WO2007090542A1 - Dispositif et procédé pour déterminer automatiquement la teneur en chlore d'échantillons - Google Patents

Dispositif et procédé pour déterminer automatiquement la teneur en chlore d'échantillons Download PDF

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Publication number
WO2007090542A1
WO2007090542A1 PCT/EP2007/000781 EP2007000781W WO2007090542A1 WO 2007090542 A1 WO2007090542 A1 WO 2007090542A1 EP 2007000781 W EP2007000781 W EP 2007000781W WO 2007090542 A1 WO2007090542 A1 WO 2007090542A1
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WO
WIPO (PCT)
Prior art keywords
combustion
sensor
chlorine
determination
drying device
Prior art date
Application number
PCT/EP2007/000781
Other languages
German (de)
English (en)
Inventor
Sabine Kraus
Hans-Joachim Kupka
Hans-Peter Sieper
Norbert Proba
Original Assignee
Elementar Analysensysteme 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 Elementar Analysensysteme Gmbh filed Critical Elementar Analysensysteme Gmbh
Priority to EP07703135A priority Critical patent/EP1982170A1/fr
Publication of WO2007090542A1 publication Critical patent/WO2007090542A1/fr

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/12—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using combustion

Definitions

  • the present invention relates to a device for elemental analysis for automatically determining the content of chlorine in solid, liquid or gaseous samples, with a combustion device having a combustion chamber, which is adjustable to a temperature via a heater of up to 1200 0 C, with an oxygen supply or a supply of synthetic air for the combustion chamber as a combustion and carrier gas, with a downstream of the combustion chamber drying device, with a drying device following determination device for HCl and with an adjoining evaluation.
  • the invention also relates to a method for automatically determining the content of chlorine in samples.
  • the elemental analysis is widely used in particular for the determination of carbon, nitrogen, sulfur, hydrogen and / or oxygen contained in solid or liquid samples.
  • the samples are burned in a combustion device with the supply of oxygen and the combustion products, carried in a carrier gas, analyzed in various stages with respect to the above elements.
  • Such analyzes can be automated with known devices.
  • the content of chlorine in solid, liquid or gaseous samples is so far been recorded via a so-called micro-coulometer.
  • the sample to be analyzed is first placed in a boat, placed in an oven (this process is usually done manually), where the sample is burned while supplying oxygen.
  • the combustion gas is then subjected to drying with liquid sulfuric acid and then fed to a microcoulometer; the measured values of the micro coulometer are then evaluated in an evaluation unit.
  • the present invention has for its object to provide an apparatus and a method for automatically determining the content of chlorine (Cl) in samples that do not show the disadvantages mentioned above.
  • the device should be substantially maintenance-free and allow automated measurement of the chlorine content on large series of samples over a large concentration range.
  • an elemental analysis device for automatically determining the content of chlorine in solid, liquid or gaseous samples, with a combustion device having a combustion chamber, which is adjustable to a temperature over a heater of up to 1200 c C, with a Oxygen supply or a supply of synthetic air for the combustion chamber as a combustion and carrier gas, with a combustion chamber downstream drying device, with a drying device following determination means for chlorine (as HCl) and with an adjoining evaluation, which is characterized in that provisions For Cl, a sensor for hydrogen chloride (HCl) comprising a flow cell is provided
  • the object is also achieved by a method for elemental analysis for automatically determining the content of chlorine in solid, liquid or gaseous samples, wherein in a combustion device, a sample is burned at temperatures of up to 1200 0 C under supply of oxygen or synthetic air as combustion and carrier gas, the gas stream is dried in a drying device and the dried measurement gas is supplied to a determination device for chlorine and the determination result is evaluated, which is characterized in that the dried measurement gas is supplied to a cuvette having at least one HCI sensor, the voltage signal delivered by the cuvette is detected and compared with a calibration curve, the voltage signal being assigned a chlorine value and this value being displayed.
  • an afterburner is arranged downstream of the incinerator in one embodiment.
  • a deficit of hydrogen for HCl formation is compensated by appropriate sample additions.
  • a drying device In connection with a flow cell, as used in the apparatus and the method according to the invention for determining the content of chlorine, a drying device can be used, which has as a drying agent H2SO4 (sulfuric acid) on a granular / granular support.
  • H2SO4 sulfuric acid
  • “Dry” sulfuric acid is relatively easy to handle. This dry sulfuric acid is available, for example, from Merck (Darmstadt). If larger amounts of water occur during combustion, it is preferred to use membrane drying as the drying device, followed by a section having the desiccant.
  • Such a drying device is characterized by the fact that it works completely maintenance-free.
  • the flow cell of the HCI sensor should be tuned to different measuring ranges by sensors of different sensitivity.
  • sensors Preferably, such sensors are used which cover a measurement range of 20 ng (20 ⁇ 10 -9 g) to 2 mg (2 ⁇ 10 -3 g).
  • Figure 1 shows a schematic structure of a first embodiment of an apparatus for elemental analysis for automatically determining the content of chlorine in solid, liquid or gaseous samples
  • Figure 2 shows a schematic structure of a second embodiment with additional post-combustion device.
  • the device comprises a combustion furnace 1 with combustion tube 2, which is surrounded by a heating device 3. About this heater 3, the combustion tube 2 is heated up to a temperature of 1200 0 C.
  • the combustion tube 2 is filled with WOß granules to ensure 100% combustion.
  • a sample injection head 4 At the top of the combustion tube 2 is a sample injection head 4, via which in particular liquid samples can be injected into the combustion tube 2.
  • the arrangement can also be used for the analysis of solid samples, moreover, for automated operation, modified accordingly.
  • the sample injection head 4 is removed and instead a solid sampler is placed.
  • an inlet 5 for oxygen or synthetic air which is provided via a corresponding supply unit 6, which can be adjusted in volume via a pressure control valve 7.
  • the structure described above is a conventional arrangement of a combustion device for the elemental analysis, as it is widely used, even with the corresponding modifications.
  • HCI sensors as used in the flow cell 10, are generally available and are used in other areas, eg. B. in the field of ambient air monitoring.
  • the measuring range of the flow cell can be adjusted in stages, for example from 0-20 ppm HCl, 0-0.3% HCl and 0-5% HCl.
  • FIG. 2 shows a further device which, insofar as it is comparable in its parts to the device shown in FIG. 1, is designated by the same reference numerals with respect to such parts.
  • the arrangement according to FIG. 2 has a heating device 3, which has, beside the combustion tube, an afterburning tube 14 which, like the incinerator 2, is filled with W ⁇ 3 granules.
  • the two combustion tubes or furnaces 2, 14 are connected in the schematic representation of Figure 2 at the lower ends with a connecting pipe 15.
  • the sample is introduced via the solids sampler 4 into the upper region of the combustion tube 2 protected by a quartz crucible 16 which bears against the inner wall of the combustion tube of the incinerator 2, which at its lower portion is penetrated by a Plug 17 made of aluminum oxide wool against the WO 3 granules is separated.
  • Both the combustion furnace 2 and the combustion device 3 are operated at temperatures between 1100 0 C and 1200 0 C.
  • the additional post-combustion device 14 ensures that the Cl in the sample is completely converted to HCl.
  • the combustion gases leaving the combustion tube 14 are conducted via a commercially available membrane gas dryer 8 '(such a membrane gas dryer is available, for example, from Permapure), which is supplied with purge gas, indicated by the arrows 18.
  • This membrane gas dryer 8 ' has the advantage that by its use, the drying device 8 can be operated over a longer period of time before the water absorber must be renewed.
  • a flow cell with an IR detector designated by reference numeral 19 in FIG. 2 is inserted, and the signal obtained by the IR detector is shown in FIG downstream electronics 11 and the PC 12 edited or displayed for evaluation on the screen 13.

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  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Combustion & Propulsion (AREA)
  • Molecular Biology (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

L'invention concerne un dispositif d'analyse d'éléments permettant de déterminer automatiquement la teneur en chlore d'échantillons solides, liquides, ou gazeux. Le dispositif selon l'invention comprend : une installation de combustion (1) comportant une chambre de combustion (2) dont la température peut être réglée au moyen d'un système de chauffage pour atteindre 1200 °C; une alimentation en oxygène (6) ou une alimentation en air artificiel pour la chambre de combustion, l'oxygène et l'air artificiel servant de gaz de combustion et de gaz porteur; une installation de séchage (8) qui est disposée en aval de la chambre de combustion; une installation de détermination de Cl qui est placée en aval de l'installation de séchage, et; une unité d'évaluation (11) qui est reliée à l'installation de détermination. Selon l'invention, l'installation de détermination de Cl comprend un détecteur de HCl qui est disposé dans une cuvette de circulation (10). Cette invention se rapporte en outre à un procédé.
PCT/EP2007/000781 2006-02-10 2007-01-30 Dispositif et procédé pour déterminer automatiquement la teneur en chlore d'échantillons WO2007090542A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP07703135A EP1982170A1 (fr) 2006-02-10 2007-01-30 Dispositif et procédé pour déterminer automatiquement la teneur en chlore d'échantillons

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DE102006006490 2006-02-10
DE102006006490.9 2006-02-10
DE102006049927.1 2006-10-19
DE102006049927A DE102006049927A1 (de) 2006-02-10 2006-10-19 Vorrichtung und Verfahren zum automatischen Bestimmen des Gehaltes an Chlor in Proben

Publications (1)

Publication Number Publication Date
WO2007090542A1 true WO2007090542A1 (fr) 2007-08-16

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2007/000781 WO2007090542A1 (fr) 2006-02-10 2007-01-30 Dispositif et procédé pour déterminer automatiquement la teneur en chlore d'échantillons

Country Status (3)

Country Link
EP (1) EP1982170A1 (fr)
DE (2) DE102006049927A1 (fr)
WO (1) WO2007090542A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114184739A (zh) * 2021-12-20 2022-03-15 唐山旭阳化工有限公司 检测粗苯中氯含量的方法

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR102155406B1 (ko) * 2017-08-18 2020-09-11 주식회사 엘지화학 아연철산화물 내 잔류 Cl의 정량분석 방법

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2459273A1 (de) * 1974-12-14 1976-06-16 Licentia Gmbh Verfahren zur bestimmung von vinylchlorid in luft und gasmischungen
JPS5560851A (en) * 1978-11-01 1980-05-08 Nippon Oil Co Ltd Device for analyzing chlorine by minute coulometric titration
JPS5637552A (en) * 1979-09-03 1981-04-11 Mitsubishi Heavy Ind Ltd Analyzing method for chlorine and fluorine
WO2001046683A2 (fr) * 1999-12-20 2001-06-28 AJ IDC Geräteentwicklungsgesellschaft mbH Analyse de la teneur totale en azote, soufre et chlore
KR20050033366A (ko) * 2003-10-06 2005-04-12 한국기계연구원 가연성 고체연료 및 폐기물에 함유된 염소량 분석용완전연소반응기

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2459273A1 (de) * 1974-12-14 1976-06-16 Licentia Gmbh Verfahren zur bestimmung von vinylchlorid in luft und gasmischungen
JPS5560851A (en) * 1978-11-01 1980-05-08 Nippon Oil Co Ltd Device for analyzing chlorine by minute coulometric titration
JPS5637552A (en) * 1979-09-03 1981-04-11 Mitsubishi Heavy Ind Ltd Analyzing method for chlorine and fluorine
WO2001046683A2 (fr) * 1999-12-20 2001-06-28 AJ IDC Geräteentwicklungsgesellschaft mbH Analyse de la teneur totale en azote, soufre et chlore
KR20050033366A (ko) * 2003-10-06 2005-04-12 한국기계연구원 가연성 고체연료 및 폐기물에 함유된 염소량 분석용완전연소반응기

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114184739A (zh) * 2021-12-20 2022-03-15 唐山旭阳化工有限公司 检测粗苯中氯含量的方法

Also Published As

Publication number Publication date
EP1982170A1 (fr) 2008-10-22
DE202006020954U1 (de) 2011-04-07
DE102006049927A1 (de) 2007-08-16

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