Knowledge Base

15 of 349
View1
  • IRMS
  • MAT 253
  • TC/EA
  • Hydrogen isotopes
  • Geological Samples

An online method combining a thermal conversion elemental analyzer with isotope ratio mass spectrometry for the determination of hydrogen isotope composition and water concentration in geological samples

Bing Gong, Yong-Fei Zheng and Ren-Xu Chen

1) CAS Key Laboratory of Crust-Mantle Materials and Environments, School of Earth and Space Science, University of Science and Technology of China, Hefei 230026, China

Rapid Communications in Mass Spectrometry (2007), V21, pp1386–1392, doi: 10.1002/rcm.2973

Goal: An online continuous-flow method, combining a thermal conversion elemental analyzer (TC/EA) with isotope ratio mass spectrometry (MS), is evaluated for the determination of both the hydrogen isotope composition and the water concentration of hydrous and nominally anhydrous minerals. The technique involves reduction of hydrous minerals or nominally anhydrous minerals by reaction with glassy carbon at 1450-C in a helium stream.

View0
  • IRMS
  • Delta Plus XP
  • TC/EA
  • Explosives
  • 13C, 15N, 18O

Investigation of isotopic linkage between precursor and product in the synthesis of a high explosive

Claire M. Lock (1) and Wolfram Meier-Augenstein (2)

1) Forensic Explosives Laboratory, Dstl, Fort Halstead, Sevenoaks, Kent TN14 7BP, UK, 2) Stable Isotope Forensics Facility, Environ. Eng. Res. Centre, S.P.A.C.E., Queen’s University Belfast, David Keir Building, Belfast BT9 5AG, UK

Forensic Science International (2008), V179, pp157–162, doi:10.1016/j.forsciint.2008.05.015

Goal: In criminal proceedings involving illegally manufactured substances, evidence demonstrating the manufacture is required for successful prosecution. In many circumstances the presence of manufacturing equipment and ‘recipes’ are clear indicators. However establishing chemical links between starting materials and products would be beneficial additional evidence in such circumstances. We report here the results of an isotope study investigating a link between hexamine used as a starting material and the product explosive RDX, manufactured using the Woolwich process. Isotopic composition of hexamine and RDX was analysed by stable isotope ratio mass spectrometry. Five different hexamine samples were selected from a group of eleven for use in this study. One of the five hexamine samples was used twice, providing data on the reproducibility of the synthesis. Carbon and nitrogen isotope analysis of the hexamine starting material and RDX products reveals a reproducible relationship between reactant and product.

View0
  • IRMS
  • Delta V Advantage
  • Elemental Analyzer
  • Fipronil
  • Authenticity
  • 13C, 15N, 34S

Isotopic Fingerprinting for the Authenticity Control of Crop Protection Active Compounds using the Representative Insecticide Fipronil

Philipp Weller (1), Markus Boner (2), Hilmar Foerstel (2), Horst Becker (1), Benjamin Peikert (1) and Wolfgang Dreher (1)

1) BASF SE, Agricultural Solutions, APE/MB, Speyerer Strasse 2, 67117 Limburgerhof, Germany, 2) TÜV Rheinland Agroisolab GmbH, TÜV Rheinland-Gruppe, Germany

Journal of Agricultural and Food Chemistry (2011), V59 (9), pp 4365–4370, doi:

Goal: Isotopic fingerprinting was evaluated for its potential to generate characteristic fingerprints of crop protection products in an extensive survey, using the insecticide Fipronil. One hundred and twenty batches of Fipronil from the BASFproduction site in France were analyzed for the isotope ratios of δ13C, δ15N, and δ34S. Samples spanned a production time of four years and were analyzed by elemental analysis, coupled to isotope ratio mass spectrometry (EA/IRMS). A number of Fipronil samples from other sources were analyzed in the same manner and were compared to the samples from BASF by means of multivariate data analysis. The isotopic fingerprint was sufficiently specific to differentiate between Fipronil from BASF production and Fipronil from other producers. This suggests that isotopic fingerprinting is suitable for the authenticity control of active compounds in crop protection products. It is anticipated that this technique will deliver great benefit in the defense against counterfeits and illegal parallel imports.

View2
  • IRMS
  • Delta Plus XP
  • Hair
  • 2H and 18O

Stable 2H isotope analysis of modern-day human hair and nails can aid forensic human identification

Isla Fraser and Wolfram Meier-Augenstein

Environmental Forensics and Human Health Lab., Environmental Engineering Research Centre, Queen’s University Belfast, Belfast BT9 5AG, UK

Rapid Communications in Mass Spectrometry (2007), V21, pp3279–3285, doi: 10.1002/rcm.3209

Goal: Continuous-flow isotope ratio mass spectrometry (CF-IRMS) was used to compare 2H isotopic composition at natural abundance level of human scalp hair and fingernail samples collected from subjects worldwide with interpolated d2H precipitation values at corresponding locations. The results showed a strong correlation between d2H values of meteoric water a nd hair (r2 = 0.86), while the corresponding correlation for nails was not as strong (r2 = 0.6). Offsets of -180 permil and -127 permil were observed when calculating solutions of the linear regression analyses for d2H vs. d18O correlation plots of hair and nail samples, respectively. Compared with the +10 permil offset of the global meteoric water line equation these findings suggested that d18O data from hair and nail would be of limited diagnostic value. The results of this pilot study provide for the first time tentative correlations of 2H isotopic composition of human hair and nails with local water.

View1
  • IRMS
  • Delta Plus XP
  • Flash 1112
  • Olive Oil
  • 2H/1H, 18O/16O and 13C/12C
  • Climate

Coast and year effect on H, O and C stable isotope ratios of Tyrrhenian and Adriatic italian olive oils

L. Bontempo (1), F. Camin (1), R. Larcher (1), G. Nicolini (1), M. Perini (1) and A. Rossmann (2)

1) Edmund Mach Foundation, IASMA Research Center, Agrifood Quality Department, via E. Mach, 38010 San Michele all’Adige (TN), Italy, 2) Isolab GmbH, Laboratorium für Stabile Isotope, Woelkestrasse 9/I, 85301 Schweitenkirchen, Germany

Rapid Communications in Mass Spectrometry (2009), V23, pp1043–1048, doi: 10.1002/rcm.3968

Goal: The paper discusses the 2H/1H, 18O/16O and 13C/12C ratios of 196 authentic Italian extra-virgin olive oils produced in 3 years on the Tyrrhenian and Adriatic coasts. The 2H/1H and 18O/16O ratios were linearly and positively correlated. The year of production influenced mainly 18O/16O in relation to the amount of rainfall and the atmospheric humidity in the period of oil accumulation in the olives. The 2H/1H ratio significantly distinguished the olive oils produced on the Adriatic coast from those on the Tyrrhenian coast in each year. This coast effect is a consequence of the different sources and isotopic compositions of the rainfall and the different climatic conditions on the two coasts. The paper contributes towards understanding the influence of climatic factors on isotopic variability and towards improving the traceability of the geographical origin of olive oils, using 2H/1H as a more innovative parameter.

View2
  • IRMS
  • Flash 1112
  • Honey Adulteration
  • 13C/12C

13C/12C pattern of honey from Turkey and determination of adulteration in commercially available honey samples using EA-IRMS

Adnan Simsek, Mine Bilsel and Ahmet C. Goren

TÜBITAK UME, National Metrology Institute, Chemistry Group Laboratories, P.O. Box 54, 41470 Gebze-Kocaeli, Turkey

Food Chemistry (2012), V130, pp1115–1121, doi:10.1016/j.foodchem.2011.08.017

Goal: Honey adulteration particularly by adding cheap sugars such as High Fructose Corn Syrup (HFCS) and cane sugar syrup into natural honey is widespread. This study reports (13C/12C,‰) patterns of 31 authentic honey samples obtained from different sources and regions of Turkey as well as 43 commercial honey samples to determine the adulteration using mass spectrometer coupled to elemental analyzer (EAIRMS). The analyses indicated that the ranges of (13C/12C,‰) values of honey and protein fractions of Turkish honey are from 23.30 to 27.58‰ and 24.13 to 26.76‰, respectively. These values for commercial honey samples were determined to range from 11.28 to 25.54‰ and 19.35 to 25.61‰, respectively. The numbers of adulterated commercial honey samples were found to be 10, which corresponds to 23% of the total number of the samples. Diastase activity, HMF content, electrical conductivity and moisture content of honey samples were also determined. Method validation and uncertainty budget calculations were also reported.

View1
  • IRMS
  • Delta XP
  • Flash 1112
  • C, H, N and O isotopes
  • Sourcing Explosives

Sourcing explosives: A multi-isotope approach

David Widory (1), Jean-Jacques Minet (2) and Martine Barbe-Leborgne (2)

1) BRGM, 3 Avenue Claude Guillemin, BP 6009, 45060 Orléans Cedex 2, France, 2) LCPP, 39bis rue de Dantzig, 75015 Paris, France

Science and Justice (2009), V49, p62–72, doi: 10.1016/j.scijus.2008.11.001

Goal: Although explosives are easily identified with current instrumental techniques, it is generally impossible to distinguish between sources of the same substance. To alleviate this difficulty, we present a multistable isotope (δ13C, δ15N, δ18O, δD) approach for appraising the possibility of discriminating explosives. The results from 30 distinct PETN, TNT and ANFO samples show that the different families of explosives are clearly differentiated by both their specific isotope signatures and their combination with corresponding element concentrations. Coupling two or more of the studied isotope systematics yields an even more precise differentiation on the basis of their raw-material origin and/or manufacturing process.

View1
  • IRMS
  • Delta V
  • Flash 1112
  • GC Combustion
  • 13C
  • Oil

Gas chromatography combined with mass spectrometry, flame ionization detection and elemental analyzer/isotope ratio mass spectrometry for characterizing and detecting the authenticity of commercial essential oils of Rosa damascena Mill.

Federica Pellati (1), Giulia Orlandini (1), Katryna A. van Leeuwen (2), Giulia Anesin (1,2), Davide Bertelli (1), Mauro Paolini (2), Stefania Benvenuti (1) and Federica Camin (2)

1) Department of Life Sciences, University of Modena and Reggio Emilia, Via G. Campi 183, 41125 Modena, Italy, 2) Food Quality and Nutrition Department, IASMA Research and Innovation Centre, Fondazione Edmund Mach, Via E. Mach 1, 38010 San Michele all’Adige (TN), Italy

Rapid Communications in Mass Spectrometry (2013), V27, p591–602, doi: 10.1002/rcm.6489

Goal: The essential oil of Rosa damascena Mill. is known for its fine perfumery application, use in cosmetic preparations and for several pharmacological activities. Due to its high value, it can be easily adulterated with flavors or cheaper oils. This study is aimed at a detailed phytochemical characterization of commercial samples of R. damascena essential oil and at their authenticity assessment. Nineteen commercial samples of R. damascena essential oil of different geographic origin and an additional authentic one, directly extracted by hydro-distillation from fresh flowers, were considered. GC/MS and GC/FID techniques were applied for the phytochemical analysis of the samples. EA/IRMS (Elemental Analyzer/Isotope RatioMass Spectrometry) and GC/C (Combustion)/IRMS were used to determine the d13C composition of bulk samples and of some specific components.

View0
  • IRMS
  • Delta Plus
  • TC/EA
  • Deuterium
  • Sulfur

Combining Isotopic and Genetic Markers to Identify Breeding Origins of Migrant Birds

J.F. Kelly (1), K.C. Ruegg (2) and T.B. Smith (3)

1) Oklahoma Biological Survey and Department of Zoology, University of Oklahoma, 111 East Chesapeake St., Norman, Oklahoma 73019 USA, 2) Museum of Vertebrate Zoology, University of California, Berkeley, California 94720-3140 USA, 3) Department of Ecology and Evolutionary Biology and Center for Tropical Research, University of California, Los Angeles, California 90095-1496 USA

Ecological Applications (2005), V15 (5), pp. 1487–1494

Goal: A quantitative method for linking reproductive and nonreproductive phases of migratory life cycles is fundamental to understanding the biology of migratory organisms. Here we combine genetic (mtDNA) and biochemical (stable isotope) information to examine seasonal movements in the Swainson’s Thrush (Catharus ustulatus), a Neotropical migrant. We show that when these intrinsic markers are used in concert, they can predict the sitespecific origin of thrushes with 76–80% accuracy. Genetic and isotope data needed for these classifications can be obtained from migratory organisms at any phase of the life cycle.

View1
  • IRMS
  • 13C and 15N
  • chronology
  • human–elephant conflict

Stable isotopes in elephant hair document migration patterns and diet changes

Thure E. Cerling (1,2), George Wittemyer (3), Henrik B. Rasmussen (4), Fritz Vollrath (4), Claire E. Cerling (2), Todd J. Robinson (2) and Iain Douglas-Hamilton (5)

1) Department of Geology and Geophysics, 135 South 1460 East, University of Utah, Salt Lake City, UT 84112, USA, 2) Department of Biology, 257 South 1400 East, University of Utah, Salt Lake City, UT 84112, USA, 3) University of California, Berkeley, CA 94720, USA, 4) Department of Zoology, Oxford University, Oxford OX1 3PS, United Kingdom, 5) Save The Elephants Foundation, Nairobi, Kenya

Proceedings of the National Academy of Sciences of the USA (2006), V103 (2), pp371–373, doi: 10.1073/pnas.0509606102

Goal: We use chronologies of stable isotopes measured from elephant (Loxodonta africana) hair to determine migration patterns and seasonal diet changes in elephants in and near Samburu National Reserve in northern Kenya. Stable carbon isotopes record diet changes, principally enabling differentiation between browse and tropical grasses, which use the C3 and C4 photosynthetic pathways, respectively; stable nitrogen isotopes record regional patterns related to aridity, offering insight into localized ranging behavior. Isotopically identified range shifts were corroborated by global positioning system radio tracking data of the studied individuals. Comparison of the stable isotope record in the hair of one migrant individual with that of a resident population shows important differences in feeding and ranging behavior over time. Our analysis indicates that differences are the result of excursions into mesic environments coupled with intermittent crop raiding by the migrant individual. Variation in diet, quantified by using stable isotopes, can offer insight into diet-related wildlife behavior.

View1
  • IRMS
  • Delta V Plus
  • Flash 1112
  • C, N and S isotopes
  • Bone Callogen

Establishing collagen quality criteria for sulphur isotope analysis of archaeological bone collagen

Olaf Nehlich (1) and Michael P. Richards (1,2)

1) Department of Human Evolution, Max-Planck Institute for Evolutionary Anthropology, Germany, 2) Department of Archaeology, Durham University, UK

Archaeological and Anthropological Sciences (2009), V1 (59), pp59–75, doi: 10.1007/s12520-009-0003-6

Goal: Sulphur isotope measurements of bone collagen from archaeological sites are beginning to be applied more often, yet there are no clear criteria to assess the quality of the collagen and therefore the validity of the sulphur isotope values. We provide elemental data from different methods (DNA sequences, amino acid sequences and mass spectrometric measurements) which are used to establish a reliable system of quality criteria for sulphur isotope analyses of bone collagen. The difference in the amount of sulphur from fish and mammalian collagen type I led to the suggestion to use different criteria to assess the in vivo character of the collagen between these two categories. For establishing quality ranges, the bone collagen of 140 modern animals were analysed.

View0
  • IRMS
  • Delta XL
  • Deuterium isotopes
  • 34S
  • Bird Feathers

Estimating the latitudinal origins of migratory birds using hydrogen and sulfur stable isotopes in feathers: influence of marine prey base

Casey A. Lott (1,2), Timothy D. Meehan (3) and Julie A. Heath (4)

1) HawkWatch International, 1800 South West Temple Suite 226, Salt Lake City, UT 84115 USA, 2) Audubon of Florida’s Tavernier Science Center, 115 Indian Mound Trail, FL 33070 Tavernier, USA, 3) Department of Biology, University of New Mexico, Castetter Hall, Albuquerque, NM 87131 USA, 4) Department of Wildlife Ecology and Conservation, University of Florida, Gainesville, FL 32611 USA

Oecologia (2003), V134, pp505–510, doi: 10.1007/s00442-002-1153-8

Goal: Hydrogen stable isotope analysis of feathers is an important tool for estimating the natal or breeding latitudes of nearctic-neotropical migratory birds. This method is based on the latitudinal variation of hydrogen stable isotope ratios in precipitation in North America (δDp) and the inheritance of this variation in newly formed feathers (δDf). We hypothesized that the typically strong relationship between δDp and δDf would be decoupled in birds that forage in marine food webs because marine waters have relatively high δD values compared to δD values for local precipitation. Birds that forage on marine prey bases should also have feathers with high δ34S values, since δ34S values for marine sulfate are generally higher than δ34S values in terrestrial systems. To examine this potential marine effect on feather stable isotope ratios, we measured δD and δ34S in the feathers of nine different species of raptors from both inland and coastal locations across North America.

View0
  • IRMS
  • Delta Plus
  • NA 2500
  • 13C and 15N

Towards the trophic structure of the Bouvet Island marine ecosystem

U. Jacob (1), T. Brey (2), I. Fetzer (3), S. Kaehler, K. Mintenbeck (1), K. Dunton (2), K. Beyer (1), U. Struck (4), E.A. Pakhomov (5,6), W.E. Arntz (1)

1) Alfred Wegener Institute for Polar and Marine Research, PO Box 120161, 27515 Bremerhaven, Germany, 2) Marine Science Institute, University of Texas, 750 Channelview Drive Port, Austin, TX 78373-5015, USA, 3) Centre for Environmental Research Leipzig-Halle, Permoserstraße 15, 04318 Leipzig, Germany, 4) GeoBio-Center at Ludwig-Maximilans-Universität, Richard-Wagner-Strasse 10, 80333 München, Germany, 5) Zoology Department, Faculty of Science and Technology, University of Fort Hare, Private Bag X1314, Alice 5700, South Africa, 6) Department of Earth and Ocean Sciences, University of British Columbia, Stores Road, Stores Road, Vancouver, BC, V6T 1Z4, Canada

Polar Biology (2005), V , pp , doi: 10.1007/s00300-005-0071-8

Goal: Although Bouvet Island is of considerable importance for Southern Ocean species conservation, information on the marine community species inventory and trophic functioning is scarce. Our combined study of stable isotopes and feeding relationships shows that (1) the marine system conforms to the trophic pattern described for other Antarctic systems within the Antarctic circumpolar current (ACC); (2) both the benthic and the pelagic subsystem are almost exclusively linked via suspended particulate organic matter (SPOM); and (3) there is no evidence of a subsystem driven by macroalgae. Bouvet Island can therefore be characterized as a benthic ‘‘oasis’’ within a self-sustaining open ocean pelagic system.

View0
  • IRMS
  • Delta V Adv
  • Flash 2000 HT
  • 15N

Determination of the natural abundance δ15N of nortropane alkaloids by gas chromatography–isotope ratio mass spectrometry of their ethylcarbamate esters

Katarzyna Kosieradzka, Illa Tea, Emmanuel Gentil and Richard J. Robins

Elucidation of Biosynthesis by Isotopic Spectrometry Group, Unit for Interdisciplinary Chemistry: Synthesis-Analysis-Modelling (CEISAM), University of Nantes—CNRS UMR6230, 2, rue de la Houssinière, 44322 Nantes, France

Analytical Bioanalytical Chemistry (2010), V396, pp1405–1414, doi: 10.1007/s00216-009-3354-z

Goal: A method is described which allows both the quantification of nortropane alkaloids and the determination of their natural abundance δ15N values. The protocol exploits the derivatisation of the alkaloids by reaction with ethyl chloroformate in aqueous medium and the quantitative extraction of the ensuing ethylcarbamate esters. The improved chromatographic properties of these derivatives gives ample separation of the isomeric nortropine and norpseudotropine for measurement of their δ15N (‰) values by isotope ratio mass spectrometry interfaced to gas chromatography. Adequate separation could not be achieved with the underivatised compounds. Repeatability and precision are sufficient to allow differences in the δ15N values (Δδ15N)>0.8‰ to be measured, with a standard deviation routinely ∼0.3‰. The methodology has been tested by determining the changes in the δ15N values of nortropine and norpseudotropine during degradation by cell suspension cultures of a Pseudomonas strain expressing a specific capacity for tropine catabolism. The precision and reproducibility are shown sufficient to allow the evolution of the δ15N values to be followed during the fermentation.

View0
  • IRMS
  • Delta XP
  • TC/EA
  • 2H and 18O

Validation of deuterium and oxygen18 in urine and saliva samples from children using on-line continuous-flow isotope ratio mass spectrometry

H. Schierbeek (1), R. Rieken (2,3), K. Y. Dorst (1), C. Penning (2), J. B. van Goudoever (1)

1) Erasmus Medical Center – Sophia Children's Hospital, Department of Paediatrics, Division of Neonatology, PO Box 2040, 3000 CA Rotterdam, The Netherlands, 2) Intellectual Disability Medicine, Department of General Practice, Erasmus MC, Rotterdam, The Netherlands, 3) Department of Paediatric Surgery, Erasmus MC – Sophia, Rotterdam, The Netherlands

Rapid Communications in Mass Spectrometry (2009), V23 (22), pp3549–3554, doi: 10.1002/rcm.4279

Goal: The doubly labelled water method is valuable for measuring energy expenditure in humans. It usually involves blood or urine sampling, which might be difficult in neonates and children with cerebral palsy or other disabilities. We therefore aimed to validate a method making use of saliva samples analyzed by automated thermal conversion elemental analyzer in combination with isotope ratio mass spectrometry (TC-EA/IRMS). The subjects received labelled water orally and urine and saliva samples were collected and analyzed. Deuterium as well as oxygen18 was measured in one single run using a peak jump method. Excellent linearity was found for measurement of enrichments of deuterium (R2 = 0.9999) and oxygen18 (R2 = 0.9999).