EP1240510A2 - Analyse de la teneur totale en azote, soufre et chlore - Google Patents

Analyse de la teneur totale en azote, soufre et chlore

Info

Publication number
EP1240510A2
EP1240510A2 EP00990796A EP00990796A EP1240510A2 EP 1240510 A2 EP1240510 A2 EP 1240510A2 EP 00990796 A EP00990796 A EP 00990796A EP 00990796 A EP00990796 A EP 00990796A EP 1240510 A2 EP1240510 A2 EP 1240510A2
Authority
EP
European Patent Office
Prior art keywords
sample
furnace
analytical
detector
analytical system
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Withdrawn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
EP00990796A
Other languages
German (de)
English (en)
Inventor
Herbert A. Hernandez
Norbert W. Lenk
Ulrich Kathe
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.)
Aj Idc Gerateentwicklungsgesellschaft Mbh
Original Assignee
Aj Idc Gerateentwicklungsgesellschaft Mbh
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 Aj Idc Gerateentwicklungsgesellschaft Mbh filed Critical Aj Idc Gerateentwicklungsgesellschaft Mbh
Publication of EP1240510A2 publication Critical patent/EP1240510A2/fr
Withdrawn legal-status Critical Current

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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
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/403—Cells and electrode assemblies
    • G01N27/404—Cells with anode, cathode and cell electrolyte on the same side of a permeable membrane which separates them from the sample fluid, e.g. Clark-type oxygen sensors
    • G01N27/4045—Cells with anode, cathode and cell electrolyte on the same side of a permeable membrane which separates them from the sample fluid, e.g. Clark-type oxygen sensors for gases other than oxygen

Definitions

  • the present invention relates to an apparatus and method for determination of total nitrogen, sulfur and/or chlorine content in aqueous and hydrocarbon matrices, and more particularly to oxidizing a sample by combustion and detecting specific chemical compounds using an electrochemical detector.
  • toxic gas monitors are available for measuring parts per million levels of gaseous nitric oxide (NO), sulfur dioxide (S0 2 ) and hydrogen chloride (HCI) using electrochemical principles.
  • NO gaseous nitric oxide
  • S0 2 sulfur dioxide
  • HCI hydrogen chloride
  • a worker at risk to exposure to a toxic gas may wear a device for sampling and testing the air he or she breathes.
  • the device may warn the worker of an acute exposure or record a cumulative exposure.
  • Such a device is typically measuring a very minute concentration using a very large sample volume, yet the device must be small enough to be worn by a worker.
  • a simple sensor operating on electrochemical principles has two electrodes, a sensing electrode and a counter electrode, separated by a thin layer of electrolyte and connected by a low resistance external circuit. Gas diffusing into the sensor is reacted at the surface of the sensing electrode, by oxidation or reduction, causing a current to flow between the electrodes through the external circuit. The current is proportional to the concentration of gas and can be measured across a load resistor in the external circuit. For reaction to take place the sensing electrode potential must be within a specific range.
  • U.S. Patent Nos. 4,474,648 and 4,587,003 both issued to Tantram et al. and entitled "Gas Sensor," are illustrative of electrochemical gas sensors and are incorporated by reference for all purposes.
  • the sensing electrode potential follows that of the counter electrode. If the gas concentration continues to rise, the sensing electrode potential will eventually move outside its permitted range. At this point the sensor becomes nonlinear, which effectively limits the upper concentration of gas a two- electrode sensor can be used to measure. Nonlinearity due to polarization is avoided by adding a third electrode, a reference electrode, and using an external poten- tiostatic operating circuit.
  • the sensing electrode will exhibit a small signal, which is known as its baseline.
  • the baseline can be set to zero, but the magnitude of the baseline increases exponentially with temperature.
  • a fourth electrode, an auxiliary electrode, can be used to offset the effects of temperature changes.
  • An analyzer using fluorescence and chemiluminescent detectors requires a number of components such as an ultraviolet light source and associated optics, photomul- tiplier tubes and an ozone generator. These various components are each a potential source of error in a measurement, and some components are sensitive, delicate or fragile as well as expensive. Consequently, a need remains for a simpler and less expensive laboratory or field analyzer capable of measuring total nitrogen, sulfur and/or chlorine.
  • the present invention provides an analyzer system and a method for measuring total nitrogen, sulfur and/or chlorine in a solid, liquid or gaseous sample.
  • the sample is fed to a furnace module where it is burned in the presence of oxygen to produce a combustion gas.
  • Essentially all nitrogen in the sample except diatomic nitrogen (N 2 ), is converted to nitric oxide (NO).
  • Essentially all sulfur in the sample is converted to sulfur dioxide (S0 2 ), and essentially all chlorine in the sample is converted to hydrogen chloride (HCI).
  • Water is typically in the combustion gas and is preferably removed in a dryer. Dry combustion gas is fed to an electrochemical detector, one detector for each specific compound to be measured.
  • a control system provides a user interface for monitoring and controlling several components such as the furnace module and the detector.
  • Fig. l is a schematic diagram of an analytical system according to the present invention.
  • Fig.2 is a schematic diagram of a control and interface system for the analytical system of Fig. l .
  • an analytical system 1 0 for measuring total nitrogen, sulfur and/or chlorine in a sample is illustrated schematically according to the present in- vention.
  • An inert carrier gas 1 2, such as high-purity argon, is fed to a sample introduction apparatus 1 4, and a mass flow controller 1 6 regulates the flow of carrier gas 1 2.
  • Sample introduction apparatus 1 4 receives the sample for analysis, and the sample can be an aqueous or a hydrocarbon matrix and can be solid, liquid, gaseous or otherwise. Solid samples can be introduced by a quartz capsule or a quartz sam- pie boat.
  • Liquid samples can be introduced by microliter syringe, quartz capsule or quartz sample boat and gaseous samples can be introduced by a gas sample valve or by a gas-tight syringe.
  • the sample introduction apparatus must be suitable for the state of the sample and must be capable of delivering the sample accurately and repeatably.
  • Oxygen 1 8 which is preferably a high-purity oxygen, is mixed with the sample from sample introduction apparatus 1 4, and the mixture is fed to a high-temperature furnace module 20. Oygen 1 8 is also fed directly to furnace module 20, and a mass flow controller 22 regulates the combined total flow of oxygen 1 8.
  • Furnace module 22 includes a high-temperature tube furnace, which can be a quartz combustion tube capable of continuous operation in the range of about 900 to 1 200'C or a ceramic combustion tube capable of continuous operation up to at least about 1 600 * C and preferably up to about 1 800'C.
  • the quartz combustion tube is packed with quartz chips, and a type K thermocouple or its equivalent is used for temperature measurement.
  • a cooling fan is provided for removing excess heat from a housing for furnace module 22.
  • a furnace suitable for use as furnace module 20 is available from APS Technologies, inc. of Spring, Texas.
  • furnace module 22 the sample is vaporized in the high-temperature oxygen-rich atmosphere, and the sample is oxidized.
  • This oxidation of the sample and all of its constituents produces a combustion gas containing stable oxides, except for chlorine, which is unstable as an oxide.
  • Chlorine reacts with water in the combustion gas to produce hydrogen chloride (hereinafter referred to as "HCI"), the water being produced as a by-product of combustion or introduced as part of the sample.
  • HCI hydrogen chloride
  • Nitrogen in the sample except diatomic nitrogen, N 2 , is converted to nitric oxide (hereinafter referred to as "NO"), and sulfur in the sample is converted to sulfur dioxide (hereinafter referred to as "S0 2 ").
  • Nitrogen, sulfur and chlorine in the sample can exist as essentially any compound, and compounds containing the elements nitrogen, sulfur and chlorine in the sample are converted essentially completely to NO, S0 ⁇ and HCI, respectively.
  • measure- ment of these compounds provides a measurement of the total amount of these elements in the sample.
  • the nitrogen and sulfur may be bound to a hydrocarbon molecule, and the chlorine may be present as a chlorinated organic compound.
  • the combustion gas produced in furnace module 22 is dried in a gas dehydration unit 24 to remove water, producing a water-free or dry combustion gas sample.
  • Water in the combustion gas may have been produced in furnace module 22 as an oxidation by-product or, for example, it may have been part of an aqueous sample. In either case it is preferable to remove the water.
  • Gas dehydration unit 24 includes a permeation dryer such as that sold by Perma Pure, Inc. under the registered trademark Nafion, part number PD-624-1 2PP-APS or an equivalent dryer.
  • a 98% sulfuric acid scrubber with a heated gas transfer tube can be used to remove water from the combustion gas, thus producing the water-free or dry combustion gas sample.
  • Micro-electrochemical detector system 26 includes at least one electrochemical detector and as many as three. In this embodiment three electrochemical detectors are illustrated, an electrochemical NO detector 26a, an electrochemical S0 2 detector 26b and an electrochemical HCI detector 26c. Electrochemical NO detector 26a selectively detects NO, and other compounds or species in the dry combustion gas sample do not interfere with the measurement of NO in the sample. Electrochemical S0 2 detector 26b selectively detects S0 2 , and other compounds or species in the dry combustion gas sample do not interfere with the measurement of S0 2 in the sample. Likewise, electrochemical HCI detector 26c selectively detects HCI, and other compounds or species in the dry combustion gas sample do not interfere with the measurement of HCI in the sample.
  • Electrochemical detector system 26 has solenoid valves 28 for directing sample flow through electrochemical detectors 26a, 26b and 26c, which may be operated in parallel or in series, and if in series, then in any sequence since there is no interference in measurements. Vents 30 are provided for venting the sample from electrochemical detectors 26a, 26b and 26c.
  • electrochemical detectors 26a, 26, b and 26c can be used in electrochemical detector system 26 or any one or two can be used. A particular application will dictate which of electrochemical detectors 26a, 26b and/or 26c to use. For more information on electrochemical detectors 26a, 26b and 26c, see the patents concerning electrochemical detectors which were incorporated by reference above.
  • a control system 32 provides a user interface, processing capability and electronics for operating, through an electronic interface 34, sample introduction apparatus 1 4, mass flow controllers 1 6, 22, furnace module 20, gas dehydration unit 24 and electrochemical detector system 26. Dark, heavy lines indicate electrical connection between components, while light, fine lines indicate the flow of sample, carrier gas 1 2 and/or oxygen 1 8.
  • Control system 32 uses presently a personal computer, and a graphical interface is provided using software such as that provided by Microsoft corporation under the trademarks Windows 95 or Windows NT.
  • a monitor 36, a keyboard and a pointing device, such as a mouse provide an interface to control system 32 for a user.
  • Control system 32 stores and displays data via monitor 36 or a printer 38, and control system 32 can be networked with other computers via a network system 40.
  • Software such as is used typically with such analyzer systems, is provided for control of the various components and for Manipulation, display and analysis of data.
  • Control system 32 includes a PC bus 42, which is the main bus in the personal computer.
  • PC boards 44a, 44b, 44c and 44d plug directly into PC bus 42 and provide essentially realtime control for the various components in analytical system 1 0 while the personal computer provides supervisory control, monitoring and data storage and analysis.
  • PC board 44a is connected to a furnace PC board 46 and is always included.
  • PC board 44a provides essentially realtime control for furnace module 22, sample introduction apparatus 1 4 and mass flow controllers 1 6 and 22, as well as for various timed events. At least one of PC boards 44b, 44c or 44d is included, depending on the application and thus the chemical compound to be detected and measured.
  • a detector interface board 48 provides a power, a ground and a signal connection between PC boards 44b, 44c and/or 44d and elec- trochemical detector cells 26a', 26b' and/or 26c' via coaxial cables.
  • An interconnect cable connects PC board 44a to furnace PC board 46 and PC boards 44b, 44c and 44d to detector interface board 48.
  • control system 32 is activated and furnace module 20 is heated to its operating temperature.
  • Inert carrier gas 1 2 such as dry argon or helium with a minimum purity of 99.9%, and oxygen 1 8, with preferably a minimum purity of 99.7%, are available from pressurized sources and mass flow controllers 1 6 and 22, respectively, control flow of these gases through the system.
  • Analytical system 1 0 is previously assembled with a proper array of electrochemical detectors 26a, 26b and/or 26c for the sample to be analyzed.
  • a 1 to 1 00 ⁇ L sample is fed to analytical system 1 0 via sample introduction apparatus 1 4 using a quartz boat, quartz capsule, syringe or valve as described above.
  • an automatic sampler can be used for feeding samples sequentially to the system.
  • Oxygen present in the high-temperature (900 to 1 600 ° C, typically about I000 ° C) tube furnace provides a highly oxidative atmosphere for oxidizing the sample as it is carried through furnace module 20. If the sample contains nitrogen, sulfur and chlorine compounds, then combustion gas from furnace module 20 or gas dehydra- tion unit 24 contains NO, S0 2 and HCI, respectively.
  • the sample can contain all three, any one, or any two compounds containing nitrogen, sulfur and/or chlorine.
  • Electrochemical detectors 26a, 26b and/or 26c yield a signal proportional to the concentration of NO, S0 2 and/or HCI, respectively, in the sample, which, by calculation, is used to determine the total nitrogen, sulfur and/or chlorine in the sample. Such determination can be viewed on monitor 36, printed on printer 38 or transferred to another computer via network 40.
  • Chemiluminescent and fluorescent detectors became the standard or typical detector of choice for measuring total nitrogen and sulfur, respectively. This was the case in spite of the complexity of the equipment due to the number of components and the sensitivity or fragility of the components. In years past alternative detectors were considered including detectors based on electrochemical analysis. However, electrochemical analysis was dismissed as an unsatisfactory solution, and this view continued to exist until subsequent experimentation resulted in the present invention.
  • Table 1 is representative data obtained for the analysis of nitrogen in a hydrocarbon matrix by combustion/chemiluminescence and by combustion/electrochemical detection.
  • the electrochemical detector had a higher sensitivity (1 53,463 vs. 1 09,658 counts) for measuring nitrogen in the sample than did the chemiluminescent detector. This was a surprising result because in earlier years electrochemical analysis had been dismissed as an unsatisfactory method for determining total nitrogen in a sample. Further, the electrochemical detector had a better repeatability (as indicated by the standard deviation of 4,51 7 vs. 7,51 9 counts) than did the chemiluminescent detector. This was also an unexpected result. It was discovered that the signal-to-noise ratio for analytical system 1 0 is significantly better than that for a prior art system using chemiluminescent and fluorescent detectors, both the sensitivity being greater and the noise being less.
  • a signal-to-noise ratio for a prior art system using chemiluminescent and fluorescent detectors is commonly accepted as 2 to 1 , but the signal-to-noise ratio for analytical system 1 0 is significantly better at 1 0 to 1 or greater.
  • the detectable quantity of nitrogen, sulfur or chlorine in a sample using analytical system 1 0 is less than about 1 part per million by weight or 1 mg/kg.
  • Table 2 is representative data for the analysis of nitrogen, sulfur and chlorine in a hydrocarbon matrix by combustion/electrochemical detection. All samples were injected with a microliter syringe, attached to a liquid autosampler system which tends to remove sampling as a source of error. TABLE 2.
  • the integrator count data in Table 2 indicates good sensitivity for nitrogen, sulfur or chlorine by the electrochemical detectors, and the standard deviation indicates good repeatability.
  • electrochemical detectors which were used for personnel safety monitoring, were better detectors for use in analyzers in the field of industrial process measurements than chemiluminescent and fluorescent detectors.
  • Analytical system 1 0 and its electrochemical detector system 26 are simpler for a user to operate and maintain than is an analytical system using chemiluminescent and fluorescent detectors.
  • Prior art analytical systems using chemiluminescent and fluorescent detectors require an ozone generator, an ultraviolet light source, optics and photomultiplier tubes, each of which is a source of error, such as baseline drift, and each of which contributes to the cost of building the analytical system.
  • Analytical system 1 0 on the other hand requires fewer components, and electrochemical detector system 26 is more durable and capable of withstanding environmental factors encountered typically in a laboratory or field environment. Analytical system 1 0 is sufficiently durable for use in a field environment as a process analyzer with the addition of a proper housing and enclosure to meet field safety requirements and necessary modifications such as cabling for remote operation. Electrochemical detectors 26a, 26b and 26c are less expensive than some of the components in the prior art analytical system, so analytical system 1 0 costs less to build than does the prior art system. Analytical system 1 0 offers the further advantage of chlorine analysis, which is not available in a typical prior art analyzer system used for total nitrogen and/or sulfur analysis.

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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)
  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)

Abstract

L'invention concerne l'analyse de la teneur totale en azote, soufre et/ou chlore, qu'on effectue en brûlant un échantillon liquide ou gazeux avec de l'oxygène dans un four à haute température afin de former un gaz de combustion qui est alors séché. On passe le gaz de combustion sec dans un détecteur électrochimique pour que chaque élément soit mesuré, les détecteurs étant disposés soit en parallèle soit en série, ce qui fournit une détermination individuelle de la teneur de l'élément dans l'échantillon. Un système de commande fournit une interface utilisateur permettant de manipuler et de commander l'introduction de l'échantillon dans le four et le fonctionnement du four, de l'unité de séchage et du détecteur électrochimique. Le système stocke, enregistre et affiche, par ailleurs, les données.
EP00990796A 1999-12-20 2000-12-19 Analyse de la teneur totale en azote, soufre et chlore Withdrawn EP1240510A2 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US468011 1983-02-18
US46801199A 1999-12-20 1999-12-20
PCT/EP2000/012940 WO2001046683A2 (fr) 1999-12-20 2000-12-19 Analyse de la teneur totale en azote, soufre et chlore

Publications (1)

Publication Number Publication Date
EP1240510A2 true EP1240510A2 (fr) 2002-09-18

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Country Status (4)

Country Link
EP (1) EP1240510A2 (fr)
JP (1) JP2004520566A (fr)
CN (1) CN1413301A (fr)
WO (1) WO2001046683A2 (fr)

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US6830730B2 (en) 2001-09-11 2004-12-14 Spectrolanalytical Instruments Method and apparatus for the on-stream analysis of total sulfur and/or nitrogen in petroleum products
DE102006049927A1 (de) * 2006-02-10 2007-08-16 Elementar Analysensysteme Gmbh Vorrichtung und Verfahren zum automatischen Bestimmen des Gehaltes an Chlor in Proben
US7666423B2 (en) 2006-07-28 2010-02-23 Children's Memorial Hospital Methods of inhibiting tumor cell aggressiveness using the microenvironment of human embryonic stem cells
CN101571507B (zh) * 2008-04-29 2012-07-04 浙江省电力试验研究院 磷酸酯抗燃油氯含量高温燃烧微库仑分析方法
JP5399795B2 (ja) * 2009-07-14 2014-01-29 株式会社 ナックテクノサービス 有機・無機試料中のハロゲンおよび硫黄の分析方法ならびに二段挿入方式オートサンプラを備えた自動分析装置
CN102798695A (zh) * 2012-08-27 2012-11-28 苏州金宏气体股份有限公司 测定高纯及超纯氨中痕量氯含量的方法
CN103454356A (zh) * 2013-09-11 2013-12-18 神华集团有限责任公司 测定煤直接液化产品中总氯含量的方法
CN104991034A (zh) * 2015-06-26 2015-10-21 浙江凯恩特种材料股份有限公司 电气用纸及其生产用纸板与纸浆微量氯元素燃烧测试方法
US11360064B2 (en) * 2016-03-30 2022-06-14 3M Innovative Properties Company Oxy-pyrohydrolysis system and method for total halogen analysis
CN106153699B (zh) * 2016-07-28 2019-03-15 中国石油化工股份有限公司 一种提高总硫分析准确性的方法
GB201710412D0 (en) * 2017-06-29 2017-08-16 Johnson Matthey Plc A system and method for measuring total chloride content in a process product stream
KR102155406B1 (ko) * 2017-08-18 2020-09-11 주식회사 엘지화학 아연철산화물 내 잔류 Cl의 정량분석 방법
US20220011237A1 (en) * 2018-12-12 2022-01-13 Shimadzu Corporation Sulfur chemiluminescence detector

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Also Published As

Publication number Publication date
JP2004520566A (ja) 2004-07-08
WO2001046683A2 (fr) 2001-06-28
CN1413301A (zh) 2003-04-23
WO2001046683A3 (fr) 2001-12-27

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