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WO1999052127A2 - Reacteur de pyrolyse pour la pyrolyse d'echantillons organiques et inorganiques, analyseur elementaire renfermant ce reacteur, et procede de spectrometrie de masse - Google Patents

Reacteur de pyrolyse pour la pyrolyse d'echantillons organiques et inorganiques, analyseur elementaire renfermant ce reacteur, et procede de spectrometrie de masse Download PDF

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Publication number
WO1999052127A2
WO1999052127A2 PCT/EP1999/002157 EP9902157W WO9952127A2 WO 1999052127 A2 WO1999052127 A2 WO 1999052127A2 EP 9902157 W EP9902157 W EP 9902157W WO 9952127 A2 WO9952127 A2 WO 9952127A2
Authority
WO
WIPO (PCT)
Prior art keywords
pyrolysis
pyrolysis reactor
carbon
tube
organic
Prior art date
Application number
PCT/EP1999/002157
Other languages
German (de)
English (en)
Other versions
WO1999052127A3 (fr
Inventor
Matthias Gehre
Babara E. Kornexl
Original Assignee
Ufz-Umweltforschungszentrum Leipzig-Halle 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
Application filed by Ufz-Umweltforschungszentrum Leipzig-Halle Gmbh filed Critical Ufz-Umweltforschungszentrum Leipzig-Halle Gmbh
Priority to AU35219/99A priority Critical patent/AU3521999A/en
Publication of WO1999052127A2 publication Critical patent/WO1999052127A2/fr
Publication of WO1999052127A3 publication Critical patent/WO1999052127A3/fr

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Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D21/00—Arrangement of monitoring devices; Arrangement of safety devices
    • 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 of groups F27B1/00 - F27B15/00
    • F27B17/02—Furnaces of a kind not covered by any of groups F27B1/00 - F27B15/00 specially designed for laboratory use
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
    • H01J49/0468—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components with means for heating or cooling the sample
    • H01J49/0472—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components with means for heating or cooling the sample with means for pyrolysis

Definitions

  • the invention relates to a method for mass-spectrometric on-line determination of the oxygen iso topical composition of a sample, with which the ⁇ 18CD values of both organic and inorganic samples can be determined accurately and correctly in a very short time.
  • the subject is also a new pyrolysis reactor and an elemental analyzer containing this pyrolysis reactor.
  • the determination of the oxygen isotope ratio 0/0 in any organic or inorganic sample is important in geology, hydrology, anthropology, ecology, food chemistry or medicine. For reasons of effectiveness, it is desirable to carry out such determinations on-line if possible.
  • EP 0 419 167 (also corresponds to US Pat. No. 5,314,827) describes an on-line mass spectrometric method for determining the isotope composition of at least one of the elements oxygen, nitrogen and hydrogen in a sample, in which the sample is also in a catalytic reactor before the MS determination , which contains elemental carbon and a platinum / rhodium alloy as a catalyst, is pyrolyzed, the pyrolysis temperature being up to 1200 ° C. This method also does not allow an exact and correct determination of the isotope composition of oxygen in an inorganic sample.
  • the object of the present invention was therefore to provide a method for determining the oxygen isotope composition ( ⁇ 0) of a sample with on-line coupling of the pyrolysis reactor and isotope ratio mass spectrometer (IRMS), with which both organic and inorganic samples are equally accurate and correct can be determined in a short time and that allows the measurement of the smallest sample quantities of solid, liquid and gaseous substances.
  • IRMS isotope ratio mass spectrometer
  • the temperature is particularly preferably between 1350-1550 ° C., very particularly preferably 1400 ° C.
  • Helium serves as a carrier gas to transport the pyrolysis products into the IRMS and as a protective gas.
  • Graphite, spectral carbon or glassy carbon can be used as the carbon source.
  • Nickel or platinum is used as the catalyst.
  • graphite powder and nickel powder are used as the catalyst.
  • inorganic samples such.
  • Nitrate and sulfate it is assumed that the pyrolysis proceeds according to the following equations: for nitrate: 2 KN0 3 + 8 C ⁇ N 2 + 6 CO + [2 KC] for sulfate: BaS0 4 + 6 C ⁇ 4 CO + [ BaC 2 + S]
  • the pyrolysis reactor is connected in a conventional manner to the IRMS via a gas chromatography column.
  • the gas chromatography column is temperature-controlled (preferably at approx. 70 ° C.) and serves to separate the CO from nitrogen and / or hydrogen. If necessary, a trap can be placed in front of the gas chromatography column to exclude other disruptive pyrolysis products (e.g. HCN).
  • the solid or liquid samples are wrapped in silver or tin capsules and released into the pyrolysis furnace at regular intervals by the autosampler according to the set time program. Liquid and gaseous samples can also be injected through a septum.
  • the invention also relates to a new pyrolysis reactor 1 for pyrolysis of the samples with the generation of CO as the measurement gas, which is preferred for carrying out the The method according to the invention can be used, and an elemental analyzer 12 comprising this pyrolysis reactor 1 and a gas chromatography column 10.
  • the elemental analyzer 12 can include two fans 9a and 9b, which are used to cool the screw connections of the pyrolysis reactor 1 to the elemental analyzer 12.
  • the elemental analyzer optionally includes a trap 11, which is arranged after the pyrolysis reactor and before the gas chromatography column.
  • the pyrolysis reactor is designed as specified in the claims.
  • a preferred embodiment is shown in FIG. 1.
  • the variant shown includes glassy carbon chips 7 which, at the high temperatures according to the invention, serve as an additional carbon source for the pyrolysis of inorganic samples, such as. B. nitrates.
  • the structure of the elemental analyzer according to the invention with coupling to the IRMS is shown in FIG. 2.
  • the outer diameter of the outer tube is 17 mm
  • the inner diameter is 14 mm
  • the length is 470 mm
  • the inner glassy carbon tube 3 has an outer diameter of 12 mm, an inner diameter of 7 mm and a length of 380 mm. These parts are commercially available. Only the matching funnels 5a and 5b are not currently available on the market and have to be manufactured.

Landscapes

  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Clinical Laboratory Science (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

L'invention concerne un procédé de détermination en ligne par spectrométrie de masse de la composition en isotopes d'oxygène d'un échantillon, au moyen duquel les valeurs δ18O des échantillons à la fois organiques et inorganiques peuvent être déterminées correctement et avec précision dans un temps minimum. L'invention concerne également un nouveau réacteur de pyrolyse et un analyseur élémentaire renfermant ce réacteur de pyrolyse.
PCT/EP1999/002157 1998-04-02 1999-03-26 Reacteur de pyrolyse pour la pyrolyse d'echantillons organiques et inorganiques, analyseur elementaire renfermant ce reacteur, et procede de spectrometrie de masse WO1999052127A2 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU35219/99A AU3521999A (en) 1998-04-02 1999-03-26 Pyrolysis reactor for the pyrolysis or organic and inorganic samples, elementaryanalyser containing said pyrolysis reactor and method for mass-spectrometry

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19816348.7 1998-04-02
DE1998116348 DE19816348C1 (de) 1998-04-02 1998-04-02 Pyrolysereaktor zur Pyrolyse organischer und anorganischer Proben, Elementaranalysator enthaltend diesen Pyrolysereaktor und Verfahren zur massenspektrometrischen on-line Bestimmung der Sauerstoffisotopenzusammensetzung organischer und anorganischer Proben

Publications (2)

Publication Number Publication Date
WO1999052127A2 true WO1999052127A2 (fr) 1999-10-14
WO1999052127A3 WO1999052127A3 (fr) 1999-12-09

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AU (1) AU3521999A (fr)
DE (1) DE19816348C1 (fr)
WO (1) WO1999052127A2 (fr)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007115423A1 (fr) * 2006-04-07 2007-10-18 Universität Bern Chambre d'equilibre, appareil et procede pour determiner en ligne la composition isotopique d'hydrogene stable non echangeable dans un echantillon de substance
CN103592362A (zh) * 2013-11-27 2014-02-19 中国科学院大连化学物理研究所 一种分析煤热解低分子产物的方法
CN105372361A (zh) * 2014-08-26 2016-03-02 中国科学院大连化学物理研究所 原位热解飞行时间质谱分析聚合物热解低分子产物的方法
CN105372360A (zh) * 2014-08-26 2016-03-02 中国科学院大连化学物理研究所 原位热解飞行时间质谱分析聚合物热解气态挥发物的方法
GB2557891A (en) * 2016-09-02 2018-07-04 Thermo Fisher Scient Bremen Gmbh Improved sample preparation apparatus and method for elemental analysis spectrometer

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DE19938395B4 (de) * 1999-08-05 2004-12-09 Ufz-Umweltforschungszentrum Leipzig-Halle Gmbh Verfahren zur massenspektrometrischen On-line-Bestimmung von Sauerstoffisotopenzusammensetzungen in geologischen Proben
RU2225428C2 (ru) * 2002-03-04 2004-03-10 Ипатов Владимир Васильевич Способ получения древесного угля, тепловой энергии и горючего газа и устройство для его осуществления
DE10260119A1 (de) * 2002-12-19 2004-07-15 Forschungszentrum Jülich GmbH Verfahren und Vorrichtung zur Freisetzung von Sauerstoffisotopen aus sauerstoffhaltigen Feststoffen
US20080187907A1 (en) * 2004-02-26 2008-08-07 Bartholomew Calvin H Catalytic Production of Biomakers From Biological Materials
DE102005017192B4 (de) * 2005-04-13 2013-11-14 Forschungszentrum Jülich GmbH Vorrichtung sowie Verfahren zur Messung der stabilen Isotopenverhältnisse von Sauerstoff, Wasserstoff und Stickstoff aus anorganischen und organischen Verbindungen sowie zur Bestimmung der quantitativen elementaren Zusammensetzung der Verbindungen
DE102007031678A1 (de) * 2007-07-06 2009-01-08 Thermo Fisher Scientific (Bremen) Gmbh Vorrichtung mit einer Verbindung zweier Kapillaren
EP2031387B1 (fr) * 2007-08-03 2010-01-27 Università degli Studi di Parma Dispositif réacteur pour analyses isotopiques
DE102008008288B4 (de) * 2008-02-07 2015-07-09 Elementar Analysensysteme Gmbh Verfahren zur Sauerstoffelementaranalyse und zur Sauerstoffisotopenmessung stickstoffhaltiger, organischer Substanzen
EP2236208A1 (fr) * 2009-04-03 2010-10-06 Università degli Studi di Parma Dispositif réacteur pour analyses chimiques et isotopiques
DE102009054151B3 (de) * 2009-11-23 2011-06-30 Elementar Analysensysteme GmbH, 63452 Verfahren zur Sauerstoffelementaranalyse und zur Sauerstoffisotopenmessung stickstoffhaltiger, organischer Substanzen
DE102010001677B4 (de) 2010-02-08 2012-01-19 Helmholtz-Zentrum Potsdam Deutsches GeoForschungsZentrum - GFZ Stiftung des Öffentlichen Rechts des Landes Brandenburg Verfahren zur thermischen Umsetzung von Probenmaterial in Messgas
DE102015102126A1 (de) 2015-02-13 2016-08-18 Thermo Fisher Scientific Gmbh Verfahren und Reaktor zur quantitativen Gewinnung von molekularem Wasserstoff aus Substanzen sowie deren Verwendung zur massenspektrometrischen online Bestimmung des Isotopenverhältnisses von Wasserstoff
US11465113B2 (en) 2015-02-13 2022-10-11 Thermo Fisher Scientific (Bremen) Gmbh Use of a reactor, methods, and device for quantitatively obtaining molecular hydrogen from substances
CN114609288A (zh) * 2022-03-21 2022-06-10 中国科学院地质与地球物理研究所 一种硅酸盐氧同位素测试系统和方法

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB8921285D0 (en) * 1989-09-20 1989-11-08 Vg Instr Group Isotopic composition analyzer
FR2734363B1 (fr) * 1995-05-16 1997-08-01 Pernod Ricard Methode de mesure de la teneur en 18o et/ou 15n d'une substance chimique, appareillage et dispositif de pyrolyse

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007115423A1 (fr) * 2006-04-07 2007-10-18 Universität Bern Chambre d'equilibre, appareil et procede pour determiner en ligne la composition isotopique d'hydrogene stable non echangeable dans un echantillon de substance
CN103592362A (zh) * 2013-11-27 2014-02-19 中国科学院大连化学物理研究所 一种分析煤热解低分子产物的方法
CN103592362B (zh) * 2013-11-27 2016-04-06 中国科学院大连化学物理研究所 一种分析煤热解低分子产物的方法
CN105372361A (zh) * 2014-08-26 2016-03-02 中国科学院大连化学物理研究所 原位热解飞行时间质谱分析聚合物热解低分子产物的方法
CN105372360A (zh) * 2014-08-26 2016-03-02 中国科学院大连化学物理研究所 原位热解飞行时间质谱分析聚合物热解气态挥发物的方法
GB2557891A (en) * 2016-09-02 2018-07-04 Thermo Fisher Scient Bremen Gmbh Improved sample preparation apparatus and method for elemental analysis spectrometer
US10332735B2 (en) 2016-09-02 2019-06-25 Thermo Fisher Scientific (Bremen) Gmbh Sample preparation apparatus and method for elemental analysis spectrometer
US10707065B2 (en) 2016-09-02 2020-07-07 Thermo Fisher Scientific (Bremen) Gmbh Sample preparation apparatus and method for elemental analysis spectrometer
GB2557891B (en) * 2016-09-02 2021-05-12 Thermo Fisher Scient Bremen Gmbh Improved sample preparation apparatus and method for elemental analysis spectrometer

Also Published As

Publication number Publication date
WO1999052127A3 (fr) 1999-12-09
AU3521999A (en) 1999-10-25
DE19816348C1 (de) 1999-08-05

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