DE19728930A1 - Secondary multi-element standard - Google Patents
Secondary multi-element standardInfo
- Publication number
- DE19728930A1 DE19728930A1 DE19728930A DE19728930A DE19728930A1 DE 19728930 A1 DE19728930 A1 DE 19728930A1 DE 19728930 A DE19728930 A DE 19728930A DE 19728930 A DE19728930 A DE 19728930A DE 19728930 A1 DE19728930 A1 DE 19728930A1
- Authority
- DE
- Germany
- Prior art keywords
- element standard
- secondary multi
- standard according
- ray
- porous matrix
- 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- Withdrawn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
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
- G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions
- G01N23/2076—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions for spectrometry, i.e. using an analysing crystal, e.g. for measuring X-ray fluorescence spectrum of a sample with wavelength-dispersion, i.e. WDXFS
Abstract
Description
Die Erfindung betrifft die Bestimmung, die Speicherung, die Reproduktion und den Vergleich der relativen spektralen Effektivität von Meßeinrichtungen für die energiedispersive Röntgen analytik.The invention relates to the determination, storage, reproduction and comparison the relative spectral effectiveness of measuring devices for energy dispersive X-ray analytics.
Es ist bereits bekannt, zertifizierte Referenzmaterialien, u. a. radioaktive Quellen, geologisches und biologisches Material sowie Aerosole, zur Bestimmung von Effektivitäts-Werten für Meßeinrichtungen einzusetzen (J. L. Campbell, P. L. McGhee, Nucl. Instr. and Meth. A 248 (1986) 393; O. Valcovic, D. Ceccato, G. Moschini, S. Galassini, E. Menapace, Nucl. Instr. and Meth. B 89 (1994) 233; U. Wätjen, P.Maier-Komor, R. Pengo, N. I. Zaika, M. Budnar, V. Valkovic, Nucl. Instr. and Meth. B 99 (1995) 376). Nachteilig ist dabei, daß das Ergebnis voneinander unabhängige Einzelmessungen darstellt und daß die emittierten Röntgenlinien den niederenergetischen Analysierbereich nur ungenügend abdecken.It is already known to use certified reference materials, e.g. a. radioactive sources, geological and biological material as well as aerosols, for determining effectiveness values for Use measuring devices (J.L. Campbell, P.L. McGhee, Nucl. Instr. And Meth. A 248 (1986) 393; O. Valcovic, D. Ceccato, G. Moschini, S. Galassini, E. Menapace, Nucl. Instr. and Meth. B 89 (1994) 233; U. Wätjen, P.Maier-Komor, R. Pengo, N.I. Zaika, M. Budnar, V. Valkovic, Nucl. Instr. and Meth. B 99 (1995) 376). The disadvantage is that the result represents independent individual measurements and that the emitted X-ray lines the insufficiently cover the low-energy analysis range.
Es ist auch ein synthetischer Kompositionsstandard bekannt, der aus drei chemischen Elementen besteht, nämlich einer Dünnschicht (Element 1) auf bzw. unter einem Salz mit zwei Elementen (U. Wätjen, H. Bax, P. Rietveld, Nucl. Instr. and Meth. B 75 (1993) 131). Die emittierten Röntgenlinien genügen für eine größere Bandbreite jedoch nicht den Anforderungen für eine spektrale Effektivitätsbestimmung.There is also known a synthetic composition standard consisting of three chemical elements exists, namely a thin layer (element 1) on or under a salt with two elements (U. Wätjen, H. Bax, P. Rietveld, Nucl. Instr. And Meth. B 75 (1993) 131). The emitted However, X-ray lines do not meet the requirements for a larger bandwidth spectral effectiveness determination.
Der Erfindung liegt die Aufgabe zugrunde, eine Vielzahl von Meßpunkten zu erfassen und so die Bestimmung, Speicherung, Reproduktion und den Vergleich der relativen spektralen Effektivität von Meßeinrichtungen für die energiedispersive Röntgenanalytik rationell zu gestalten.The invention has for its object to detect a variety of measuring points and so the determination, storage, reproduction and comparison of the relative spectral Effectiveness of measuring devices for energy dispersive X-ray analysis rationally shape.
Erfindungsgemäß wird die Aufgabe mit einem sekundären Multielement-Standard gelöst, der aus einer porigen Matrix besteht mit einer darin deponierten Vielzahl von Komponenten zur Generierung des gewünschten Röntgenspektums. Die Komponenten liegen in der Matrix vorzugsweise als Metallsalze vor. Die Auswahl der Salze erfolgt anhand der interessierenden Röntgenenergien, in der vorliegenden Erfindung im Energiebereich 0,5 bis 15 keV.According to the invention the object is achieved with a secondary multi-element standard consists of a porous matrix with a large number of components deposited in it Generation of the desired X-ray spectrum. The components are in the matrix preferably as metal salts. The salts are selected on the basis of those of interest X-ray energies, in the present invention in the energy range 0.5 to 15 keV.
Die porige Matrix kann als Vlies oder Gewebe ausgeführt sein. Es kann aber auch ein saug fähiges analytisches Papier eingesetzt sein, vorteilhaft ein Chromatografiepapier. Es läßt sich auch ein naßfester Filterkarton verwenden.The porous matrix can be designed as a fleece or fabric. But it can also be a suction capable analytical paper, advantageously a chromatography paper. It can be also use a wet filter box.
Es werden vorzugsweise die in nachstehender Tabelle angegebenen Elemente verwendet, die in Form der dort bezeichneten Metallsalze eingesetzt werden. Dazu werden die Salze etwa mit der in der Tabelle genannten Menge in einem Liter Wasser gelöst.The elements specified in the table below are preferably used, which are described in Form of the metal salts referred to there are used. For this purpose the salts are mixed with the dissolved in one liter of water in the table.
Mit der erfindungsgemäßen Lösung lassen sich Effektivitätskurven aufnehmen, aus denen detaillierte Aussagen zur spektralen relativen Effektivität getroffen werden können. With the solution according to the invention, effectiveness curves can be recorded, from which detailed statements on spectral relative effectiveness can be made.
Die Erfindung wird nachfolgend an einem Ausführungsbeispiel näher erläutert. In der zugehörigen Zeichnung wird eine gemessene Intensitätsverteilung der charakteristischen Röntgenstrahlung des sekundären Multielement-Standards dargestellt, gemessen mittels Si(Li)-De tektor mit 25 µm Be-Fenster.The invention is explained in more detail below using an exemplary embodiment. In the accompanying drawing, a measured intensity distribution of the characteristic X-ray radiation of the secondary multi-element standard shown, measured using Si (Li) -De tector with 25 µm loading window.
Fig. 1 zeigt die Verteilung für eine Elementegruppe, die auf einem Träger enthalten ist, Fig. 1 shows the distribution for a group of elements that is included on a support,
Fig. 2 zeigt die Verteilung für eine andere Elementegruppe, die auf dem anderen Träger enthal ten ist. Fig. 2 shows the distribution for another group of elements, which is contained on the other carrier.
Der erfindungsgemäße sekundäre Multielement-Standard besteht aus flächigem Fasergebilde, in bevorzugter Ausführungsform aus saugfähigem analytischen Papier in Form von Chromato grafiepapier einer Dicke von etwa 0,2 mm.The secondary multi-element standard according to the invention consists of flat fiber structures, in a preferred embodiment of absorbent analytical paper in the form of chromato graphic paper about 0.2 mm thick.
Zur besseren Energieauflösung eng benachbarter Elemente besteht der sekundäre Multielement- Standard vorzugsweise aus zwei Stücken Chromatografiepapier. Die beiden Stücken des Chromatografiepapiers (Papier 1 und Papier 2) sind mit nachstehend angegebenen Metallsalzen versehen. Die hinter den Salzen in Klammern gesetzten Zahlen sind die vorteilhaften Mengen der Salze in Gramm, die einem Liter destillierten Wassers zugesetzt worden sind. Die beiden Chromatografiepapiere wurden in je einer der mit Salzen angereicherten Flüssigkeiten satt getränkt und anschließend getrocknet. In der dritten Spalte ist die für das Dotierungselement charakteristische Röntgenenergie angegeben.To improve the energy resolution of closely adjacent elements, there is a secondary multi-element Standard preferably from two pieces of chromatography paper. The two pieces of the Chromatography paper (Paper 1 and Paper 2) are with the metal salts shown below Mistake. The numbers in parentheses after the salts are the advantageous amounts of the salts, in grams, added to one liter of distilled water. The two Chromatography papers were saturated in one of the liquids enriched with salts soaked and then dried. In the third column is that for the doping element characteristic x-ray energy given.
Dabei dient die Verwendung des Zn-Salzes sowohl im Papier 1 als auch im Papier 2 dem Abgleich der Ergebnisse aus beiden Messungen, ggfs. kann dies anstelle von Zn auch über das Element S geschehen.The use of the Zn salt serves both in paper 1 and in paper 2 Comparison of the results from both measurements, if necessary Element S happen.
Claims (9)
8. Secondary multi-element standard according to claim 1, characterized in that the elements listed in the table below are contained in the carrier material in the form of the metal salts listed with approximately the proportion weighed in per liter of water.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19728930A DE19728930A1 (en) | 1997-07-07 | 1997-07-07 | Secondary multi-element standard |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19728930A DE19728930A1 (en) | 1997-07-07 | 1997-07-07 | Secondary multi-element standard |
Publications (1)
Publication Number | Publication Date |
---|---|
DE19728930A1 true DE19728930A1 (en) | 1999-01-14 |
Family
ID=7834873
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
DE19728930A Withdrawn DE19728930A1 (en) | 1997-07-07 | 1997-07-07 | Secondary multi-element standard |
Country Status (1)
Country | Link |
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DE (1) | DE19728930A1 (en) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102004018260B4 (en) * | 2003-04-16 | 2006-04-20 | Horiba Ltd. | Collection filter and method for the quantitative analysis of airborne suspended particles |
DE102005054443A1 (en) * | 2005-11-15 | 2007-05-31 | Fachhochschule Münster | Standard set for calibration |
US8696201B2 (en) | 2010-11-19 | 2014-04-15 | Siemens Aktiengesellschaft | Device and method for calibrating an X-ray detector, calibration apparatus and X-ray apparatus |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE2716689A1 (en) * | 1977-04-15 | 1978-10-19 | Ibm Deutschland | Calibration standard prodn. for X=ray fluorescence analysis of solids - by dripping plastics dispersion containing impurity atoms on to rotating substrate and then hardening film |
US4728792A (en) * | 1985-05-20 | 1988-03-01 | Warner Gerald T | Sorption sheet for sorbing a plurality of discrete samples and method of producing such a sorption sheet and use thereof |
-
1997
- 1997-07-07 DE DE19728930A patent/DE19728930A1/en not_active Withdrawn
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE2716689A1 (en) * | 1977-04-15 | 1978-10-19 | Ibm Deutschland | Calibration standard prodn. for X=ray fluorescence analysis of solids - by dripping plastics dispersion containing impurity atoms on to rotating substrate and then hardening film |
US4728792A (en) * | 1985-05-20 | 1988-03-01 | Warner Gerald T | Sorption sheet for sorbing a plurality of discrete samples and method of producing such a sorption sheet and use thereof |
Non-Patent Citations (5)
Title |
---|
2-247550 A * |
HAUPT,O., SCHAEFER,C., STRAUSS,S., et.al.: Production of calibration standards for x-ray fluorescence analysis of aerosol particles precipitated on different filter materials. In: Fresenius J. Anal Chem., 1996, 355, S.375-378 * |
JP 59-212743 A.,In: Patents Abstracts of Japan, P-348,April 12,1985,Vol.9,No.83 * |
JP Patents Abstracts of Japan: 55- 20478 A * |
PANG,Thomas W.S., D'ONOFRIO,Anthony M., LO,Francis B., et.al.: Precipitation Technique to Prepare Thin-film Standards of Lead and Zinc for X-Ray Fluorescence Spectrometry, 1987, 16 (1), 45-49 * |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102004018260B4 (en) * | 2003-04-16 | 2006-04-20 | Horiba Ltd. | Collection filter and method for the quantitative analysis of airborne suspended particles |
DE102005054443A1 (en) * | 2005-11-15 | 2007-05-31 | Fachhochschule Münster | Standard set for calibration |
US7960177B2 (en) | 2005-11-15 | 2011-06-14 | Fachhochschule Münster | Set of calibration standards |
US8696201B2 (en) | 2010-11-19 | 2014-04-15 | Siemens Aktiengesellschaft | Device and method for calibrating an X-ray detector, calibration apparatus and X-ray apparatus |
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Legal Events
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OM8 | Search report available as to paragraph 43 lit. 1 sentence 1 patent law | ||
8110 | Request for examination paragraph 44 | ||
8125 | Change of the main classification |
Ipc: G01N 23/00 |
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8130 | Withdrawal |