title: Wood cellulose preparation methods and mass spectrometric analyses of delta13C, delta18O, and nonexchangeable delta2H values in cellulose, sugar, and starch: an interlaboratory comparison.
abstract: Interlaboratory comparisons involving nine European stable isotope laboratories have shown that the routine methods of cellulose preparation resulted in data that generally agreed within the precision of the isotope ratio mass spectrometry (IRMS) method used: +/-0.2 per thousand for carbon and +/-0.3 per thousand for oxygen. For carbon, the results suggest that holocellulose is enriched up to 0.39 per thousand in 13C relative to the purified alpha-cellulose. The comparisons of IRMS measurements of carbon on cellulose, sugars, and starches showed low deviations from -0.23 to +0.23 per thousand between laboratories. For oxygen, IRMS measurements varied between means from -0.39 to 0.58 per thousand, -0.89 to 0.42 per thousand, and -1.30 to 1.16 per thousand for celluloses, sugars, and starches, respectively. This can be explained by different effects arising from the use of low- or high-temperature pyrolysis and by the variation between laboratories in the procedures used for drying and storage of samples. The results of analyses of nonexchangeable hydrogen are very similar in means with standard deviations between individual methods from +/-2.7 to +/-4.9 per thousand. The use of a one-point calibration (IAEA-CH7) gave significant positive offsets in delta2H values up to 6 per thousand. Detailed analysis of the results allows us to make the following recommendations in order to increase quality and compatibility of the common data bank: (1) removal of a pretreatment with organic solvents, (2) a purification step with 17% sodium hydroxide solution during cellulose preparation procedure, (3) measurements of oxygen isotopes under an argon hood, (4) use of calibration standard materials, which are of similar nature to that of the measured samples, and (5) using a two-point calibration method for reliable result calculation.
authors.affiliation: Department of Isotope Hydrology, UFZ-Helmholtz Centre for Environmental Research, Theodor-Lieser-Strasse 4, D-06120 Halle, Germany. tatjana.boettger@ufz.de
authors.forename: Tatjana
authors.initials: T
authors.lastname: Boettger
authors.forename: Marika
authors.initials: M
authors.lastname: Haupt
authors.forename: Kay
authors.initials: K
authors.lastname: Knöller
authors.forename: Stephan M
authors.initials: SM
authors.lastname: Weise
authors.forename: John S
authors.initials: JS
authors.lastname: Waterhouse
authors.forename: Katja T
authors.initials: KT
authors.lastname: Rinne
authors.forename: Neil J
authors.initials: NJ
authors.lastname: Loader
authors.forename: Eloni
authors.initials: E
authors.lastname: Sonninen
authors.forename: Hogne
authors.initials: H
authors.lastname: Jungner
authors.forename: Valerie
authors.initials: V
authors.lastname: Masson-Delmotte
authors.forename: Michel
authors.initials: M
authors.lastname: Stievenard
authors.forename: Marie-Thérèse
authors.initials: MT
authors.lastname: Guillemin
authors.forename: Monique
authors.initials: M
authors.lastname: Pierre
authors.forename: Anna
authors.initials: A
authors.lastname: Pazdur
authors.forename: Markus
authors.initials: M
authors.lastname: Leuenberger
authors.forename: Marc
authors.initials: M
authors.lastname: Filot
authors.forename: Matthias
authors.initials: M
authors.lastname: Saurer
authors.forename: Christina E
authors.initials: CE
authors.lastname: Reynolds
authors.forename: Gerd
authors.initials: G
authors.lastname: Helle
authors.forename: Gerhard H
authors.initials: GH
authors.lastname: Schleser
mesh_terms: D002138:Calibration; D002241:Carbohydrates / Q000032:analysis*; D002247:Carbon Isotopes / Q000032:analysis; D002482:Cellulose / Q000032:analysis* / Q000737:chemistry; D003903:Deuterium / Q000032:analysis; D007554:Isotopes / Q000032:analysis*; D013058:Mass Spectrometry / Q000379:methods*; D009930:Organic Chemicals / Q000737:chemistry; D010103:Oxygen Isotopes / Q000032:analysis; D012972:Sodium Hydroxide / Q000737:chemistry; D012997:Solvents / Q000737:chemistry; D013213:Starch / Q000032:analysis*; D013696:Temperature; D014934:Wood
chemical_list: D002241:Carbohydrates; D002247:Carbon Isotopes; D007554:Isotopes; D009930:Organic Chemicals; D010103:Oxygen Isotopes; D012997:Solvents; D012972:Sodium Hydroxide; D002482:Cellulose; D013213:Starch; D003903:Deuterium