WO2012016624A1 - Détermination des rapports isotopiques de carbone et d'azote dans des échantillons d'eau - Google Patents

Détermination des rapports isotopiques de carbone et d'azote dans des échantillons d'eau Download PDF

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Publication number
WO2012016624A1
WO2012016624A1 PCT/EP2011/003412 EP2011003412W WO2012016624A1 WO 2012016624 A1 WO2012016624 A1 WO 2012016624A1 EP 2011003412 W EP2011003412 W EP 2011003412W WO 2012016624 A1 WO2012016624 A1 WO 2012016624A1
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WIPO (PCT)
Prior art keywords
nitrogen
adsorption
isotope
combustion
cooled device
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PCT/EP2011/003412
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German (de)
English (en)
Inventor
Lutz Lange
Ralf Dunsbach
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Elementar Analysensysteme Gmbh
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Application filed by Elementar Analysensysteme Gmbh filed Critical Elementar Analysensysteme Gmbh
Publication of WO2012016624A1 publication Critical patent/WO2012016624A1/fr

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    • 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
    • G01N31/005—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods investigating the presence of an element by oxidation
    • 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
    • G01N33/18—Water
    • G01N33/1826—Organic contamination in water
    • G01N33/1846—Total carbon analysis
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes

Definitions

  • the present invention relates to a method for determining the isotope ratios of carbon in water samples, wherein after Hochtemperaturauf- circuit of the sample, the resulting C0 2 is collected in an adsorption column, after the completion of combustion, the adsorption column is heated and the liberated CO 2 by a Carrier gas is an isotope ratio mass spectrometer (IRMS) is supplied.
  • IRMS isotope ratio mass spectrometer
  • the invention relates to a device for determining the isotopic ratios of carbon in water samples, with a combustion tube, a C0 2 -Adsorptionsklale which is heated, and with an isotopic ratio mass spectrometer, wherein the assembly is purged by a carrier gas to the constituents to be determined the combustion gases to the isotope ratio mass spectrometer.
  • Determining the isotope ratios of carbon in water samples is always of interest when analyzing predominantly water samples for their origin.
  • isotopic analysis of TOC (total organic carbon) in water can provide information about the source of potential groundwater contamination.
  • CONFIRMATION COPY Peroxodisulfatans oxidized to C0 2 , which is concentrated on various purification stages on a GC column and then fed to the mass spectrometer.
  • US Pat. No. 7,213,443 B2 discloses a method and a device for providing gas for the isotope ratio analysis.
  • the gas is generated from an eluate of a liquid chromatograph (LC), after which the gas is separated from the eluate.
  • the gas is then fed to an infrared mass spectrometer (IRMS) for isotopic ratio analysis.
  • LC liquid chromatograph
  • IRMS infrared mass spectrometer
  • This document also describes the coupling of an HPLC (High Performance Liquid Chromatography) with an oxidation interface, wherein the TOC (total organic carbon) in the liquid phase is oxidized to CO 2 and then the isotopic composition is examined.
  • HPLC High Performance Liquid Chromatography
  • the interface consists of the sample feed and a reaction chamber with UV lamp. The oxidation of the organic carbon is realized by the UV radiation of the lamp.
  • the present invention has for its object to provide a method and a corresponding device, which in addition to the determination of the isotopic ratios of carbons in water samples additional statements on the isotopic ratios of nitrogen in this sample can be made without requiring additional complex procedures and corresponding Devices become necessary.
  • This object is achieved in a method of the type mentioned in that for additional determination of the isotope ratios of nitrogen in the water sample, the nitrogen formed is collected in a cooled device after the adsorption that in a reaction zone in the area in front of the cooled device during combustion Nitrogen oxides formed are reduced to nitrogen and that the cooled device until the complete liberation of the nitrogen, is heated and the nitrogen with the carrier gas to the isotope ratio mass spectrometer (IRMS) is supplied.
  • IRMS isotope ratio mass spectrometer
  • the device used to achieve the object comprises a combustion tube, a C02 adsorption column which is heatable, a cooled device arranged after the C0 2 adsorption column, for collecting the nitrogen released from the water sample, a reaction zone in front of the cooled device, to reduce the oxides of nitrogen formed during combustion to nitrogen, and an isotope ratio mass spectrometer (IRMS), wherein the assembly is purged by a carrier gas to the constituents of the combustion gases to the isotope ratio mass spectrometer (IRMS) supply.
  • IRMS isotope ratio mass spectrometer
  • the cooled device is formed by a cold trap.
  • a cold trap which is, for example, a cooled molecular sieve, has the advantage that the entrapment of the nitrogen can be carried out at higher temperatures than when using a pure cooled device.
  • combustion should be performed at temperatures> 800 ° C. If combustion occurs at lower temperatures, there is no assurance that complete oxidation of all organic compounds will occur.
  • a combustion temperature of 1150 ° C is to be selected.
  • the SO 2 formed during the combustion should be adsorbed on an additional adsorption trap and the adsorbed SO 2 should be fed to the isotope ratio mass spectrometer (IRMS) as the last isotope determination by heating the adsorption trap.
  • IRMS isotope ratio mass spectrometer
  • Figure 1 shows schematically the structure of a device according to the invention
  • Figure 2 is an overview of measurements carried out with the device according to the invention in the form of bar graphs.
  • the device as shown in FIG. 1, comprises a TOC analyzer 1, which is shown only schematically.
  • This TOC analyzer 1 comprises a heatable combustion tube, a sample receiver which can be inserted into the combustion tube with the aqueous sample to be analyzed, and a heater which is designed so that the combustion tube in the region of the sample is at approximately 1150 ° C can be heated to burn the sample at this temperature.
  • the combustion tube is equipped with a connection for a carrier gas.
  • helium is supplied as the carrier gas.
  • the TOC analyzer contains multi-stage drying to ensure complete removal of the water from the carrier gas.
  • the carrier gas flow is equalized over a mass flow controller upstream of the IR detector. The amount of C0 2 , S0 2 and NO produced during combustion is determined by means of IR detection.
  • the TOC analyzer 1 is initially fluidly connected to a reduction tube 2, which is connected on the output side to an SO 2 trap 3.
  • the SO 2 trap 3 is in turn connected on the output side to a CO 2 trap 4.
  • Both the SO 2 trap 3 and the CO 2 trap 4 are designed as U-tube. Both traps are filled with suitable adsorption reagents.
  • the CO 2 trap 4 is followed by a cold trap 5.
  • the gas leaving the cold trap 5 is then fed to an isotope ratio mass spectrometer (IRMS) 6.
  • IRMS isotope ratio mass spectrometer
  • the aqueous sample is input to the TOC analyzer 1.
  • the amount of sample can range from 0.1-1.5 ml.
  • the sample is then burned at 1150 ° C.
  • the organic carbon contained in the sample is converted to CO 2 .
  • This reaction takes place in helium as a carrier gas to CuO as an oxidant, which is filled in the combustion tube of the TOC analyzer instead.
  • the sulfur compounds contained in the sample are converted to SO 2 , while the nitrogen compounds are converted to a mixture of different nitrogen oxides, mainly NO, and to N 2 .
  • the CO2, SO 2 and NO are first quantified in the IR detector, which is part of the TOC device 1.
  • the sample gas is passed after leaving the TOC device 1 through a reduction tube 2, in which the nitrogen oxides are reduced to N 2 . Thereafter, the measurement gas is passed through two adsorption columns 3, 4, of which the first adsorption column 3 adsorbs the SO 2 and the second adsorption column 4 adsorbs the CO 2 .
  • the nitrogen (N 2 ) is then removed in the cold trap 5 from the sample gas by the cold trap is cooled down to -147 ° C. After completion of the combustion, the cold trap 5 is first heated, for which purpose this cold trap 5 is equipped with a corresponding heating device, which is not shown. By this heating, the "frozen" N 2 is released again and in the downstream mass spectrometer 6 isotope distribution
  • the CO 2 trap 4 is now heated, for which purpose it is equipped with a corresponding heating device, which is not shown.
  • the adsorbed CO2 is released and supplied with the carrier gas to the IRMS, where it is analyzed for the isotope distribution 12 C / 13 C.
  • the S0 2 is then desorbed by heating the S0 2 trap 3 and fed to the IRMS 6 to make it 3 to analyze S to the isotopic distribution of 32 S /.
  • FIG. 2 shows the results of a determination of the isotope ratios of TIC (total inorganic carbon - total inorganic carbon) and TOC (total organic carbon - total organic carbon) carried out with the method according to the invention and the device, with a total of seven bar graphs in the overview are shown with the numbers 1 to 7.
  • Drinking water from the region Schweitenmaschinen (district Pfaffenhofen an der Ilm) was used as a sample for the TIC determination (bar chart no. 1).
  • the measured values (hatched bars) measured with the IRMS 6 are indicated in addition to the nominal values resulting from a comparative test using acid expulsion.
  • the isotope ratios for the TOC were determined in solutions of potassium hydrogen phthalate (KHP) (bar chart # 2), trichloroethene (TCE) (bar chart # 3), pentachloroethane (PCE) (bar chart # 4), citric acid (bar chart # 5 ), Caffeine with nitrogen reduction (bargraph # 6), and caffeine without nitrogen reduction (bargraph # 7) were determined and plotted.
  • KHP potassium hydrogen phthalate
  • TCE trichloroethene
  • PCE pentachloroethane
  • citric acid bar chart # 5
  • Caffeine with nitrogen reduction bargraph # 6
  • caffeine without nitrogen reduction was determined and plotted.
  • the measured value of the substances results from comparative measurements on the solid sample, determined by elemental analysis, whereby the desired value is obtained.
  • the bar graphs according to FIG. 2 show that there are practically no deviations between the measured values and the nominal values, with the nominal values being obtained from elementary analysis data. This applies in particular to non-nitrogenous samples (see bar charts Nos. (1) - (5)). For nitrogen-containing samples, a reduction distance is necessary to reduce NO2, since NO2 in the isotope measurement influences the isotope determination of CO 2 .

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Physics & Mathematics (AREA)
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Abstract

L'invention concerne un procédé de détermination des rapports isotopiques de carbone dans des échantillons d'eau, procédé suivant lequel, après la fusion à haute température de l'échantillon, le CO2 qui se forme est recueilli sur une colonne d'adsorption (4), après la fin de la combustion, la colonne d'adsorption (4) est chauffée et le CO2 alors libéré est amené par un gaz porteur à un spectromètre de masse à rapport isotopique (6). Ce procédé est caractérisé en ce que, pour la détermination additionnelle des rapports isotopiques d'azote dans l'échantillon d'eau, l'azote formé est recueilli dans une installation refroidie (5) après la colonne d'adsorption (4), que, dans un trajet de réaction (2) dans la zone avant l'installation refroidie (5), les oxydes d'azote formés lors de la combustion sont réduits en azote, que l'installation refroidie (5) est réchauffée jusqu'à libération totale de l'azote, et que l'azote est amené avec le gaz porteur au spectromètre de masse à rapport isotopique (6). L'invention concerne en outre un dispositif pour la mise en œuvre du procédé.
PCT/EP2011/003412 2010-07-27 2011-07-08 Détermination des rapports isotopiques de carbone et d'azote dans des échantillons d'eau WO2012016624A1 (fr)

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DE201010032396 DE102010032396A1 (de) 2010-07-27 2010-07-27 Verfahren und Vorrichtung zur Bestimmung der Isotopenverhältnisse von Kohlenstoff in Wasserproben
DE102010032396.9 2010-07-27

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014190871A (ja) * 2013-03-27 2014-10-06 Taiyo Nippon Sanso Corp 重酸素水の全有機体炭素の測定方法
WO2015070872A1 (fr) * 2013-11-13 2015-05-21 Nanonord A/S Procédé de détermination quantitative de l'azote dans un liquide aqueux
GB2533398A (en) * 2014-12-19 2016-06-22 Isoprime Ltd Isotope analysis
CN109856308A (zh) * 2019-04-01 2019-06-07 中国地质科学院矿产资源研究所 一种分析氮氧同位素组成的方法及装置
CN110208319A (zh) * 2019-06-05 2019-09-06 北京诺德泰科仪器仪表有限公司 一种杜马斯定氮仪反应管
CN111060634A (zh) * 2019-12-31 2020-04-24 东华理工大学 一种测定水中溶解性有机碳和溶解性总氮同位素比值的方法
KR20210012644A (ko) * 2019-07-26 2021-02-03 한국과학기술연구원 화학사고 후 안정성동위원소 분석을 통한 토양내 화학물질 저감 양상 모니터링을 위한 모의 실험 시스템
CN112362721A (zh) * 2019-07-26 2021-02-12 中国石油化工股份有限公司 连续流模式下检测气体中硫同位素的装置和方法
CN112666245A (zh) * 2020-12-18 2021-04-16 中国科学院地球环境研究所 天然水中铵态氮吸附包的制备方法及其同位素的检测方法
CN113945663A (zh) * 2021-10-22 2022-01-18 自然资源部第三海洋研究所 一种toc-irms联用技术测定水中溶解有机碳同位素方法

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DE102014002266B3 (de) * 2014-02-20 2015-03-19 Elementar Analysensysteme Gmbh Verfahren und Vorrichtung zur Analyse von Stickstoff (N) in einer Probe
CN111983007A (zh) * 2020-08-27 2020-11-24 上海化工研究院有限公司 一种用于测定硝酸或硝酸盐15n同位素丰度的方法与装置
CN114137058A (zh) * 2021-11-04 2022-03-04 山东省海洋资源与环境研究院(山东省海洋环境监测中心、山东省水产品质量检验中心) 一种大型水母种间食物竞争关系的调查方法及其应用

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US7213443B2 (en) 2002-04-16 2007-05-08 University Of Bern Process and apparatus for providing gas for isotopic ratio analysis
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Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014190871A (ja) * 2013-03-27 2014-10-06 Taiyo Nippon Sanso Corp 重酸素水の全有機体炭素の測定方法
WO2015070872A1 (fr) * 2013-11-13 2015-05-21 Nanonord A/S Procédé de détermination quantitative de l'azote dans un liquide aqueux
GB2533398A (en) * 2014-12-19 2016-06-22 Isoprime Ltd Isotope analysis
US10613072B2 (en) 2014-12-19 2020-04-07 Elementar UK Ltd. Isotope analysis
CN109856308B (zh) * 2019-04-01 2024-04-02 中国地质科学院矿产资源研究所 一种分析氮氧同位素组成的方法及装置
CN109856308A (zh) * 2019-04-01 2019-06-07 中国地质科学院矿产资源研究所 一种分析氮氧同位素组成的方法及装置
CN110208319A (zh) * 2019-06-05 2019-09-06 北京诺德泰科仪器仪表有限公司 一种杜马斯定氮仪反应管
KR20210012644A (ko) * 2019-07-26 2021-02-03 한국과학기술연구원 화학사고 후 안정성동위원소 분석을 통한 토양내 화학물질 저감 양상 모니터링을 위한 모의 실험 시스템
CN112362721A (zh) * 2019-07-26 2021-02-12 中国石油化工股份有限公司 连续流模式下检测气体中硫同位素的装置和方法
CN112362721B (zh) * 2019-07-26 2024-04-16 中国石油化工股份有限公司 连续流模式下检测气体中硫同位素的装置和方法
KR102242839B1 (ko) 2019-07-26 2021-04-21 한국과학기술연구원 화학사고 후 안정성동위원소 분석을 통한 토양내 화학물질 저감 양상 모니터링을 위한 모의 실험 시스템
CN111060634A (zh) * 2019-12-31 2020-04-24 东华理工大学 一种测定水中溶解性有机碳和溶解性总氮同位素比值的方法
CN112666245B (zh) * 2020-12-18 2024-01-09 中国科学院地球环境研究所 天然水中铵态氮吸附包的制备方法及其同位素的检测方法
CN112666245A (zh) * 2020-12-18 2021-04-16 中国科学院地球环境研究所 天然水中铵态氮吸附包的制备方法及其同位素的检测方法
CN113945663A (zh) * 2021-10-22 2022-01-18 自然资源部第三海洋研究所 一种toc-irms联用技术测定水中溶解有机碳同位素方法

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