the length and / or the flow rate one of the measuring cells upstream of the tube reactor can be used for any Time of the reaction regardless of the reaction rate long time periods of data are recorded from the same reaction point.
- c) Substanzen, die routinemäßig bei kontinuierlichem Reaktorbetrieb überprüft werden müssen. Durch das Durchflußkonzept kann kontinuierlich Probe entnommen werden.c) Substances that are routinely checked during continuous reactor operation Need to become. Due to the flow concept, the sample can be continuously be removed.
Die erfindungsgemäße Probenzelle besteht aus einem Körper mit zwei oder mehr Öffnungen, die zum Einleiten oder Ausleiten der Probe geeignet sind. In dem Körper sind zwei oder mehr Fenster angebracht, durch die eine Untersuchung der Probe mit Röntgenstrahlung möglich ist. Der Meßzellenkörper besteht bevorzugt aus Polymer, Glas, Keramik oder Metall. Mit mechanischen Verschiebungs einrichtungen kann die Zelle in den Fokus eines Röntgenstrahls justiert werden. Als röntgenstrahldurchlässige Fenster werden bevorzugt Fenster in Form von Folien aus Polymer, Glas, Keramik oder Metall eingesetzt. Mit der Meßzelle können Röntgenintensitätsmessungen sowohl in Transmission als auch in Reflexion vorgenommen werden, wobei die Proben in einem gasförmigen oder flüssigen Trägermaterial die Röntgenzelle durchströmen.The sample cell according to the invention consists of a body with two or more Openings that are suitable for introducing or discharging the sample. By doing Two or more windows are attached through which an examination of the body X-ray sample is possible. The measuring cell body is preferred made of polymer, glass, ceramic or metal. With mechanical displacement the cell can be adjusted in the focus of an x-ray device. As X-ray transparent windows are preferred windows in the form of foils made of polymer, glass, ceramic or metal. With the measuring cell X-ray intensity measurements in both transmission and reflection be made, the samples in a gaseous or liquid Carrier material flow through the X-ray cell.
Die in Fig. 1 dargestellte Zelle besitzt einen Auslaß und einen Einlaß und zwei röntgentransparente Polymer-Fenster. Die Zelle ist auf einem beweglichen Goniometerkopf montiert: Durch zwei senkrecht zueinander angeordnete Schlitten mit Mikrometertrieb kann die Zelle in den Fokus des Röntgenstrahls justiert werden.The cell shown in Fig. 1 has an outlet and an inlet and two x-ray transparent polymer windows. The cell is mounted on a movable goniometer head: the cell can be adjusted in the focus of the X-ray beam by means of two slides with a micrometer drive arranged perpendicular to each other.
Für die Synthese von Kompositphasen ähnlich dem mesoporösen Silicat MCM-41 (J.S. Beck, U.S. Patent 5,507,296 (1991) C.T. Kresge, M.E. Leonowicz, W.J. Roth, J.C. Vartuli, J.S. Beck, Nature 359 (1992) 710) wurden Metallprecursor lösungen mit Tensidlösungen vermischt und der Verlauf der Reaktion verweil zeitabhängig im flüssigen Medium verfolgt (Fig. 2).For the synthesis of composite phases similar to the mesoporous silicate MCM-41 (JS Beck, US Patent 5,507,296 (1991) CT Kresge, ME Leonowicz, WJ Roth, JC Vartuli, JS Beck, Nature 359 (1992) 710), metal precursor solutions were mixed with surfactant solutions and the course of the reaction remains in the liquid medium as a function of time ( FIG. 2).
Mesophasen verändern sich oft bei Trocknungsprozessen. Durch die Zelle sind stationäre Untersuchungen flüssiger Proben möglich (vergl. Fig. 3). Das Beispiel zeigt, wie sehr sich Materialien unter Synthesebedingungen und nach dem Abtrennen und Trocknen unterscheiden können. Hier kann deutlich die Schrumpfung der Einheitszellen des Materials beim Trocknen anhand der Verschiebung der Reflexe zu größeren 2θ Werten beobachtet werden. Bei einer anschließenden Calcinierung schrumpft das Material nochmals, was auf die Kondensation zusätzlicher Hydroxylgruppen zurückgeführt werden kann.Mesophases often change during drying processes. Through the cell, stationary examinations of liquid samples are possible (see Fig. 3). The example shows how much materials can differ under synthesis conditions and after separation and drying. The shrinkage of the unit cells of the material during drying can be clearly observed here by shifting the reflections to larger 2θ values. In a subsequent calcination, the material shrinks again, which can be attributed to the condensation of additional hydroxyl groups.
Bei der Synthese von MCM-41 wird einer Lösung von Tensiden in alkalischer Lösung Tetraethylorthosilicat zugegeben (J.S. Beck, U.S. Patent 5,507,296 (1991), C.T. Kresge, M.E. Leonowicz, W.J. Roth, J.C. Vartuli, J.S. Beck, Nature 359 (1992) 710). Die durch Hydrolyse ausfallende Kieselsäure lagert sich aufgrund von elektrostatischen Wechselwirkungen bevorzugt an der Oberfläche von Tensid micellen an. Aufgrund von Ladungsdichtenänderungen während der Kondensation richten sich die Tensidmoleküle als hexagonal angeordnete Stäbchen aus, zwischen denen die weitere Kondensation der Kieselsäure stattfindet (J.S. Beck, J.C. Vartuli, W.J. Roth, M.E. Leonowicz, C.T. Kresge, K.D. Schmitt, C.T.-W. Chu, D.H. Olsen, E.W. Sheppard, S.B. McCullen, J.B. Higgins, J.L. Schlenker, J. Am. Chem. Soc. 114 (1992) 10834; A. Monnier, F. Schüth, Q. Huo, D. Kumar, D. Margolese, R.S. Maxwell, G.D. Stucky, M. Krishnamurty, P. Petroff, A. Firouzi, M. Janicke, B.F. Chmelka, Science 261 (1993) 1299). Auf diese Weise wird MCM-41 gebildet (vergl. Fig. 4). In the synthesis of MCM-41, tetraethyl orthosilicate is added to a solution of surfactants in alkaline solution (JS Beck, US Patent 5,507,296 (1991), CT Kresge, ME Leonowicz, WJ Roth, JC Vartuli, JS Beck, Nature 359 (1992) 710) . The silicic acid precipitated by hydrolysis preferentially attaches to the surface of surfactant micelles due to electrostatic interactions. Due to changes in charge density during the condensation, the surfactant molecules align as hexagonal rods between which the further condensation of the silica takes place (JS Beck, JC Vartuli, WJ Roth, ME Leonowicz, CT Kresge, KD Schmitt, CT-W. Chu, DH Olsen, EW Sheppard, SB McCullen, JB Higgins, JL Schlenker, J. Am. Chem. Soc. 114 (1992) 10834; A. Monnier, F. Schüth, Q. Huo, D. Kumar, D. Margolese, RS Maxwell , DG Stucky, M. Krishnamurty, P. Petroff, A. Firouzi, M. Janicke, BF Chmelka, Science 261 (1993) 1299). In this way, MCM-41 is formed (see Fig. 4).
Aus einer Reaktionslösung wurden nach Zugabe von Tetraethylorthosilicat nach 15 s, 90 s und 180 s Proben gezogen und in die hier beschriebene Meßzelle eingespritzt. Die Proben wurden dann statisch vermessen. Die Graphik zeigt den zeitlichen Verlauf der MCM-41 Bildung. Bereits nach 90 s sind die für MCM-41 typischen Röntgenreflexe im Ansatz zu beobachten. Nach 180 s ist das Material gut kristallisiert und die 100, 110 und 200 Reflexe sind deutlich ausgebildet.After addition of tetraethyl orthosilicate after 15 s, a reaction solution 90 s and 180 s samples were taken and placed in the measuring cell described here injected. The samples were then measured statically. The graphic shows the MCM-41 formation over time. The MCM-41 is already there after 90 s to observe typical X-ray reflexes in the approach. The material is finished after 180 s well crystallized and the 100, 110 and 200 reflections are clearly formed.
Schwerlösliche Salze bilden sich sehr schnell nach kurzen Reaktionszeiten. Durch Untersuchungen unter Kopplung mit einem Rohrreaktorsystem konnten Diffraktogramme über den Verlauf ihrer Bildung aufgenommen werden. Direkt vor der Reaktionszelle wurden eine Barium- und eine Sulfatlösung zusammengeführt und gemischt. Die Lösung strömte dann durch die Reaktionszelle. Nach 300 ms Reaktionszeit befand sich die Reaktionslösung in der Meßzelle und wurde röntgenographisch vermessen. Die Graphik zeigt, daß bereits Bariumsulfat ausgefallen ist. Als Vergleich ist das Röntgendiagramm einer pulverförmigen Bariumsulfatprobe gezeigt, die unter Standardbedingungen vermessen wurde. Das Beispiel zeigt, daß sich die Meßzelle für die Untersuchung sehr schneller Prozesse eignet, die mit konventionellen Röntgentechniken nicht erfaßt werden können (vergl. Fig. 5).Poorly soluble salts form very quickly after short reaction times. Through investigations coupled with a tubular reactor system, diffractograms over the course of their formation could be recorded. A barium and a sulfate solution were brought together and mixed directly in front of the reaction cell. The solution then flowed through the reaction cell. After a reaction time of 300 ms, the reaction solution was in the measuring cell and was measured by X-ray. The graphic shows that barium sulfate has already precipitated. For comparison, the X-ray diagram of a powdered barium sulfate sample is shown, which was measured under standard conditions. The example shows that the measuring cell is suitable for the investigation of very fast processes that cannot be detected with conventional X-ray techniques (see FIG. 5).
Claims (6)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE1998106168 DE19806168A1 (en) | 1998-02-14 | 1998-02-14 | X-ray measuring cell capable of direct flow |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE1998106168 DE19806168A1 (en) | 1998-02-14 | 1998-02-14 | X-ray measuring cell capable of direct flow |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE19806168A1 true DE19806168A1 (en) | 1999-08-26 |
Family
ID=7857783
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DE1998106168 Withdrawn DE19806168A1 (en) | 1998-02-14 | 1998-02-14 | X-ray measuring cell capable of direct flow |
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| Country | Link |
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| DE (1) | DE19806168A1 (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3144559A (en) * | 1960-09-08 | 1964-08-11 | Exxon Research Engineering Co | Cell means for soft X-ray source |
| GB1109276A (en) * | 1964-09-18 | 1968-04-10 | Radiologie Cie Gle | Improvements in x-ray spectrometers |
| DE2621027A1 (en) * | 1976-05-12 | 1977-11-24 | Kernenergieverwert Ges Fuer | DEVICE FOR QUANTITATIVE IN-LINE ROENTE GENE FLUORESCENT ANALYSIS OF SLURES |
| GB2069688A (en) * | 1980-02-15 | 1981-08-26 | Coal Industry Patents Ltd | Assessing the concentration of mineral matter in coal-derived liquids |
| DE3718230A1 (en) * | 1986-06-02 | 1987-12-03 | Outokumpu Oy | DEVICE FOR STABILIZING THE MEASURING GEOMETRY OF AN ANALYZER |
| EP0269432A2 (en) * | 1986-11-25 | 1988-06-01 | Petro-Canada | Analyzer for fluid within piping |
| DE3404226C2 (en) * | 1983-02-07 | 1992-05-27 | E.I. Du Pont De Nemours & Co., Wilmington, Del., Us |
-
1998
- 1998-02-14 DE DE1998106168 patent/DE19806168A1/en not_active Withdrawn
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3144559A (en) * | 1960-09-08 | 1964-08-11 | Exxon Research Engineering Co | Cell means for soft X-ray source |
| GB1109276A (en) * | 1964-09-18 | 1968-04-10 | Radiologie Cie Gle | Improvements in x-ray spectrometers |
| DE2621027A1 (en) * | 1976-05-12 | 1977-11-24 | Kernenergieverwert Ges Fuer | DEVICE FOR QUANTITATIVE IN-LINE ROENTE GENE FLUORESCENT ANALYSIS OF SLURES |
| GB2069688A (en) * | 1980-02-15 | 1981-08-26 | Coal Industry Patents Ltd | Assessing the concentration of mineral matter in coal-derived liquids |
| DE3404226C2 (en) * | 1983-02-07 | 1992-05-27 | E.I. Du Pont De Nemours & Co., Wilmington, Del., Us | |
| DE3718230A1 (en) * | 1986-06-02 | 1987-12-03 | Outokumpu Oy | DEVICE FOR STABILIZING THE MEASURING GEOMETRY OF AN ANALYZER |
| EP0269432A2 (en) * | 1986-11-25 | 1988-06-01 | Petro-Canada | Analyzer for fluid within piping |
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