Electrochemical lithium insertion into polyacryionitrile (PAN)-based disordered carbons was studied using the techniques of discharge/charge tests, cyclic voltammetry, and 7Li nuclear magnetic resonance (NMR) spectroscopy. The PANbased carbons were prepared by vacuum pyrolysis of PAN at 500, 800, and 1000'C. They showed charge capacities between 254 and 380 mAh/g in the first cycle. Li NMR spectra showed two kinds of lithium insertion sites in the PANbased carbons: a reversible site where lithium is removed in the subsequent charge process and an irreversible site where lithium remains intact. The NMR results suggest that lithium in fully Li-inserted PAN-based carbons has an ionic character, and reversible site lithium resides between negatively charged carbon layers.
Isotope dilution liquid chromatography/tandem mass spectrometry (ID-LC/MS/MS) has been developed as a candidate reference method to determine the level of phenylalanine in human serum. The advantages of this method include a simple sample preparation without derivatization, selective detection of analytes, and the use of an isotopic analogue as an internal standard. Phenylalanine and its isotopic analogue, phenylalanine-ring-(13)C(6), were monitored at the transitions m/z 166.2/120.2 and 172.2/126.2 in the multiple-reaction monitoring (MRM) mode, respectively. The expanded uncertainty of the measurement result of phenylalanine in the serum was approximately 1.2% within a 95% confidence level. A standard reference material, with a certified value of phenylalanine, was analyzed in order to verify this method. The result obtained by the ID-LC/MS/MS method differed somewhat from the certified value, but agreed well with the gravimetric value. The measurement result of phenylalanine in serum by ID-LC/MS/MS was compared with the results from the commercial HPLC method, which was carried out in clinics. The results from the commercial HPLC method showed inconsistent results with each other. The busted results from the commercial HPLC method suggest that it should be possible to trace the results of the commercial fields to well-characterized reference materials or methods.
Under the auspices of the Organic Analysis Working Group (OAWG) of the Comité Consultatif pour la Quantité de Matière (CCQM) a key comparison, CCQM K55.c, was coordinated by the Bureau International des Poids et Mesures (BIPM) in 2012. Twenty National Measurement Institutes or Designated Institutes and the BIPM participated. Participants were required to assign the mass fraction of valine present as the main component in the comparison sample for CCQM-K55.c. The comparison samples were prepared from analytical grade L-valine purchased from a commercial supplier and used as provided without further treatment or purification.Valine was selected to be representative of the performance of a laboratory's measurement capability for the purity assignment of organic compounds of low structural complexity [molecular weight range 100–300] and high polarity (pKOW > −2).The KCRV for the valine content of the material was 992.0 mg/g with a combined standard uncertainty of 0.3 mg/g. The key comparison reference value (KCRV) was assigned by combination of KCRVs assigned from participant results for each orthogonal impurity class. The relative expanded uncertainties reported by laboratories having results consistent with the KCRV ranged from 1 mg/g to 6 mg/g when using mass balance based approaches alone, 2 mg/g to 7 mg/g using quantitative 1H NMR (qNMR) based approaches and from 1 mg/g to 2.5 mg/g when a result obtained by a mass balance method was combined with a separate qNMR result.The material provided several analytical challenges. In addition to the need to identify and quantify various related amino acid impurities including leucine, isoleucine, alanine and α-amino butyrate, care was required to select appropriate conditions for performing Karl Fischer titration assay for water content to avoid bias due to in situ formation of water by self-condensation under the assay conditions. It also proved to be a challenging compound for purity assignment by qNMR techniques.There was overall excellent agreement between participants in the identification and the quantification of the total and individual related structure impurities, water content, residual solvent and total non-volatile content of the sample. Appropriate technical justifications were developed to rationalise observed discrepancies in the limited cases where methodology differences led to inconsistent results.The comparison demonstrated that to perform a qNMR purity assignment the selection of appropriate parameters and an understanding of their potential influence on the assigned value is critical for reliable implementation of the method, particularly when one or more of the peaks to be quantified consist of complex multiplet signals.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 the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIP...
Progesterone is one of the steroid hormones. The hormone is especially important in preparing the uterus for the implantation of the blastocyst and in maintaining pregnancy. Its concentration in serum is measured to determine ovarian function and to predict early pregnancy. The progesterone concentration is also important for in-vitro fertilization and embryo-transfer outcomes. We have established isotope dilution liquid chromatography-tandem mass spectrometry as a primary method for the measurement of progesterone in human serum. Progesterone and its isotopic analogue, progesterone-(13)C(2), in serum were monitored at mass transitions of m/z 315.2/109.2 and 317.2/111.2 respectively in multiple-reaction monitoring (MRM) mode with electrospray positive ionization. For validation of the method, progesterone in a National Institute of Standards and Technology standard reference material (NIST SRM) was measured, and the measured results were in good agreement with the reference values within the uncertainty. On the basis of the established method, progesterone certified reference material (CRM) was developed in this work. The certified value was (1.41 ± 0.036) μg kg(-1). The repeatability of 1.1% and reproducibility of 0.14% showed that ID LC-MS-MS is a reliable and reproducible method. The expanded uncertainty for the measurement of progesterone in the CRM was approximately 2.6% within 95% confidence limits. The detection limit of progesterone was approximately 0.6 μg kg(-1). The progesterone CRMs were distributed to representative clinical laboratories in the Republic of Korea for comparison with the chemiluminescence immunoassay (CLIA), which is the most sensitive immunoassay method. The results from the comparison showed quite a large bias among the participating laboratories. This implies that the CRM is a very important material for establishment of traceability to its practical use.
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