WO2003016888A2 - Electrode utilisee comme support d'echantillon dans le cadre de mesures de fluorescence x a reflexion totale (txrf) - Google Patents

Electrode utilisee comme support d'echantillon dans le cadre de mesures de fluorescence x a reflexion totale (txrf) Download PDF

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Publication number
WO2003016888A2
WO2003016888A2 PCT/DE2002/002933 DE0202933W WO03016888A2 WO 2003016888 A2 WO2003016888 A2 WO 2003016888A2 DE 0202933 W DE0202933 W DE 0202933W WO 03016888 A2 WO03016888 A2 WO 03016888A2
Authority
WO
WIPO (PCT)
Prior art keywords
electrode
specimen
use according
sample
txrf
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.)
Ceased
Application number
PCT/DE2002/002933
Other languages
German (de)
English (en)
Other versions
WO2003016888A3 (fr
Inventor
Simone Griesel
Rüdiger KIEHN
Andreas Prange
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
GKSS Forshungszentrum Geesthacht GmbH
Original Assignee
GKSS Forshungszentrum Geesthacht GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority claimed from DE10232825A external-priority patent/DE10232825A1/de
Application filed by GKSS Forshungszentrum Geesthacht GmbH filed Critical GKSS Forshungszentrum Geesthacht GmbH
Publication of WO2003016888A2 publication Critical patent/WO2003016888A2/fr
Publication of WO2003016888A3 publication Critical patent/WO2003016888A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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

Definitions

  • Electrode as a sample holder for TXRF measurements
  • the invention relates to the use of an electrode for X-ray fluorescence spectroscopy, in particular total reflection X-ray fluorescence spectroscopy.
  • a salt matrix separation and an enrichment of the trace elements is necessary.
  • the element traces can be separated from the salt matrix by means of complexing with sodium dibenzyldithiocarbamate.
  • the trace elements are then concentrated by reverse phase chromatography.
  • This sample preparation is possible for the simultaneous analysis of 13 elements, in particular vanadium, manganese, iron, cobalt, nickel, copper, zinc, selenium, mercury, lead, uranium, molybdenum and cadium.
  • sample preparation harbors a large number of contamination risks due to the large number of individual steps and chemical additions. Furthermore, this sample preparation is very time-consuming, but also in terms of consumables.
  • an electrochemical analysis of saline samples with the so-called. Stripping voltametry done.
  • the elements to be analyzed are enriched in a hanging drop of mercury and then stripped off again. The analysis takes place during the stripping step.
  • the analysis is possible for 20 different elements, of which currently. six can be analyzed simultaneously (copper, lead, cadimium, nickel, cobalt, zinc).
  • the object is achieved according to the invention by using an electrode as a sample carrier for X-ray fluorescence spectroscopy, in particular total reflection X-ray fluorescence spectroscopy.
  • the invention combines an electrochemical sample preparation and (total reflection) X-ray fluorescence spectroscopy.
  • the salt matrix is separated and the trace elements are enriched in one step.
  • the electrode first becomes one Exposed to electrode deposition, for example in an electrolytic cell, so that trace elements accumulate on the surface of the electrode.
  • These deposits of trace elements can be analyzed directly after the electrode deposition of the electrode, ie without further treatment by means of the (total reflection) x-ray fluorescence spectroscopy.
  • the electrode can be exposed to simultaneous electrode deposition of over 20 elements, e.g.
  • the invention has a low risk of contamination and a low consumption of chemicals.
  • no mercury is used for the sample preparation.
  • the invention is applicable on site, since the sea water sample preparation for (total reflection) X-ray fluorescence spectroscopy takes place in one step.
  • the trace elements of a saline matrix can accumulate on the electrode when the electrode and / or the sample carrier are exposed to an electrode position, preferably in a liquid, in particular saline, atmosphere.
  • the electrode has a specimen for better handling.
  • the one from the electrode after the Electrode deposition detachable specimen is used directly as a specimen carrier for X-ray fluorescence measurement.
  • the electrode is preferably conical and / or the sample body is disc-shaped.
  • the electrode in particular the tip of the electrode, is made of Teflon and / or the sample .
  • Body made of glassy carbon.
  • the electrode and / or the specimen are placed in an electrolytic cell.
  • a uniform distribution of the trace elements is achieved if the electrode and / or the specimen are rotated or rotated in the electrolytic cell.
  • Fig. 4 shows an energy spectrum of estuary water with electrode deposition
  • Fig. 5 shows an intensity curve for measurements of different elements when changing the measurement angle.
  • FIG. 1 schematically shows the structure of an electrolytic cell 10 with a reference electrode 12, for example made of silver (Ag) or silver chloride (AgCl), and a counter electrode 11, for example with a platinum wire.
  • a reference electrode 12 for example made of silver (Ag) or silver chloride (AgCl)
  • AgCl silver chloride
  • Another electrode 15 is connected between the counter electrode 11 and the reference electrode 12 via a voltage 16.
  • the electrode 15 has an electrode tip 17.
  • the electrodes 11, 12, 15 are immersed in a container 13 filled with water and a saline matrix 14.
  • a disk-shaped sample body 18 is formed on the electrode tip 17 of the electrode 15 and is rotated in the water 14 during the deposition of trace elements of the saline matrix.
  • the sample body 18 is preferably made of glassy carbon.
  • the electrode tip 17 made of Teflon serves as a holder for the sample body 18.
  • the surface of the sample body 18 is used in the electrolytic cell 10 as the electrode surface.
  • a voltage is generated by the voltage 16 between the counter electrode 11 and the electrode 15 so that trace elements can accumulate on the sample body 18.
  • the separation potential was between 0 and -2,500 mV in tests carried out and -2,000 mV in estuarine water.
  • the electrode deposition time varied between 1 and 60 minutes, with a deposition time of 30 minutes proving to be optimal.
  • the specimen 18 After deposition of trace elements from the salt matrix on the surface of the specimen 18, the specimen 18 is removed from the electrode tip 17 and introduced into a (total refl exi ons) X-ray fluorescence spectrometer, TXRF-Spektro eter for short (FIG. 2).
  • FIG. 2 shows the schematic structure of a TXRF spectrometer for the detection of trace elements on the sample body 18.
  • An X-ray tube 21 is used to generate a tube beam 22 which, after leaving the X-ray tube 21, passes through a primary beam fi 1 ter 23, a monochromator 24 and a beam limiting diaphragm 25.
  • the X-ray beam 22 is then directed onto the surface of the sample body or sample carrier 18.
  • the X-ray fluorescence beam is detected by means of a detector 27.
  • the detector 27 has furthermore via a detector diaphragm 26.
  • the X-ray beam 22 reflected on the sample body 18 is absorbed by a beam catcher 28.
  • FIGS. 3 and 4 show TXRF spectra (energy spectra) of estuarine water (salinity 14 g / 1) as reference material without electrode deposition (FIG. 3) and with electrode deposition (FIG. 4).
  • the measurement results are quantified using element-specific yield factors and by using an internal standard, which is deposited together with the other elements.
  • FIG. 5 shows the intensity curve for the measurement of different elements when the measurement angle changes in a TXRF spectrometer (FIG. 2).
  • TXRF spectrometer To the separation behavior of the.
  • several TXRF measurements were carried out at different penetration angles on the same sample. The results show a similar course of identity for the different elements lead, iron, cobalt, copper, arsenic and uranium. This means that the deposited metal layer shows a homogeneous composition on the sample body.
  • An internal standard can also be used to evaluate the measurement results. From the course of the Intenti tmaschineskurve can be concluded that the elements are deposited as thin layers on the sample carrier.

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)
  • Sampling And Sample Adjustment (AREA)

Abstract

L'invention concerne une électrode (15) utilisée comme support d'échantillon pour la spectroscopie de fluorescence X, en particulier la spectroscopie de fluorescence X à réflexion totale.
PCT/DE2002/002933 2001-08-10 2002-08-08 Electrode utilisee comme support d'echantillon dans le cadre de mesures de fluorescence x a reflexion totale (txrf) Ceased WO2003016888A2 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DE10138320.7 2001-08-10
DE10138320 2001-08-10
DE10232825.0 2002-07-19
DE10232825A DE10232825A1 (de) 2001-08-10 2002-07-19 Elektrode als Probenträger für TXRF-Messungen

Publications (2)

Publication Number Publication Date
WO2003016888A2 true WO2003016888A2 (fr) 2003-02-27
WO2003016888A3 WO2003016888A3 (fr) 2003-10-09

Family

ID=26009877

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/DE2002/002933 Ceased WO2003016888A2 (fr) 2001-08-10 2002-08-08 Electrode utilisee comme support d'echantillon dans le cadre de mesures de fluorescence x a reflexion totale (txrf)

Country Status (1)

Country Link
WO (1) WO2003016888A2 (fr)

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE1004446A3 (fr) * 1990-06-13 1992-11-24 Solvay Installation pour l'analyse d'un materiau.

Also Published As

Publication number Publication date
WO2003016888A3 (fr) 2003-10-09

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