Wood cellulose preparation methods and mass spectrometric analyses of δ¹³C, δ¹⁸O, and nonexchangeable δ²H values in cellulose, sugar, and starch: An interlaboratory comparison

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‰ for carbon and ±0.3‰ for oxygen. For carbon, the results suggest that holocellulose is enriched up to 0.39‰ in ¹³C relative to the purified α-cellulose. The comparisons of IRMS measurements of carbon on cellulose, sugars, and starches showed low deviations from -0.23 to +0.23‰ between laboratories. For oxygen, IRMS measurements varied between means from -0.39 to 0.58‰, -0.89 to 0.42‰, and -1.30 to 1.16‰ 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‰. The use of a one-point calibration (IAEA-CH7) gave significant positive offsets in δ²H values up to 6‰. 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.