DE102010010358A1 - Method for detecting sulfur dioxide in analysis gas for e.g. reduction or oxidation of nitric oxide during sulfur dioxide determination, involves converting interfering gases into harmless gases by direct ionization in flow reactor - Google Patents
Method for detecting sulfur dioxide in analysis gas for e.g. reduction or oxidation of nitric oxide during sulfur dioxide determination, involves converting interfering gases into harmless gases by direct ionization in flow reactor Download PDFInfo
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- DE102010010358A1 DE102010010358A1 DE102010010358A DE102010010358A DE102010010358A1 DE 102010010358 A1 DE102010010358 A1 DE 102010010358A1 DE 102010010358 A DE102010010358 A DE 102010010358A DE 102010010358 A DE102010010358 A DE 102010010358A DE 102010010358 A1 DE102010010358 A1 DE 102010010358A1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0011—Sample conditioning
- G01N33/0014—Sample conditioning by eliminating a gas
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- 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
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
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- 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
- G01N21/66—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
- G01N21/67—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence using electric arcs or discharges
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- 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
- G01N21/66—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
- G01N21/68—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence using high frequency electric fields
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
Description
Die Erfindung betrifft ein Verfahren und eine Vorrichtung zum Nachweis eines Stoffes in einem Analysengas mittels UV-Fluoreszenzdetektion.The invention relates to a method and a device for detecting a substance in an analysis gas by means of UV fluorescence detection.
Die Erfindung ist vorzugsweise zum Nachweis von Schwefeldioxid in einem Gasgemisch geeignet.The invention is preferably suitable for the detection of sulfur dioxide in a gas mixture.
In vielen Fällen enthalten die zu analysierenden Gasgemische Störgase, die das Messergebnis verfälschen.In many cases, the gas mixtures to be analyzed contain interfering gases, which falsify the measurement result.
Die Detektion von SO2 mit UV-Fluoreszenz ist querempfindlich gegenüber NO. Dies ist in der Elementaranalytik insofern problematisch, da gerade in petrochemischen Proben neben Schwefel oft auch große Mengen an Stickstoff enthalten sein können, die dann die Schwefelbestimmung empfindlich stören oder sogar unmöglich machen. Ein spezielles Problem ist z. B. die Bestimmung des Schwefelgehaltes in schwefelarmen Dieselkraftstoffen. Zur Verbesserung der Zündwilligkeit werden dem Diesel zunehmend Additive zur Erhöhung der Cetanzahl zugesetzt. Diese Cetanimprover sind Stickstoffverbindungen, wie 2-Ethylhexylnitrat.The detection of SO 2 with UV fluorescence is cross-sensitive to NO. This is problematic in elemental analysis, since in petrochemical samples in addition to sulfur often large amounts of nitrogen may be included, which then severely disrupt the determination of sulfur or even impossible. A special problem is z. B. the determination of the sulfur content in low-sulfur diesel fuels. In order to improve the ignitability, additives are increasingly being added to the diesel to increase the cetane number. These cetane improvers are nitrogen compounds such as 2-ethylhexyl nitrate.
In
Zur Beseitigung von Störgasen, die querempfindlich auf die Detektion von zu analysierenden Gasen wirken, ist es bekannt, parallel zum Gasstrom einen Ozongenerator zu betreiben und das dabei erzeugte Ozon dem Messgas zuzuführen, wobei die Störgase durch Oxidation zu Gasen umgewandelt werden, die das Messergebnis nicht stören.To eliminate interfering gases, which act cross-sensitively on the detection of gases to be analyzed, it is known to operate an ozone generator in parallel to the gas stream and to supply the ozone generated thereby to the measurement gas, the interfering gases being converted by oxidation into gases which do not produce the measurement result to disturb.
Dabei ist nachteilig, dass für die Analyse ein Hilfsgas und eine Mischvorrichtung erforderlich sind. Ferner unterliegt die Ozondosierung Schwankungen, die eine komplizierte Konzentrationsüberwachung erforderlich macht.It is disadvantageous that an auxiliary gas and a mixing device are required for the analysis. Furthermore, the ozone dosage is subject to fluctuations requiring complicated concentration monitoring.
Der Erfindung liegt die Aufgabe zugrunde, ein Verfahren und eine Vorrichtung der eingangs genannten Art anzugeben, mit dem Querempfindlichkeiten durch Störsubstanzen verringert werden, ohne dass ein Hilfsgas benutzt werden muss.The invention has for its object to provide a method and an apparatus of the type mentioned, are reduced with the cross-sensitivities by interfering substances without an auxiliary gas must be used.
Die Aufgabe wird erfindungsgemäß mit einem Verfahren, welches die in die im Anspruch 1 angegebenen Merkmale aufweist, und mit einer Vorrichtung, welche die im Anspruch 8 angegebenen Merkmale aufweist, gelöst.The object is achieved with a method which has the features specified in
Vorteilhafte Ausgestaltungen sind in den Unteransprüchen angegeben.Advantageous embodiments are specified in the subclaims.
Die im Analysengas enthaltenen Störgase werden durch direkte Ionisierung des Analysengases in einem Durchflussreaktor in unschädliche Gase umgewandelt. Das Analysengas wird im Durchflussreaktor einem elektromagnetischen Feld hoher Feldstärke ausgesetzt, wobei die Ionisierungsenergie in Abhängigkeit vom Anwendungszweck eingestellt wird.The interfering gases contained in the analysis gas are converted into harmless gases by direct ionization of the analysis gas in a flow-through reactor. The analysis gas is exposed in the flow reactor to a high field electromagnetic field, the ionization energy being adjusted depending on the application.
Üblicherweise wird das Analysengas dem Detektor zugeführt, nachdem es den Durchflussreaktor durchströmt hat.Usually, the analysis gas is supplied to the detector after flowing through the flow-through reactor.
Besonders geeignet ist das Verfahren zur Reduktion oder Oxidation von NO bei der SO2-Bestimmung.Particularly suitable is the method for the reduction or oxidation of NO in the SO 2 determination.
Eine bevorzugte Verwendung des Verfahrens dient zur SO2-Bestimmung in einem Analysengas, wobei im Analysengas enthaltene Störgase durch direkte Ionisierung des Analysengases in einem Durchflussreaktor in unschädliche Gase umgewandelt werden.A preferred use of the method is for SO 2 determination in an analysis gas, wherein interfering gases contained in the analysis gas are converted into harmless gases by direct ionization of the analysis gas in a flow-through reactor.
Dabei kann die SO2-Bestimmung mit einem UV-Fluoreszenzdetektor oder mittels jodometrischer Titration durch Mikrocoulometrie erfolgen.In this case, the SO 2 determination can be carried out with a UV fluorescence detector or by means of iodometric titration by microcoulometry.
Es können sowohl Querempfindlichkeiten unmittelbar vor dem Eintritt in den Detektor verringert werden, als auch Abgase eines Analysengerätes am Ausgang des Analysators zur Erhöhung der Reaktivität des Trägergases, welches gleichzeitig als Oxidationsmittel für den Aufschluss am Eingang eines Aufschlussreaktors fungiert, behandelt werden.Both cross-sensitivities immediately before entry into the detector can be reduced, and exhaust gases from an analyzer at the output of the analyzer can be treated to increase the reactivity of the carrier gas, which simultaneously acts as an oxidant for digestion at the inlet of a digestion reactor.
Die Querempfindlichkeit herkömmlicher UV-Fluoreszenzdetektoren gegenüber NO liegt bei ca. 1:100, d. h. 500 ppm Stickstoff in der Probe werden als 5 ppm Schwefel angezeigt. Außerdem werden bei hohen Stickstoffgehalten in der Probe streuende Messsignale am UV-Fluoreszenzdetektor erhalten, die eine matrixabhängige Kalibrierung, besonders zur Schwefelbestimmung im Spurenbereich, nicht erlauben.The cross-sensitivity of conventional UV fluorescence detectors to NO is about 1: 100, d. H. 500 ppm of nitrogen in the sample is reported as 5 ppm of sulfur. In addition, at high nitrogen contents in the sample scattering measurement signals are obtained at the UV fluorescence detector, which does not allow a matrix-dependent calibration, especially for trace sulfur determination.
Durch die Zerstörung des NO vor Eintritt in den UV-Fluoreszenzdetektor wird die Schwefelbestimmung auch neben großen Stickstoffgehalten möglich. Der Mikroplasmareaktor wurde dazu zwischen Verbrennung und Detektor installiert. Das Analysengas wurde vor Eintritt in den Mikroplasmareaktor über einen Membrantrockner getrocknet. Versuche haben gezeigt, dass auch Anteile von SO2 im Plasma oxidiert werden und sich somit der Analytik entziehen. Unter konstanten Bedingungen ist dieser Anteil über übliche Konzentrationsbereiche proportional zum SO2-Gehalt. Es werden auch bei Zwischenschaltung des Mikroplasmareaktors lineare Kalibrierkurven für Schwefel erhalten. Mit steigender Plasmaintensität werden höhere Anteile an SO2 umgewandelt. Damit sinkt die Empfindlichkeit des Verfahrens. Daher ist es sinnvoll, die Plasmaintensität der umzusetzenden Menge an NO anzupassen. Dies ist mit dem Mikroplasmareaktor gut realisierbar. Für Einstellung zur Beseitigung von ca. 500 ppm Stickstoff in der Probe sinkt die SO2-Ausbeute am Detektor um ca. 30%. Die Reproduzierbarkeit der Messwerte wird durch das Plasma nicht verändert. Die erreichbaren Nachweisgrenzen werden nur durch die Signalhöhe am Detektor limitiert.By destroying the NO before entering the UV fluorescence detector, the sulfur determination is also next to large nitrogen levels possible. The microplasma reactor was installed between combustion and detector. The analysis gas was dried over a membrane dryer before entering the microplasma reactor. Experiments have shown that also portions of SO 2 are oxidized in the plasma and thus escape the analytics. Under constant conditions, this proportion is above the usual concentration ranges proportional to the SO 2 content. Even with the interposition of the micro-plasma reactor, linear calibration curves for sulfur are obtained. As the plasma intensity increases, higher levels of SO 2 are converted. This reduces the sensitivity of the process. Therefore, it makes sense to adjust the plasma intensity of the amount of NO to be reacted. This is well feasible with the microplasma reactor. For setting to remove about 500 ppm of nitrogen in the sample, the SO 2 yield at the detector decreases by about 30%. The reproducibility of the measured values is not changed by the plasma. The achievable detection limits are only limited by the signal height at the detector.
Die Erfindung wird im Folgenden anhand von Ausführungsbeispielen näher erläutert.The invention will be explained in more detail below with reference to exemplary embodiments.
In den zugehörigen Zeichnungen zeigen:In the accompanying drawings show:
Der in
In
BezugszeichenlisteLIST OF REFERENCE NUMBERS
- 11
- Analysatoranalyzer
- 22
- DurchflussreaktorFlow reactor
- 33
- Detektordetector
- 44
- Verteilerdistributor
- 55
- Trocknerdryer
- 66
- Ausgangoutput
- 77
- Elektrodeelectrode
- 88th
- Gegenelektrodecounter electrode
- 99
- Dielektrikumdielectric
- 1010
- Plasmaplasma
- AA
- Analysengasanalysis gas
- TT
- Trägergascarrier gas
- PP
- Probesample
ZITATE ENTHALTEN IN DER BESCHREIBUNG QUOTES INCLUDE IN THE DESCRIPTION
Diese Liste der vom Anmelder aufgeführten Dokumente wurde automatisiert erzeugt und ist ausschließlich zur besseren Information des Lesers aufgenommen. Die Liste ist nicht Bestandteil der deutschen Patent- bzw. Gebrauchsmusteranmeldung. Das DPMA übernimmt keinerlei Haftung für etwaige Fehler oder Auslassungen.This list of the documents listed by the applicant has been generated automatically and is included solely for the better information of the reader. The list is not part of the German patent or utility model application. The DPMA assumes no liability for any errors or omissions.
Zitierte PatentliteraturCited patent literature
- DE 2806208 A1 [0005] DE 2806208 A1 [0005]
Claims (16)
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DE102010010358A DE102010010358B4 (en) | 2009-12-07 | 2010-03-05 | Method and device for detecting gases |
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DE102009056961 | 2009-12-07 | ||
DE102009056961.8 | 2009-12-07 | ||
DE102010010358A DE102010010358B4 (en) | 2009-12-07 | 2010-03-05 | Method and device for detecting gases |
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Citations (17)
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US4019056A (en) * | 1975-04-28 | 1977-04-19 | Diax Corporation | Infrared laser detector employing a pressure controlled differential optoacoustic detector |
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US7054008B2 (en) * | 2003-02-19 | 2006-05-30 | Mississippi State University | Method and apparatus for elemental and isotope measurements and diagnostics-microwave induced plasma-cavity ring-down spectroscopy |
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2010
- 2010-03-05 DE DE102010010358A patent/DE102010010358B4/en active Active
Patent Citations (18)
Publication number | Priority date | Publication date | Assignee | Title |
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US4019056A (en) * | 1975-04-28 | 1977-04-19 | Diax Corporation | Infrared laser detector employing a pressure controlled differential optoacoustic detector |
US4077774A (en) * | 1977-02-14 | 1978-03-07 | Beckman Instruments, Inc. | Interferent-free fluorescence detection of sulfur dioxide |
DE2806208A1 (en) | 1977-02-14 | 1978-08-17 | Beckman Instruments Inc | METHOD AND DEVICE FOR DETECTION OF SULFUR DIOXYDE IN A GAS SAMPLE |
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US5935519A (en) * | 1988-11-25 | 1999-08-10 | Sievers Instruments, Inc. | Apparatus for the detection of sulfur |
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US6151952A (en) * | 1998-10-26 | 2000-11-28 | California Analytical Instruments, Inc. | System for mass emission sampling of combustion products |
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