Elementar Analysensysteme GmbH

Hanau am Main, Germany

Elementar Analysensysteme GmbH

Hanau am Main, Germany
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Elementar Analysensysteme GmbH | Date: 2016-12-28

The invention relates to an analyzer and to a method for analyzing carbon and sulfur in metals and in other inorganic substances, comprising a vertical combustion tube having an external induction coil, a charging device for inserting a specimen crucible for the specimen into the combustion tube in the region of the induction coil, and an oxygen supply line and a carrier gas supply line at the upper end of the combustion tube. The charging device feeds the specimen from the upper end of the combustion tube, the combustion products are discharged at the lower end of the combustion tube, and the oxygen supply is done by way of an oxygen lance having a baffle, which closes off the cross-section of the combustion tube above the specimen crucible, leaving an annular gap to the inner side of the combustion tube, via which a carrier gas flowing around the crucible can be supplied.


Sieper H.-P.,Elementar Analysensysteme GmbH | Kupka H.-J.,Elementar Analysensysteme GmbH | Lange L.,Elementar Analysensysteme GmbH | Rossmann A.,Isolab GmbH | And 2 more authors.
Rapid Communications in Mass Spectrometry | Year: 2010

The quantitative conversion of organically bound oxygen into CO, a prerequisite for the 18O/ 16O analysis of organic compounds, is generally performed by high-temperature conversion in the presence of carbon at ~1450°C. Since this high-temperature procedure demands complicated and expensive equipment, a lower temperature method that could be utilized on standard elemental analyzers was evaluated. By substituting glassy carbon with carbon black, the conversion temperature could be reduced to 1170°C. However, regardless of the temperature, N-containing compounds yielded incorrect results, despite quantitative conversion of the bound oxygen into CO. We believe that the problems were partially caused by interfering gases produced by a secondary decomposition of N- and C-containing polymers formed during the decomposition of the analyte. In order to overcome the interference, we replaced the gas chromatographic (GC) separation of CO and N 2 by reversible CO adsorption, yielding the possibility of collecting and purifying the CO more efficiently. After CO collection, the interfering gases were vented by means of a specific stream diverter, thus preventing them from entering the trap and the mass spectrometer. Simultaneously, a make-up He flow was used to purge the gas-specific trap before the desorption of the CO and its subsequent mass spectrometric analysis. Furthermore, the formation of interfering gases was reduced by the use of polyethylene as an additive for analytes with a N:O ratio greater than 1. These methodological modifications to the thermal conversion of N-containing analytes, depending on their structure or O:N ratio, led to satisfactory results and showed that it was possible to optimize the conditions for their individual oxygen isotope ratio analysis, even at 1170°C. With these methodological modifications, correct and precise δ 18O results were obtained on N-containing analytes even at 1170°C. Differences from the expected standard values were below ±1‰ with standard deviations of the analysis <0.2‰. © 2010 John Wiley & Sons, Ltd.


Frey W.,Max Planck Institute for Chemistry | Borrmann S.,Max Planck Institute for Chemistry | Borrmann S.,Johannes Gutenberg University Mainz | Kunkel D.,Max Planck Institute for Chemistry | And 23 more authors.
Atmospheric Chemistry and Physics | Year: 2011

In situ measurements of ice crystal size distributions in tropical upper troposphere/lower stratosphere (UT/LS) clouds were performed during the SCOUT-AMMA campaign over West Africa in August 2006. The cloud properties were measured with a Forward Scattering Spectrometer Probe (FSSP-100) and a Cloud Imaging Probe (CIP) operated aboard the Russian high altitude research aircraft M-55 Geophysica with the mission base in Ouagadougou, Burkina Faso. A total of 117 ice particle size distributions were obtained from the measurements in the vicinity of Mesoscale Convective Systems (MCS). Two to four modal lognormal size distributions were fitted to the average size distributions for different potential temperature bins. The measurements showed proportionately more large ice particles compared to former measurements above maritime regions. With the help of trace gas measurements of NO, NOy, CO2, CO, and O3 and satellite images, clouds in young and aged MCS outflow were identified. These events were observed at altitudes of 11.0 km to 14.2 km corresponding to potential temperature levels of 346 K to 356 K. In a young outflow from a developing MCS ice crystal number concentrations of up to (8.3 ± 1.6) cm-3 and rimed ice particles with maximum dimensions exceeding 1.5 mm were found. A maximum ice water content of 0.05 g m-3 was observed and an effective radius of about 90 μm. In contrast the aged outflow events were more diluted and showed a maximum number concentration of 0.03 cm -3, an ice water content of 2.3 × 10-4 g m-3, an effective radius of about 18 μm, while the largest particles had a maximum dimension of 61 μm. Close to the tropopause subvisual cirrus were encountered four times at altitudes of 15 km to 16.4 km. The mean ice particle number concentration of these encounters was 0.01 cm-3 with maximum particle sizes of 130 μm, and the mean ice water content was about 1.4 × 10-4 g m-3. All known in situ measurements of subvisual tropopause cirrus are compared and an exponential fit on the size distributions is established for modelling purposes.A comparison of aerosol to ice crystal number concentrations, in order to obtain an estimate on how many ice particles may result from activation of the present aerosol, yielded low ratios for the subvisual cirrus cases of roughly one cloud particle per 30 000 aerosol particles, while for the MCS outflow cases this resulted in a high ratio of one cloud particle per 300 aerosol particles. © 2011 Author(s).


Piper T.,University of Lausanne | Piper T.,German Sport University Cologne | Degenhardt K.,University of Lausanne | Federherr E.,Elementar Analysensysteme GmbH | And 3 more authors.
Analytical and Bioanalytical Chemistry | Year: 2013

The hydrogen isotope ratio (HIR) of body water and, therefore, of all endogenously synthesized compounds in humans, is mainly affected by the HIR of ingested drinking water. As a consequence, the entire organism and all of its synthesized substrates will reflect alterations in the isotope ratio of drinking water, which depends on the duration of exposure. To investigate the effect of this change on endogenous urinary steroids relevant to doping-control analysis the hydrogen isotope composition of potable water was suddenly enriched from -50 to 200 ‰ and maintained at this level for two weeks for two individuals. The steroids under investigation were 5β-pregnane-3α,20α-diol, 5α-androst-16-en-3α-ol, 3α-hydroxy-5α-androstan-17-one (ANDRO), 3α-hydroxy-5β-androstan-17-one (ETIO), 5α-androstane- 3α,17β-diol, and 5β-androstane-3α,17β-diol (excreted as glucuronides) and ETIO, ANDRO and 3β-hydroxyandrost-5-en-17-one (excreted as sulfates). The HIR of body water was estimated by determination of the HIR of total native urine, to trace the induced changes. The hydrogen in steroids is partly derived from the total amount of body water and cholesterol-enrichment could be calculated by use of these data. Although the sum of changes in the isotopic composition of body water was 150 ‰, shifts of approximately 30 ‰ were observed for urinary steroids. Parallel enrichment in their HIR was observed for most of the steroids, and none of the differences between the HIR of individual steroids was elevated beyond recently established thresholds. This finding is important to sports drug testing because it supports the intended use of this novel and complementary methodology even in cases where athletes have drunk water of different HIR, a plausible and, presumably, inevitable scenario while traveling. © 2012 Springer-Verlag Berlin Heidelberg.


Fourel F.,University Claude Bernard Lyon 1 | Martineau F.,University Claude Bernard Lyon 1 | Lecuyer C.,University Claude Bernard Lyon 1 | Lecuyer C.,Institut Universitaire de France | And 4 more authors.
Rapid Communications in Mass Spectrometry | Year: 2011

We have used a high-precision, easy, low-cost and rapid method of oxygen isotope analysis applied to various O-bearing matrices, organic and inorganic (sulfates, nitrates and phosphates), whose 18O/16O ratios had already been measured. It was first successfully applied to 18O analyses of natural and synthetic phosphate samples. The technique uses high-temperature elemental analysis-pyrolysis (EA-pyrolysis) interfaced in continuous-flow mode to an isotope ratio mass spectrometry (IRMS) system. Using the same pyrolysis method we have been able to generate a single calibration curve for all those samples showing pyrolysis efficiencies independent of the type of matrix pyrolysed. We have also investigated this matrix-dependent pyrolysis issue using a newly developed pyrolysis technique involving 'purge-and-trap' chromatography. As previously stated, silver phosphate being a very stable material, weakly hygroscopic and easily synthesized with predictable 18O/16O values, could be considered as a good candidate to become a reference material for the determination of 18O/ 16O ratios by EA-pyrolysis-IRMS. Copyright © 2011 John Wiley & Sons, Ltd.


Federherr E.,Elementar Analysensysteme GmbH | Federherr E.,University of Duisburg - Essen | Willach S.,University of Duisburg - Essen | Roos N.,Agilent Technologies | And 3 more authors.
Rapid Communications in Mass Spectrometry | Year: 2016

Rationale In aqueous samples compound-specific stable isotope analysis (CSIA) plays an important role. No direct method (without sample preparation) for stable nitrogen isotope analysis (δ15N SIA) of non-volatile compounds is known yet. The development of a novel HPLC/IRMS interface based on high-temperature combustion (HTC) for both δ13C and δ15N CSIA and its proof of principle are described in this study. Methods To hyphenate high-performance liquid chromatography (HPLC) with isotope ratio mass spectrometry (IRMS) a modified high-temperature combustion total organic carbon analyzer (HTC TOC) was used. A system to handle a continuously large amount of water (three-step drying system), favorable carrier and reaction gas mix and flow, an efficient high-temperature-based oxidation and subsequent reduction system and a collimated beam transfer system were the main requirements to achieve the necessary performance. Results The proof of principle with caffeine solutions of the system succeeded. In this initial testing, both δ13C and δ15N values of tested compounds were determined with precision and trueness of ≤0.5 ‰. Further tests resulted in lower working limit values of 3.5 μgC for δ13C SIA and 20 μgN for δ15N SIA, considering an accuracy of ±0.5 ‰ as acceptable. Conclusions The development of a novel HPLC/IRMS interface resulted in the first system reported to be suitable for both δ13C and δ15N direct CSIA of non-volatile compounds. This highly efficient system will probably open up new possibilities in SIA-based research fields. Copyright © 2016 John Wiley & Sons, Ltd.


Federherr E.,University of Duisburg - Essen | Federherr E.,Elementar Analysensysteme GmbH | Cerli C.,University of Amsterdam | Kirkels F.M.S.A.,University of Amsterdam | And 5 more authors.
Rapid Communications in Mass Spectrometry | Year: 2014

RATIONALE: Traditionally, dissolved organic carbon (DOC) stable isotope analysis (SIA) is performed using either offline sample preparation followed by elemental analyzer/isotope ratiomass spectrometry (EA/IRMS) or awet chemical oxidation (WCO)-based device coupled to an isotope ratio mass spectrometer. The first method is time-consuming and laborious. The second involves the risks of underestimation of DOC concentration and isotopic fractionation due to incomplete oxidation. The development of an analytical method for accurate and sensitive DOC SIA is described in this study. METHODS: A high-temperature combustion (HTC) system improves upon traditional methods. A novel total organic carbon (TOC) system, specially designed for SIA, was coupled to an isotope ratio mass spectrometer. An integrated purge and trap technique (peak focusing), flexible injection volume (0.05-3 mL), favorable carrier gas flow, modified ash crucible, new design of combustion tube and optimized drying system were used to achieve the necessary performance. RESULTS: The system can reliably measure concentrations up to 1000 mgC/L. Compounds resistant to oxidation, such as barbituric acid, melamine and humic acid, were analyzed with recovery rates of 100 ± 1% proving complete oxidation. In this initial testing, the δ13C values of these compounds were determined with precision and trueness of ≤0.2‰ even with 3.5% salinity. Further tests with samples with low DOC concentrations resulted in LOQSIA method values of 0.5 mgC/L and 0.2 mgC/L for LOQSIA instr, considering an accuracy of ±0.5‰ as acceptable. CONCLUSIONS: The novel HTC system coupled to an isotope ratio mass spectrometer resulted in significantly improved sensitivity. The system is suitable for salt-containing liquids and compounds that are resistant to oxidation, and it offers a large concentration range. A second paper (which follows this one in this issue) will present a more comprehensive assessment of the analytical performance with a broad set of solutions and real samples. This highly efficient TOC stable isotopic analyzer will probably open up new possibilities in biogeochemical carbon cycle research. Copyright © 2014 John Wiley & Sons, Ltd.


Kirkels F.M.S.A.,University of Amsterdam | Cerli C.,University of Amsterdam | Federherr E.,University of Duisburg - Essen | Federherr E.,Elementar Analysensysteme GmbH | And 3 more authors.
Rapid Communications in Mass Spectrometry | Year: 2014

RATIONALE: Dissolved organic carbon (DOC) plays an important role in carbon cycling, making precise and routine measurement of δ13C values and DOC concentration highly desirable. A new promising system has been developed for this purpose. However, broad-scale application of this new technique requires an in-depth assessment of analytical performance, and this is described here. METHODS: A high-temperature combustion Total Organic Carbon analyzer was interfaced with continuous flow isotope ratio mass spectrometry (TOC/IRMS) for the simultaneous analysis of the bulk DOC concentration and δ13C signature. The analytical performance (precision, memory effects, linearity, volume/concentration effects, accuracy) was thoroughly evaluated, including realistic and challenging conditions such as low DOC concentrations and natural DOC. RESULTS: High precision (standard deviation, SD predominantly ≤0.15 ‰) and accuracy (R2 = 0.9997) were achieved for the δ13C analysis of a broad diversity of DOC solutions. Simultaneously, good results were obtained for the measurement of DOC concentration. Assessment of natural abundance and slightly 13C-enriched DOC, a wide range of concentrations (∼0.2-150 mgC/L) and injection volumes (0.05-3 mL), demonstrated minor/negligible memory effects, good linearity and flexible usage. Finally, TOC/IRMS was successfully applied to determine low DOC concentrations (<2 mgC/L) and DOC from diverse terrestrial, freshwater and marine environments (SD ≤0.23 ‰). CONCLUSIONS: TOC/IRMS enables fast and reliable measurement of DOC concentrations and δ13C values in aqueous samples, without pre-concentration and freeze-drying. Further investigations should focus on complex, saline matrices and very low DOC concentrations, to achieve a potential lower limit of 0.2 mgC/L. Thus, TOC/IRMS will give DOC research in terrestrial and aquatic environments a huge impulse with high-resolution, routine δ13C analysis. Copyright © 2014 John Wiley & Sons, Ltd.


PubMed | Elementar Analysensysteme GmbH, Agilent Technologies and University of Duisburg - Essen
Type: Journal Article | Journal: Rapid communications in mass spectrometry : RCM | Year: 2016

In aqueous samples compound-specific stable isotope analysis (CSIA) plays an important role. No direct method (without sample preparation) for stable nitrogen isotope analysis ((15) N SIA) of non-volatile compounds is known yet. The development of a novel HPLC/IRMS interface based on high-temperature combustion (HTC) for both (13) C and (15) N CSIA and its proof of principle are described in this study.To hyphenate high-performance liquid chromatography (HPLC) with isotope ratio mass spectrometry (IRMS) a modified high-temperature combustion total organic carbon analyzer (HTC TOC) was used. A system to handle a continuously large amount of water (three-step drying system), favorable carrier and reaction gas mix and flow, an efficient high-temperature-based oxidation and subsequent reduction system and a collimated beam transfer system were the main requirements to achieve the necessary performance.The proof of principle with caffeine solutions of the system succeeded. In this initial testing, both (13) C and (15) N values of tested compounds were determined with precision and trueness of 0.5. Further tests resulted in lower working limit values of 3.5 gC for (13) C SIA and 20 gN for (15) N SIA, considering an accuracy of 0.5 as acceptable.The development of a novel HPLC/IRMS interface resulted in the first system reported to be suitable for both (13) C and (15) N direct CSIA of non-volatile compounds. This highly efficient system will probably open up new possibilities in SIA-based research fields. Copyright 2016 John Wiley & Sons, Ltd.


PubMed | Elementar Analysensysteme GmbH
Type: Journal Article | Journal: Rapid communications in mass spectrometry : RCM | Year: 2010

The quantitative conversion of organically bound oxygen into CO, a prerequisite for the (18)O/(16)O analysis of organic compounds, is generally performed by high-temperature conversion in the presence of carbon at 1450C. Since this high-temperature procedure demands complicated and expensive equipment, a lower temperature method that could be utilized on standard elemental analyzers was evaluated. By substituting glassy carbon with carbon black, the conversion temperature could be reduced to 1170C. However, regardless of the temperature, N-containing compounds yielded incorrect results, despite quantitative conversion of the bound oxygen into CO. We believe that the problems were partially caused by interfering gases produced by a secondary decomposition of N- and C-containing polymers formed during the decomposition of the analyte. In order to overcome the interference, we replaced the gas chromatographic (GC) separation of CO and N(2) by reversible CO adsorption, yielding the possibility of collecting and purifying the CO more efficiently. After CO collection, the interfering gases were vented by means of a specific stream diverter, thus preventing them from entering the trap and the mass spectrometer. Simultaneously, a make-up He flow was used to purge the gas-specific trap before the desorption of the CO and its subsequent mass spectrometric analysis. Furthermore, the formation of interfering gases was reduced by the use of polyethylene as an additive for analytes with a N:O ratio greater than 1. These methodological modifications to the thermal conversion of N-containing analytes, depending on their structure or O:N ratio, led to satisfactory results and showed that it was possible to optimize the conditions for their individual oxygen isotope ratio analysis, even at 1170C. With these methodological modifications, correct and precise (18)O results were obtained on N-containing analytes even at 1170C. Differences from the expected standard values were below 1 with standard deviations of the analysis <0.2.

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