EP0176575A1 - Four analytique comportant des sections de prechauffage et a temperature constante - Google Patents

Four analytique comportant des sections de prechauffage et a temperature constante

Info

Publication number
EP0176575A1
EP0176575A1 EP19850901916 EP85901916A EP0176575A1 EP 0176575 A1 EP0176575 A1 EP 0176575A1 EP 19850901916 EP19850901916 EP 19850901916 EP 85901916 A EP85901916 A EP 85901916A EP 0176575 A1 EP0176575 A1 EP 0176575A1
Authority
EP
European Patent Office
Prior art keywords
furnace
sample
primary
rod
tip
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Withdrawn
Application number
EP19850901916
Other languages
German (de)
English (en)
Inventor
Jaroslav Petr Matousek
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.)
Unisearch Ltd
Original Assignee
Unisearch Ltd
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
Application filed by Unisearch Ltd filed Critical Unisearch Ltd
Publication of EP0176575A1 publication Critical patent/EP0176575A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
    • G01N21/74—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using flameless atomising, e.g. graphite furnaces
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B17/00—Furnaces of a kind not covered by any preceding group
    • F27B17/02—Furnaces of a kind not covered by any preceding group specially designed for laboratory use

Definitions

  • the present invention relates to furnaces and more particularly to a furnace system suitable for constant temperature measurement and/or analysis.
  • Such furnaces are used for atomization of a sample in connection with analytical atomic spectroscopy, atomic absorption, atomic emission and atomic fluorescence.
  • a sample is deposited within a graphite furnace and subjected to both thermal pretreatment and atomization in situ by applying a preset temperature programme.
  • the present invention consists in a furnace comprising a primary furnace and a secondary furnace, said primary furnace being of generally tubular configuration projecting outwardly from said secondary furnace, in use said primary furnace providing an increasing temperature gradient towards said secondary furnace, said secondary furnace to be operated at a predetermined substantially constant temperature greater than the maximum temperature in the primary furnace, and wherein a sample to be analysed at the constant temperature of the secondary furnace is inserted therein via movement through the primary furnace.
  • the present invention provides a method of applying a substantially constant elevated temperature to a sample comprising subjecting said sample to an increasing temperature gradient so as to apply a thermal pretreatment to said sample and then subjecting said sample to said elevated predetermined substantially constant temperature immediately following said pretreatment.
  • An embodiment of a furnace in accordance with this invention is formed from graphite and a sample to be analysed is introduced into the secondary furnace via the primary furnace by being dried on the face of a graphite rod in situ or externally of the furnace. When dried externally the rod is inserted in the tubular primary furnace and driven toward the secondary furnace. In this way temperature programming of thermal pretreatment is achieved by moving the sample bearing rod through the different temperature zones in the primary furnace.
  • the sample to be analysed may be applied and dried in situ, either inside the secondary furnace or in the primary furnace. In situ application and drying can be carried out by introducing the sample to the tip of the rod via a suitably formed orifice, whereafter the rod may be withdrawn to, or already be located at, an appropriate position in the primary furnace for drying and thermal pretreatment before being driven toward the secondary furnace where the sample is atomized.
  • Fig. 1 is a part sectional view of a furnace in accordance with the present invention
  • Fig. 2 is a part sectional view of another embodiment of a furnace in accordance with the invention.
  • the furnace system depicted in Fig. 1 comprises a primary furnace 10 and a secondary furnace 11 located between terminals 12.
  • the secondary furnace 11 being connected to one terminal 12 via support rod 13 and the primary furnace 10 acting as its own support from the other terminal.
  • the primary and secondary furnaces as well as the sample introduction rod 14 may be formed from any suitable material, such as various forms of carbon including graphite, pyrolytic graphite, glassy carbon or the like and suitable materials will be apparent to the addressee.
  • the sample introduction rod 14 includes a sample supporting tip 15 at its end which is inserted in primary furnace 10 and moved in a predetermined manner toward opening 16 in secondary furnace 11.
  • Rod 14 may be manually driven through the primary furnace 10 or by such as solenoid or electro-mechanical means or pneumatic means under the action of an inert gas stream could be employed.
  • Primary furnace 10 has an increasing temperature gradient towards secondary furnace 11 and when sample supporting tip 15 is inserted in furnace 11 it is atomized at the constant temperature maintained in the secondary furnace thereby generating a transient atomic population suitable for analysis by, say, atomic spectroscopy.
  • Fig. 2 The furnace of Fig. 2 is identical with that of Fig. 1 except for the provision of an orifice 17 and equivalent parts are numbered in correspondence with those of Fig.
  • a sample can be applied to tip 15 when inserted into primary furnace 10 by injecting the sample onto the face of tip 15 through orifice 17.
  • the sample is applied in situ so as to reduce the prospect of contamination problems which may occur where the sample is applied to tip 15 externally of furnace 10.
  • the sample may be applied to the tip while it is within the furnace 11 prior to it being heated to its atomizing temperature.
  • Thermal treatment of the sample prior to atomization can be provided by a programmed controlling movement of the rod in the primary furnace.
  • a typical embodiment of a furnace of the form shown • by Fig. 1 or 2 comprises an inner graphite rod 14 of 3 mm diameter and a primary furnace 10 of 4.6 mm outer diameter.
  • the scale of secondary graphite furnace 11 can be appreciated from the relative proportions as shown by the drawings.
  • the tip 15 is formed from pyrolytic graphite which is oriented on the end of rod 14 so as to present maximum thermal reistance in a direction axially of rod 14. This is achieved by orienting the pyrolytic graphite of tip 15 so that its parallel layers are transverse to the axis of rod 14.
  • a sample to be analysed may be applied to the tip at ambient temperature or at an elevated temperature, say 120°C. If applied at an elevated temperature the sample solution may dry on contact.
  • a typical graphite furnace in accordance with the embodiments can be rapidly heated to operating temperature by application of an appropriate voltage across the primary and secondary furnaces so that while the secondary furnace is heated rapidly to essentially constant temperature, a significant temperature gradient along the length of the primary furnace is achieved.

Landscapes

  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Geology (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Clinical Laboratory Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)

Abstract

Four comportant une première section de préchauffage (10) protégeant d'une température constante et plus élevée la partie externe d'une section secondaire et un mécanisme pour faire traverser à un échantillon la section de préchauffage et l'amener dans la seconde section. Les deux sections sont de préférence en graphite et le mouvement est conféré par un mouvement rapide d'une tige (14). Le four est destiné à l'analyse spectroscopique atomique.
EP19850901916 1984-04-10 1985-04-10 Four analytique comportant des sections de prechauffage et a temperature constante Withdrawn EP0176575A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
AU4498/84 1984-04-10
AU449884 1984-04-10

Publications (1)

Publication Number Publication Date
EP0176575A1 true EP0176575A1 (fr) 1986-04-09

Family

ID=3694946

Family Applications (1)

Application Number Title Priority Date Filing Date
EP19850901916 Withdrawn EP0176575A1 (fr) 1984-04-10 1985-04-10 Four analytique comportant des sections de prechauffage et a temperature constante

Country Status (2)

Country Link
EP (1) EP0176575A1 (fr)
WO (1) WO1985004717A1 (fr)

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3181847A (en) * 1963-05-10 1965-05-04 Gen Motors Corp Temperature gradient furnace apparatus, and method of forming same
GB1218544A (en) * 1967-04-01 1971-01-06 Mullard Ltd Temperature control systems
SU531982A2 (ru) * 1975-05-04 1976-10-15 Всесоюзный Научно-Исследовательский И Проектный Институт "Теплопроект" Лабораторна печь
DE3042631A1 (de) * 1980-11-12 1982-06-16 Klaus-Richard Dr. 2000 Hamburg Sperling Verfahren und vorrichtung zum untersuchen von proben mittels flammenloser atemabsorptionsmessung
DE3044627C2 (de) * 1980-11-27 1984-06-07 Bodenseewerk Perkin-Elmer & Co GmbH, 7770 Überlingen Vorrichtung zur Probeneingabe in ein Graphitrohr bei der flammenlosen Atomabsorptions-Spektroskopie
DE3217417C2 (de) * 1982-05-08 1984-02-09 Bodenseewerk Perkin-Elmer & Co GmbH, 7770 Überlingen Vorrichtung zum Atomisieren einer Probe bei der flammenlosen Atomabsorptions-Spektroskopie
DE3307251A1 (de) * 1983-03-02 1984-09-06 Klaus-Richard Dr. 2000 Hamburg Sperling Verfahren und vorrichtung zum untersuchen von proben mittels flammenloser atomabsorptionsmessung

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO8504717A1 *

Also Published As

Publication number Publication date
WO1985004717A1 (fr) 1985-10-24

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Inventor name: MATOUSEK, JAROSLAV, PETR