A systematic comparison between the up-front Collision induced dissociation (CID) mass spectra and low-energy CID tandem mass spectra from twenty-one singly and/or doubly charged peptides has been made. CID spectra of the peptides were recorded at different electrode voltages in the up-front source region of a single quadrupole instrument and different collision energies in the collision cell of a tandem quadrupole instrument. It was observed that up-front CID and low-energy CID yielded comparable product ion spectra from protonated peptides, and that the instrumental settings necessary for obtaining comparable CID mass spectra from the two methods are correlated.
Main text The key comparison CCQM-K68.2019 was aimed at evaluating the level of comparability of laboratories' capabilities for preparing nitrous oxide in air primary reference mixtures at ambient amount fractions, in the range 320 nmol mol−1 to 350 nmol mol−1. The comparison was coordinated by the BIPM and the KRISS. It consisted in the simultaneous comparison of a suite of 2n primary gas standards, two standards to be prepared by each of the n participating laboratories. Two independent analytical methods were used by the BIPM to analyse the amount fraction of N2O in air, namely Gas Chromatography with an Electron Capture Detector (GC−ECD) and Quantum Cascade Laser Absorption Spectroscopy (QCLAS). Since the circulation of the Draft A report in April 2021, four meetings took place with participants to discuss the mathematical treatment of the comparisons results, and several models were proposed. The model chosen by participants is the Bayesian Errors−In−Variables regression with shades of dark uncertainty. In this final report, the Key Comparison Reference Values were obtained with this model, with calculations performed by B Toman and A Possolo. The key comparison CCQM-K68.2019 is considered to present an analytical challenge and therefore classified as Track C comparison in the CCQM nomenclature. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database https://www.bipm.org/kcdb/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).
The capabilities for the preparation of certified reference materials of carbon monoxide, carbon dioxide, and propane in nitrogen have been compared. The participating national metrology institutes each submitted a gravimetrically prepared gas mixture of a specified target composition typical for the automotive industry to the coordinating laboratory. All mixtures were analyzed by the coordinating laboratory using a gas chromatograph equipped with a thermal conductivity detector in three runs under repeatable conditions. Based on the calibration curve, reference values were assigned to the amount fractions of carbon monoxide, carbon dioxide, and propane. The degrees of equivalence were established as the difference between the gas composition as calculated from preparation and the measured one, and its associated uncertainty. All participants obtained satisfactory results.Main text. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/.The final report has been peer-reviewed and approved for publication by EURAMET, according to the provisions of the CIPM Mutual Recognition Arrangement (MRA).
This supplementary comparison (EURAMET.QM-S8) concerns the purity analysis of nitrogen as used in reference gas mixture preparation. This project was carried out without adding impurities to the gas used for this comparison, and is therefore more representative to evaluate the analysis of carbon monoxide, carbon dioxide, methane, oxygen, argon and water impurities in high-purity nitrogen. The analysis of the amount-of-substance fraction water was optional.Two 50 litre high purity nitrogen cylinders were purchased from a well-qualified supplier of specialty gases. The listed components were expected to be present in the pure nitrogen at the target levels as a result of the purification of the nitrogen. From the start of this comparison it was clear that the comparison may not lead to reference values for the constituents analysed.The results indicate that analyses of high purity gases are often limited by the limits of detection of analytical equipment used. The reports of the participating laboratories also indicate that there is no agreed method of determination of the uncertainty on a detection limit value. The results provide useful information on the performance of participants. For all analysed components there is reasonable agreement in results for LNE, VSL, METAS and NPL. For BAM only the argon result is in agreement.Main text. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/.The final report has been peer-reviewed and approved for publication by EURAMET, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).
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