Investigations into the role of modifiers for entrapment of hydrides in Flow injection hydride generation electrothermal atomic absorption spectrometry as exemplified by the determination of germanium

B. O. Hilligsøe, Jens E.T. Andersen, Elo H. Hansen

Research output: Contribution to journalArticle

18 Citations (Scopus)

Abstract

Pd-conditioned graphite tubes, placed in the furnace of an AAS instrument, were used for entrapment of germane as generated in an associated flow-injection system. Two different approaches were tested with the ultimate aim of allowing multiple determinations, i.e., introduction of the modifier as a Pd salt solution, and use of electrolytically Pd pre-coated tubes. While the former treatment resulted in satisfactory analytical performance, although requiring separate regeneration of the tubes prior to each sampling sequence, the electrolytically pre-coated tubes did not function satisfactorily. This in turn led to a closer investigation as to the function of Pd in entrapping hydrides and releasing the analyte. Based on an evaluation of the behaviour of the two types of tubes, supplemented by scanning tunnelling microscopy studies of tubes with and without modifier and treated in different ways, it is shown that heating at 2600°C results in a physical- chemical change of the modifier in the electrolytically coated tubes; however, this change leads only to a loss of the ability of the modifier to entrap the hydrides, while the stabilizing effect is maintained.

Original languageEnglish
Pages (from-to)585-588
Number of pages4
JournalJournal of Analytical Atomic Spectrometry
Volume12
Issue number5
DOIs
Publication statusPublished - Jan 1 1997

Fingerprint

Germanium
Atomic absorption spectrometry
Hydrides
Graphite
Scanning tunneling microscopy
Furnaces
Salts
Sampling
Heating

All Science Journal Classification (ASJC) codes

  • Analytical Chemistry
  • Spectroscopy

Cite this

@article{f2896e9d83d54736912a3ec5c41d39ba,
title = "Investigations into the role of modifiers for entrapment of hydrides in Flow injection hydride generation electrothermal atomic absorption spectrometry as exemplified by the determination of germanium",
abstract = "Pd-conditioned graphite tubes, placed in the furnace of an AAS instrument, were used for entrapment of germane as generated in an associated flow-injection system. Two different approaches were tested with the ultimate aim of allowing multiple determinations, i.e., introduction of the modifier as a Pd salt solution, and use of electrolytically Pd pre-coated tubes. While the former treatment resulted in satisfactory analytical performance, although requiring separate regeneration of the tubes prior to each sampling sequence, the electrolytically pre-coated tubes did not function satisfactorily. This in turn led to a closer investigation as to the function of Pd in entrapping hydrides and releasing the analyte. Based on an evaluation of the behaviour of the two types of tubes, supplemented by scanning tunnelling microscopy studies of tubes with and without modifier and treated in different ways, it is shown that heating at 2600°C results in a physical- chemical change of the modifier in the electrolytically coated tubes; however, this change leads only to a loss of the ability of the modifier to entrap the hydrides, while the stabilizing effect is maintained.",
author = "Hilligs{\o}e, {B. O.} and Andersen, {Jens E.T.} and Hansen, {Elo H.}",
year = "1997",
month = "1",
day = "1",
doi = "10.1039/A607478B",
language = "English",
volume = "12",
pages = "585--588",
journal = "Journal of Analytical Atomic Spectrometry",
issn = "0267-9477",
publisher = "Royal Society of Chemistry",
number = "5",

}

TY - JOUR

T1 - Investigations into the role of modifiers for entrapment of hydrides in Flow injection hydride generation electrothermal atomic absorption spectrometry as exemplified by the determination of germanium

AU - Hilligsøe, B. O.

AU - Andersen, Jens E.T.

AU - Hansen, Elo H.

PY - 1997/1/1

Y1 - 1997/1/1

N2 - Pd-conditioned graphite tubes, placed in the furnace of an AAS instrument, were used for entrapment of germane as generated in an associated flow-injection system. Two different approaches were tested with the ultimate aim of allowing multiple determinations, i.e., introduction of the modifier as a Pd salt solution, and use of electrolytically Pd pre-coated tubes. While the former treatment resulted in satisfactory analytical performance, although requiring separate regeneration of the tubes prior to each sampling sequence, the electrolytically pre-coated tubes did not function satisfactorily. This in turn led to a closer investigation as to the function of Pd in entrapping hydrides and releasing the analyte. Based on an evaluation of the behaviour of the two types of tubes, supplemented by scanning tunnelling microscopy studies of tubes with and without modifier and treated in different ways, it is shown that heating at 2600°C results in a physical- chemical change of the modifier in the electrolytically coated tubes; however, this change leads only to a loss of the ability of the modifier to entrap the hydrides, while the stabilizing effect is maintained.

AB - Pd-conditioned graphite tubes, placed in the furnace of an AAS instrument, were used for entrapment of germane as generated in an associated flow-injection system. Two different approaches were tested with the ultimate aim of allowing multiple determinations, i.e., introduction of the modifier as a Pd salt solution, and use of electrolytically Pd pre-coated tubes. While the former treatment resulted in satisfactory analytical performance, although requiring separate regeneration of the tubes prior to each sampling sequence, the electrolytically pre-coated tubes did not function satisfactorily. This in turn led to a closer investigation as to the function of Pd in entrapping hydrides and releasing the analyte. Based on an evaluation of the behaviour of the two types of tubes, supplemented by scanning tunnelling microscopy studies of tubes with and without modifier and treated in different ways, it is shown that heating at 2600°C results in a physical- chemical change of the modifier in the electrolytically coated tubes; however, this change leads only to a loss of the ability of the modifier to entrap the hydrides, while the stabilizing effect is maintained.

UR - http://www.scopus.com/inward/record.url?scp=0031145366&partnerID=8YFLogxK

UR - http://www.scopus.com/inward/citedby.url?scp=0031145366&partnerID=8YFLogxK

U2 - 10.1039/A607478B

DO - 10.1039/A607478B

M3 - Article

AN - SCOPUS:0031145366

VL - 12

SP - 585

EP - 588

JO - Journal of Analytical Atomic Spectrometry

JF - Journal of Analytical Atomic Spectrometry

SN - 0267-9477

IS - 5

ER -