Colección INTI-SNRD


Título: CCQM-K55.b (Aldrin) : Final report: october 2012. CCQM-K55.b key comparison on the characterization of organic substances for chemical purity
Fuente: Metrología, 49
Autor/es: Westwood, Steven; Josephs, Ralf; Choteau, Tiphaine; Daireaux, Adeline; Mesquida, Charline; Wielgosz, Robert; Rosso, Adriana; Ruiz de Arechavaleta, Mariana; Davies, Stephen; Wang, Hongjie; Cristina Pires do Rego, Eliane; Marques Rodrigues, Janaína; de Freitas Guimarães, Evelyn; Barreto Sousa, Marcus Vinicius; Monteiro, Tânia Maria; Alves das Neves Valente, Laura; Marques Violante, Fernando Gustavo; Rubim, Renato; Almeida, Ribeiro; Baptista Quaresma, Maria Cristina; Nogueira, Raquel; Windust, Anthony; Dai, Xinhua; Li, Xiaomin; Zhang, Wei; Li, Ming; Shao, Mingwu; Wei, Chao; Wong, Siu-kay; Cabillic, Julie; Gantois, Fanny; Philipp, Rosemarie; Pfeifer, Dietmar; Hein, Sebastian; Klyk-Seitz, Urszula-Anna; Ishikawa, Keiichiro; Castro, Esther; Gonzalez, Norma; Krylov, Anatoly; Lin, Teo Tang; Kooi, Lee Tong; Fernandes-Whaley, M.; Prévoo, D.; Archer, M.; Visser, R.; Nlhapo, N.; de Vos, B.; Ahn, Seonghee; Pookrod, Preeyaporn; Wiangnon, Kanjana; Sudsiri, Nittaya; Muaksang, Kittiya; Cherdchu, Chainarong; Gören, Ahmet Ceyhan; Bilsel, Mine; LeGoff, Thierry; Bearden, Dan; Bedner, Mary; Duewer, David; Hancock, Diane; Lang, Brian; Lippa, Katrice; Schantz, Michele; Sieber, John
Materias: Metrología; Determinación de materia orgánica; Sustancias orgánicas; Incertidumbre; Calibración; Calibradores; Mediciones
Editor/Edición: IOP Publishing; 2012
Licencia: https://creativecommons.org/licenses/by/3.0/
Afiliaciones: Westwood, Steven. Bureau International des Poids et Mesures (BIPM); Francia
Josephs, Ralf. Bureau International des Poids et Mesures (BIPM); Francia
Choteau, Tiphaine. Bureau International des Poids et Mesures (BIPM); Francia
Daireaux, Adeline. Bureau International des Poids et Mesures (BIPM); Francia
Mesquida, Charline. Bureau International des Poids et Mesures (BIPM); Francia
Wielgosz, Robert. Bureau International des Poids et Mesures (BIPM); Francia
Rosso, Adriana. Instituto Nacional de Tecnología Industrial (INTI); Argentina
Ruiz de Arechavaleta, Mariana. Instituto Nacional de Tecnología Industrial (INTI); Argentina
Davies, Stephen. National Measurement Institute (NMIA); Australia
Wang, Hongjie. National Measurement Institute (NMIA); Australia
Pires do Rego, Eliane Cristina. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil
Marques Rodrigues, Janaína. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil
de Freitas Guimarães, Evelyn. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil
Barreto Sousa, Marcus Vinicius. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil
Monteiro, Tânia Maria. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil
Alves das Neves Valente, Laura. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil
Marques Violante, Fernando Gustavo. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil
Rubim, Renato. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil
Almeida, Ribeiro. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil
Baptista Quaresma, Maria Cristina. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil
Nogueira, Raquel. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil
Windust, Anthony. Institute for National Measurement Standards. National Research Council Canada (NRC-INMS); Canadá
Dai, Xinhua. National Institute of Metrology (NIM); China
Li, Xiaomin. National Institute of Metrology (NIM); China
Zhang, Wei. National Institute of Metrology (NIM); China
Li, Ming. National Institute of Metrology (NIM); China
Shao, Mingwu. National Institute of Metrology (NIM); China
Wei, Chao. National Institute of Metrology (NIM); China
Wong, Siu-kay. Government Laboratory of Hong Kong SAR (GLHK); China
Cabillic, Julie. Laboratoire National de Métrologie et d’Essais (LNE); Francia
Gantois, Fanny. Laboratoire National de Métrologie et d’Essais (LNE); Francia
Philipp, Rosemarie. Bundesanstalt für Materialforschung (BAM); Alemania
Pfeifer, Dietmar. Bundesanstalt für Materialforschung (BAM); Alemania
Hein, Sebastian. Bundesanstalt für Materialforschung (BAM); Alemania
Klyk-Seitz, Urszula-Anna. Bundesanstalt für Materialforschung (BAM); Alemania
Ishikawa, Keiichiro. National Metrology Institute of Japan (NMIJ); Japón
Castro, Esther. Centro Nacional de Metrología (CENAM); México
Gonzalez, Norma. Centro Nacional de Metrología (CENAM); México
Krylov, Anatoly. D. I. Mendeleev Institute for Metrology (VNIIM); Rusia
Lin, Teo Tang. Health Sciences Authority (HSA); Singapur
Kooi, Lee Tong. Health Sciences Authority (HSA); Singapur
Fernandes-Whaley, M. National Metrology Institute of South Africa (NMISA); Sudáfrica
Prévoo, D. National Metrology Institute of South Africa (NMISA); Sudáfrica
Archer, M. National Metrology Institute of South Africa (NMISA); Sudáfrica
Visser, R. National Metrology Institute of South Africa (NMISA); Sudáfrica
Nlhapo, N. National Metrology Institute of South Africa (NMISA); Sudáfrica
de Vos, B. National Metrology Institute of South Africa (NMISA); Sudáfrica
Ahn, Seonghee. Korea Research Institute of Standards and Science (KRISS); Corea del Sur
Pookrod, Preeyaporn. National Institute of Metrology of Thailand (NIMT); Tailandia
Wiangnon, Kanjana. National Institute of Metrology of Thailand (NIMT); Tailandia
Sudsiri, Nittaya. National Institute of Metrology of Thailand (NIMT); Tailandia
Muaksang, Kittiya. National Institute of Metrology of Thailand (NIMT); Tailandia
Cherdchu, Chainarong. National Institute of Metrology of Thailand (NIMT); Tailandia
Gören, Ahmet Ceyhan. National Metrology Institute (TUBITAK UME); Turquía
Bilsel, Mine. National Metrology Institute (TUBITAK UME); Turquía
LeGoff, Thierry. LGC Limited; Reino Unido
Bearden, Dan. National Institute of Standards and Technology (NIST); Estados Unidos
Bedner, Mary. National Institute of Standards and Technology (NIST); Estados Unidos
Duewer, David. National Institute of Standards and Technology (NIST); Estados Unidos
Hancock, Diane. National Institute of Standards and Technology (NIST); Estados Unidos
Lang, Brian. National Institute of Standards and Technology (NIST); Estados Unidos
Lippa, Katrice. National Institute of Standards and Technology (NIST); Estados Unidos
Schantz, Michele. National Institute of Standards and Technology (NIST); Estados Unidos
Sieber, John. National Institute of Standards and Technology (NIST); Estados Unidos

Resumen: 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.b, was coordinated by the Bureau International des Poids et Mesures (BIPM) in 2010/2011. Nineteen national measurement institutes and the BIPM participated. Participants were required to assign the mass fraction of aldrin present as the main component in the comparison sample for CCQM-K55.b which consisted of technical grade aldrin obtained from the National Measurement Institute Australia that had been subject to serial recrystallization and drying prior to sub-division into the units supplied for the comparison. Aldrin was selected to be representative of the performance of a laboratory's measurement capability for the purity assignment of organic compounds of medium structural complexity [molar mass range 300 Da to 500 Da] and low polarity (pKOW < −2) for which related structure impurities can be quantified by capillary gas phase chromatography (GC). The key comparison reference value (KCRV) for the aldrin content of the material was 950.8 mg/g with a combined standard uncertainty of 0.85 mg/g. The KCRV was assigned by combination of KCRVs assigned by consensus from participant results for each orthogonal impurity class. The relative expanded uncertainties reported by laboratories having results consistent with the KCRV ranged from 0.3% to 0.6% using a mass balance approach and 0.5% to 1% using a qNMR method. The major analytical challenge posed by the material proved to be the detection and quantification of a significant amount of oligomeric organic material within the sample and most participants relying on a mass balance approach displayed a positive bias relative to the KCRV (overestimation of aldrin content) in excess of 10 mg/g due to not having adequate procedures in place to detect and quantify the non-volatile content—specifically the non-volatile organics content—of the comparison sample. There was in general excellent agreement between participants in the identification and the quantification of the total and individual related structure impurities, water content and the residual solvent content of the sample. The comparison demonstrated the utility of 1H NMR as an independent method for quantitative analysis of high purity compounds. In discussion of the participant results it was noted that while several had access to qNMR estimates for the aldrin content that were inconsistent with their mass balance determination they decided to accept the mass balance result and assumed a hidden bias in their NMR data. By contrast, laboratories that placed greater confidence in their qNMR result were able to resolve the discrepancy through additional studies that provided evidence of the presence of non-volatile organic impurity at the requisite level to bring their mass balance and qNMR estimates into agreement.
Descargar
Ver+/-