The definition of pH, its measurement and standard buffers, is well developed in aqueous solutions. Its definition in solvents other than water has been elaborated for a couple of solvents and their mixtures with water. However, the definition of a universal pH scale spanning all solvents and phases, not to mention standard procedures of measurement, is still a largely uncharted territory. UnipHied is a European collaboration and has the goal of putting the theoretical concept of an earlier introduced (2010) unified pHabs scale on a metrologically well-founded basis into practice. The pHabs scale enables the comparability of acidity between different phases. This article draws the connection of the concepts of unified acidity and secondary pH measurement.
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...
Bu makale, lisans düzeyindeki Temel Tasarım dersinin etkililiğine dair öğrenci görüşlerinin belirlenmesini amaçlamaktadır. Araştırma, Aksaray Üniversitesi, Eğitim Fakültesi, Güzel Sanatlar Eğitimi Bölümü, Resim-İş Eğitimi Anabilim Dalı'nda eğitim gören 17 öğrenci üzerinden yürütülmüştür. Veri toplamada 8 soruluk yarı yapılandırılmış görüşme formu kullanılmış, verilerin analizinde NVivo 8 programı tercih edilmiştir. Öğrenci görüşlerinin değerlendirilmesinde ise içerik analizi yapılmış ve elde edilen bulguların frekansları tespit edilmiştir. Araştırma sonucunda lisans düzeyindeki Temel Tasarım dersinin genel olarak etkili olduğu belirlenmiştir.
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