CCQM-K55.b (Aldrin) : Final report: october 2012. CCQM-K55.b key comparison on the characterization of organic substances for chemical purity
- Autores
- Westwood, S.; Josephs, R.; Choteau, T.; Daireaux, A.; Mesquida, C.; Wielgosz, R.; Rosso, A.; Ruiz de Arechavaleta, M.; Davies, S.; Wang, Hongjie; Cristina Pires do Rego, E.; Marques Rodrigues, J.; Freitas Guimarães, E. de.; Barreto Sousa, M. V.; Monteiro, T. M.; Alves das Neves Valente, L.; Marques Violante, F. G.; Rubim, R.; Almeida, R.; Baptista Quaresma, M. C.; Nogueira, R.; Windust, A.; Dai, X.; Li, X.; Zhang, W.; Li, M.; Shao, M.; Wei, C.; Wong, S.; Cabillic, J.; Gantois, F.; Philipp, R.; Pfeifer, D.; Hein, S.; Klyk-Seitz, U.; Ishikawa, K.; Castro, E.; Gonzalez, N.; Krylov, A.; Lin, T. T.; Kooi, L. T.; Fernandes-Whaley, M.; Prévoo, D.; Archer, M.; Visser, R.; Nlhapo, N.; de Vos, B.; Ahn, S.; Pookrod, P.; Wiangnon, K.; Sudsiri, N.; Muaksang, K.; Cherdchu, C.; Gören, A. C.; Bilsel, M.; LeGoff, T.; Bearden, D.; Bedner, M.; Duewer, D.; Hancock, D.; Lang, B.; Lippa, K.; Schantz, M.; Sieber, J.
- Año de publicación
- 2012
- Idioma
- inglés
- Tipo de recurso
- artículo
- Estado
- versión publicada
- Descripción
- 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.
Fil: Westwood, S. Bureau International des Poids et Mesures (BIPM); Francia
Fil: Josephs, R. Bureau International des Poids et Mesures (BIPM); Francia
Fil: Choteau, T. Bureau International des Poids et Mesures (BIPM); Francia
Fil: Daireaux, A. Bureau International des Poids et Mesures (BIPM); Francia
Fil: Mesquida, C. Bureau International des Poids et Mesures (BIPM); Francia
Fil: Wielgosz, R. Bureau International des Poids et Mesures (BIPM); Francia
Fil: Rosso, A. Instituto Nacional de Tecnología Industrial (INTI); Argentina
Fil: Ruiz de Arechavaleta, M. Instituto Nacional de Tecnología Industrial (INTI); Argentina
Fil: Davies, S. National Measurement Institute (NMIA); Australia
Fil: Wang, H. National Measurement Institute (NMIA); Australia
Fil: Pires do Rego, E. C. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil
Fil: Marques Rodrigues, J. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil
Fil: Freitas Guimarães, E. de. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil
Fil: Barreto Sousa, M. V. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil
Fil: Monteiro, T. M. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil
Fil: Alves das Neves Valente, L. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil
Fil: Marques Violante, F. G. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil
Fil: Rubim, R. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil
Fil: Almeida, R. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil
Fil: Baptista Quaresma, M. C. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil
Fil: Nogueira, R. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil
Fil: Windust, A. Institute for National Measurement Standards. National Research Council Canada (NRC-INMS); Canadá
Fil: Dai, X. National Institute of Metrology (NIM); China
Fil: Li, X. National Institute of Metrology (NIM); China
Fil: Zhang, W. National Institute of Metrology (NIM); China
Fil: Li, M. National Institute of Metrology (NIM); China
Fil: Shao, M. National Institute of Metrology (NIM); China
Fil: Wei, C. National Institute of Metrology (NIM); China
Fil: Wong, S. Government Laboratory of Hong Kong SAR (GLHK); China
Fil: Cabillic, J. Laboratoire National de Métrologie et d’Essais (LNE); Francia
Fil: Gantois, F. Laboratoire National de Métrologie et d’Essais (LNE); Francia
Fil: Philipp, R. Bundesanstalt für Materialforschung (BAM); Alemania
Fil: Pfeifer, D. Bundesanstalt für Materialforschung (BAM); Alemania
Fil: Hein, S. Bundesanstalt für Materialforschung (BAM); Alemania
Fil: Klyk-Seitz, U. Bundesanstalt für Materialforschung (BAM); Alemania
Fil: Ishikawa, K. National Metrology Institute of Japan (NMIJ); Japón
Fil: Castro, E. Centro Nacional de Metrología (CENAM); México
Fil: Gonzalez, N. Centro Nacional de Metrología (CENAM); México
Fil: Krylov, A. D. I. Mendeleev Institute for Metrology (VNIIM); Rusia
Fil: Lin, T. T. Health Sciences Authority (HSA); Singapur
Fil: Kooi, L. T. Health Sciences Authority (HSA); Singapur
Fil: Fernandes-Whaley, M. National Metrology Institute of South Africa (NMISA); Sudáfrica
Fil: Prévoo, D. National Metrology Institute of South Africa (NMISA); Sudáfrica
Fil: Archer, M. National Metrology Institute of South Africa (NMISA); Sudáfrica
Fil: Visser, R. National Metrology Institute of South Africa (NMISA); Sudáfrica
Fil: Nlhapo, N. National Metrology Institute of South Africa (NMISA); Sudáfrica
Fil: de Vos, B. National Metrology Institute of South Africa (NMISA); Sudáfrica
Fil: Ahn, S. Korea Research Institute of Standards and Science (KRISS); Corea del Sur
Fil: Pookrod, P. National Institute of Metrology of Thailand (NIMT); Tailandia
Fil: Wiangnon, K. National Institute of Metrology of Thailand (NIMT); Tailandia
Fil: Sudsiri, N. National Institute of Metrology of Thailand (NIMT); Tailandia
Fil: Muaksang, K. National Institute of Metrology of Thailand (NIMT); Tailandia
Fil: Cherdchu, C. National Institute of Metrology of Thailand (NIMT); Tailandia
Fil: Gören, A. C. National Metrology Institute (TUBITAK UME); Turquía
Fil: Bilsel, M. National Metrology Institute (TUBITAK UME); Turquía
Fil: LeGoff, T. LGC Limited; Reino Unido
Fil: Bearden, D. National Institute of Standards and Technology (NIST); Estados Unidos
Fil: Bedner, M. National Institute of Standards and Technology (NIST); Estados Unidos
Fil: Duewer, D. National Institute of Standards and Technology (NIST); Estados Unidos
Fil: Hancock, D. National Institute of Standards and Technology (NIST); Estados Unidos
Fil: Lang, B. National Institute of Standards and Technology (NIST); Estados Unidos
Fil: Lippa, K. National Institute of Standards and Technology (NIST); Estados Unidos
Fil: Schantz, M. National Institute of Standards and Technology (NIST); Estados Unidos
Fil: Sieber, J. National Institute of Standards and Technology (NIST); Estados Unidos - Fuente
- Metrología, 49
- Materia
-
Metrología
Determinación de materia orgánica
Sustancias orgánicas
Incertidumbre
Calibración
Calibradores
Mediciones - Nivel de accesibilidad
- acceso abierto
- Condiciones de uso
- https://creativecommons.org/licenses/by/3.0/
- Repositorio
.jpg)
- Institución
- Instituto Nacional de Tecnología Industrial
- OAI Identificador
- nuevadc:Rosso2012CCQM_pdf
Ver los metadatos del registro completo
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nuevadc:Rosso2012CCQM_pdf |
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Repositorio Institucional del Instituto Nacional de Tecnología Industrial (INTI) |
| spelling |
CCQM-K55.b (Aldrin) : Final report: october 2012. CCQM-K55.b key comparison on the characterization of organic substances for chemical purityWestwood, S.Josephs, R.Choteau, T.Daireaux, A.Mesquida, C.Wielgosz, R.Rosso, A.Ruiz de Arechavaleta, M.Davies, S.Wang, HongjieCristina Pires do Rego, E.Marques Rodrigues, J.Freitas Guimarães, E. de.Barreto Sousa, M. V.Monteiro, T. M.Alves das Neves Valente, L.Marques Violante, F. G.Rubim, R.Almeida, R.Baptista Quaresma, M. C.Nogueira, R.Windust, A.Dai, X.Li, X.Zhang, W.Li, M.Shao, M.Wei, C.Wong, S.Cabillic, J.Gantois, F.Philipp, R.Pfeifer, D.Hein, S.Klyk-Seitz, U.Ishikawa, K.Castro, E.Gonzalez, N.Krylov, A.Lin, T. T.Kooi, L. T.Fernandes-Whaley, M.Prévoo, D.Archer, M.Visser, R.Nlhapo, N.de Vos, B.Ahn, S.Pookrod, P.Wiangnon, K.Sudsiri, N.Muaksang, K.Cherdchu, C.Gören, A. C.Bilsel, M.LeGoff, T.Bearden, D.Bedner, M.Duewer, D.Hancock, D.Lang, B.Lippa, K.Schantz, M.Sieber, J.MetrologíaDeterminación de materia orgánicaSustancias orgánicasIncertidumbreCalibraciónCalibradoresMedicionesUnder 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.Fil: Westwood, S. Bureau International des Poids et Mesures (BIPM); FranciaFil: Josephs, R. Bureau International des Poids et Mesures (BIPM); FranciaFil: Choteau, T. Bureau International des Poids et Mesures (BIPM); FranciaFil: Daireaux, A. Bureau International des Poids et Mesures (BIPM); FranciaFil: Mesquida, C. Bureau International des Poids et Mesures (BIPM); FranciaFil: Wielgosz, R. Bureau International des Poids et Mesures (BIPM); FranciaFil: Rosso, A. Instituto Nacional de Tecnología Industrial (INTI); ArgentinaFil: Ruiz de Arechavaleta, M. Instituto Nacional de Tecnología Industrial (INTI); ArgentinaFil: Davies, S. National Measurement Institute (NMIA); AustraliaFil: Wang, H. National Measurement Institute (NMIA); AustraliaFil: Pires do Rego, E. C. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); BrasilFil: Marques Rodrigues, J. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); BrasilFil: Freitas Guimarães, E. de. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); BrasilFil: Barreto Sousa, M. V. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); BrasilFil: Monteiro, T. M. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); BrasilFil: Alves das Neves Valente, L. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); BrasilFil: Marques Violante, F. G. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); BrasilFil: Rubim, R. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); BrasilFil: Almeida, R. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); BrasilFil: Baptista Quaresma, M. C. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); BrasilFil: Nogueira, R. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); BrasilFil: Windust, A. Institute for National Measurement Standards. National Research Council Canada (NRC-INMS); CanadáFil: Dai, X. National Institute of Metrology (NIM); ChinaFil: Li, X. National Institute of Metrology (NIM); ChinaFil: Zhang, W. National Institute of Metrology (NIM); ChinaFil: Li, M. National Institute of Metrology (NIM); ChinaFil: Shao, M. National Institute of Metrology (NIM); ChinaFil: Wei, C. National Institute of Metrology (NIM); ChinaFil: Wong, S. Government Laboratory of Hong Kong SAR (GLHK); ChinaFil: Cabillic, J. Laboratoire National de Métrologie et d’Essais (LNE); FranciaFil: Gantois, F. Laboratoire National de Métrologie et d’Essais (LNE); FranciaFil: Philipp, R. Bundesanstalt für Materialforschung (BAM); AlemaniaFil: Pfeifer, D. Bundesanstalt für Materialforschung (BAM); AlemaniaFil: Hein, S. Bundesanstalt für Materialforschung (BAM); AlemaniaFil: Klyk-Seitz, U. Bundesanstalt für Materialforschung (BAM); AlemaniaFil: Ishikawa, K. National Metrology Institute of Japan (NMIJ); JapónFil: Castro, E. Centro Nacional de Metrología (CENAM); MéxicoFil: Gonzalez, N. Centro Nacional de Metrología (CENAM); MéxicoFil: Krylov, A. D. I. Mendeleev Institute for Metrology (VNIIM); RusiaFil: Lin, T. T. Health Sciences Authority (HSA); SingapurFil: Kooi, L. T. Health Sciences Authority (HSA); SingapurFil: Fernandes-Whaley, M. National Metrology Institute of South Africa (NMISA); SudáfricaFil: Prévoo, D. National Metrology Institute of South Africa (NMISA); SudáfricaFil: Archer, M. National Metrology Institute of South Africa (NMISA); SudáfricaFil: Visser, R. National Metrology Institute of South Africa (NMISA); SudáfricaFil: Nlhapo, N. National Metrology Institute of South Africa (NMISA); SudáfricaFil: de Vos, B. National Metrology Institute of South Africa (NMISA); SudáfricaFil: Ahn, S. Korea Research Institute of Standards and Science (KRISS); Corea del SurFil: Pookrod, P. National Institute of Metrology of Thailand (NIMT); TailandiaFil: Wiangnon, K. National Institute of Metrology of Thailand (NIMT); TailandiaFil: Sudsiri, N. National Institute of Metrology of Thailand (NIMT); TailandiaFil: Muaksang, K. National Institute of Metrology of Thailand (NIMT); TailandiaFil: Cherdchu, C. National Institute of Metrology of Thailand (NIMT); TailandiaFil: Gören, A. C. National Metrology Institute (TUBITAK UME); TurquíaFil: Bilsel, M. National Metrology Institute (TUBITAK UME); TurquíaFil: LeGoff, T. LGC Limited; Reino UnidoFil: Bearden, D. National Institute of Standards and Technology (NIST); Estados UnidosFil: Bedner, M. National Institute of Standards and Technology (NIST); Estados UnidosFil: Duewer, D. National Institute of Standards and Technology (NIST); Estados UnidosFil: Hancock, D. National Institute of Standards and Technology (NIST); Estados UnidosFil: Lang, B. National Institute of Standards and Technology (NIST); Estados UnidosFil: Lippa, K. National Institute of Standards and Technology (NIST); Estados UnidosFil: Schantz, M. National Institute of Standards and Technology (NIST); Estados UnidosFil: Sieber, J. National Institute of Standards and Technology (NIST); Estados UnidosIOP Publishing2012info:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersionhttp://purl.org/coar/resource_type/c_6501info:ar-repo/semantics/articuloapplication/pdfRosso2012CCQM.pdfhttps://app.inti.gob.ar/greenstone3/sites/localsite/collect/nuevadc/index/assoc/Rosso201.dir/doc.pdfMetrología, 49reponame:Repositorio Institucional del Instituto Nacional de Tecnología Industrial (INTI)instname:Instituto Nacional de Tecnología Industrialenginfo:eu-repo/semantics/openAccesshttps://creativecommons.org/licenses/by/3.0/openAccess2025-10-16T10:46:42Znuevadc:Rosso2012CCQM_pdfinstacron:INTIInstitucionalhttps://app.inti.gob.ar/greenstone3/biblioOrganismo científico-tecnológicohttps://argentina.gob.ar/intihttps://app.inti.gob.ar/greenstone3/oaiserver?verb=Identifypfalcato@inti.gob.arArgentinaopendoar:2025-10-16 10:46:42.753Repositorio Institucional del Instituto Nacional de Tecnología Industrial (INTI) - Instituto Nacional de Tecnología Industrialfalse |
| dc.title.none.fl_str_mv |
CCQM-K55.b (Aldrin) : Final report: october 2012. CCQM-K55.b key comparison on the characterization of organic substances for chemical purity |
| title |
CCQM-K55.b (Aldrin) : Final report: october 2012. CCQM-K55.b key comparison on the characterization of organic substances for chemical purity |
| spellingShingle |
CCQM-K55.b (Aldrin) : Final report: october 2012. CCQM-K55.b key comparison on the characterization of organic substances for chemical purity Westwood, S. Metrología Determinación de materia orgánica Sustancias orgánicas Incertidumbre Calibración Calibradores Mediciones |
| title_short |
CCQM-K55.b (Aldrin) : Final report: october 2012. CCQM-K55.b key comparison on the characterization of organic substances for chemical purity |
| title_full |
CCQM-K55.b (Aldrin) : Final report: october 2012. CCQM-K55.b key comparison on the characterization of organic substances for chemical purity |
| title_fullStr |
CCQM-K55.b (Aldrin) : Final report: october 2012. CCQM-K55.b key comparison on the characterization of organic substances for chemical purity |
| title_full_unstemmed |
CCQM-K55.b (Aldrin) : Final report: october 2012. CCQM-K55.b key comparison on the characterization of organic substances for chemical purity |
| title_sort |
CCQM-K55.b (Aldrin) : Final report: october 2012. CCQM-K55.b key comparison on the characterization of organic substances for chemical purity |
| dc.creator.none.fl_str_mv |
Westwood, S. Josephs, R. Choteau, T. Daireaux, A. Mesquida, C. Wielgosz, R. Rosso, A. Ruiz de Arechavaleta, M. Davies, S. Wang, Hongjie Cristina Pires do Rego, E. Marques Rodrigues, J. Freitas Guimarães, E. de. Barreto Sousa, M. V. Monteiro, T. M. Alves das Neves Valente, L. Marques Violante, F. G. Rubim, R. Almeida, R. Baptista Quaresma, M. C. Nogueira, R. Windust, A. Dai, X. Li, X. Zhang, W. Li, M. Shao, M. Wei, C. Wong, S. Cabillic, J. Gantois, F. Philipp, R. Pfeifer, D. Hein, S. Klyk-Seitz, U. Ishikawa, K. Castro, E. Gonzalez, N. Krylov, A. Lin, T. T. Kooi, L. T. Fernandes-Whaley, M. Prévoo, D. Archer, M. Visser, R. Nlhapo, N. de Vos, B. Ahn, S. Pookrod, P. Wiangnon, K. Sudsiri, N. Muaksang, K. Cherdchu, C. Gören, A. C. Bilsel, M. LeGoff, T. Bearden, D. Bedner, M. Duewer, D. Hancock, D. Lang, B. Lippa, K. Schantz, M. Sieber, J. |
| author |
Westwood, S. |
| author_facet |
Westwood, S. Josephs, R. Choteau, T. Daireaux, A. Mesquida, C. Wielgosz, R. Rosso, A. Ruiz de Arechavaleta, M. Davies, S. Wang, Hongjie Cristina Pires do Rego, E. Marques Rodrigues, J. Freitas Guimarães, E. de. Barreto Sousa, M. V. Monteiro, T. M. Alves das Neves Valente, L. Marques Violante, F. G. Rubim, R. Almeida, R. Baptista Quaresma, M. C. Nogueira, R. Windust, A. Dai, X. Li, X. Zhang, W. Li, M. Shao, M. Wei, C. Wong, S. Cabillic, J. Gantois, F. Philipp, R. Pfeifer, D. Hein, S. Klyk-Seitz, U. Ishikawa, K. Castro, E. Gonzalez, N. Krylov, A. Lin, T. T. Kooi, L. T. Fernandes-Whaley, M. Prévoo, D. Archer, M. Visser, R. Nlhapo, N. de Vos, B. Ahn, S. Pookrod, P. Wiangnon, K. Sudsiri, N. Muaksang, K. Cherdchu, C. Gören, A. C. Bilsel, M. LeGoff, T. Bearden, D. Bedner, M. Duewer, D. Hancock, D. Lang, B. Lippa, K. Schantz, M. Sieber, J. |
| author_role |
author |
| author2 |
Josephs, R. Choteau, T. Daireaux, A. Mesquida, C. Wielgosz, R. Rosso, A. Ruiz de Arechavaleta, M. Davies, S. Wang, Hongjie Cristina Pires do Rego, E. Marques Rodrigues, J. Freitas Guimarães, E. de. Barreto Sousa, M. V. Monteiro, T. M. Alves das Neves Valente, L. Marques Violante, F. G. Rubim, R. Almeida, R. Baptista Quaresma, M. C. Nogueira, R. Windust, A. Dai, X. Li, X. Zhang, W. Li, M. Shao, M. Wei, C. Wong, S. Cabillic, J. Gantois, F. Philipp, R. Pfeifer, D. Hein, S. Klyk-Seitz, U. Ishikawa, K. Castro, E. Gonzalez, N. Krylov, A. Lin, T. T. Kooi, L. T. Fernandes-Whaley, M. Prévoo, D. Archer, M. Visser, R. Nlhapo, N. de Vos, B. Ahn, S. Pookrod, P. Wiangnon, K. Sudsiri, N. Muaksang, K. Cherdchu, C. Gören, A. C. Bilsel, M. LeGoff, T. Bearden, D. Bedner, M. Duewer, D. Hancock, D. Lang, B. Lippa, K. Schantz, M. Sieber, J. |
| author2_role |
author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author author |
| dc.subject.none.fl_str_mv |
Metrología Determinación de materia orgánica Sustancias orgánicas Incertidumbre Calibración Calibradores Mediciones |
| topic |
Metrología Determinación de materia orgánica Sustancias orgánicas Incertidumbre Calibración Calibradores Mediciones |
| dc.description.none.fl_txt_mv |
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. Fil: Westwood, S. Bureau International des Poids et Mesures (BIPM); Francia Fil: Josephs, R. Bureau International des Poids et Mesures (BIPM); Francia Fil: Choteau, T. Bureau International des Poids et Mesures (BIPM); Francia Fil: Daireaux, A. Bureau International des Poids et Mesures (BIPM); Francia Fil: Mesquida, C. Bureau International des Poids et Mesures (BIPM); Francia Fil: Wielgosz, R. Bureau International des Poids et Mesures (BIPM); Francia Fil: Rosso, A. Instituto Nacional de Tecnología Industrial (INTI); Argentina Fil: Ruiz de Arechavaleta, M. Instituto Nacional de Tecnología Industrial (INTI); Argentina Fil: Davies, S. National Measurement Institute (NMIA); Australia Fil: Wang, H. National Measurement Institute (NMIA); Australia Fil: Pires do Rego, E. C. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil Fil: Marques Rodrigues, J. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil Fil: Freitas Guimarães, E. de. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil Fil: Barreto Sousa, M. V. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil Fil: Monteiro, T. M. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil Fil: Alves das Neves Valente, L. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil Fil: Marques Violante, F. G. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil Fil: Rubim, R. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil Fil: Almeida, R. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil Fil: Baptista Quaresma, M. C. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil Fil: Nogueira, R. Instituto Nacional de Metrologia, Qualidade e Tecnologia (INMetro); Brasil Fil: Windust, A. Institute for National Measurement Standards. National Research Council Canada (NRC-INMS); Canadá Fil: Dai, X. National Institute of Metrology (NIM); China Fil: Li, X. National Institute of Metrology (NIM); China Fil: Zhang, W. National Institute of Metrology (NIM); China Fil: Li, M. National Institute of Metrology (NIM); China Fil: Shao, M. National Institute of Metrology (NIM); China Fil: Wei, C. National Institute of Metrology (NIM); China Fil: Wong, S. Government Laboratory of Hong Kong SAR (GLHK); China Fil: Cabillic, J. Laboratoire National de Métrologie et d’Essais (LNE); Francia Fil: Gantois, F. Laboratoire National de Métrologie et d’Essais (LNE); Francia Fil: Philipp, R. Bundesanstalt für Materialforschung (BAM); Alemania Fil: Pfeifer, D. Bundesanstalt für Materialforschung (BAM); Alemania Fil: Hein, S. Bundesanstalt für Materialforschung (BAM); Alemania Fil: Klyk-Seitz, U. Bundesanstalt für Materialforschung (BAM); Alemania Fil: Ishikawa, K. National Metrology Institute of Japan (NMIJ); Japón Fil: Castro, E. Centro Nacional de Metrología (CENAM); México Fil: Gonzalez, N. Centro Nacional de Metrología (CENAM); México Fil: Krylov, A. D. I. Mendeleev Institute for Metrology (VNIIM); Rusia Fil: Lin, T. T. Health Sciences Authority (HSA); Singapur Fil: Kooi, L. T. Health Sciences Authority (HSA); Singapur Fil: Fernandes-Whaley, M. National Metrology Institute of South Africa (NMISA); Sudáfrica Fil: Prévoo, D. National Metrology Institute of South Africa (NMISA); Sudáfrica Fil: Archer, M. National Metrology Institute of South Africa (NMISA); Sudáfrica Fil: Visser, R. National Metrology Institute of South Africa (NMISA); Sudáfrica Fil: Nlhapo, N. National Metrology Institute of South Africa (NMISA); Sudáfrica Fil: de Vos, B. National Metrology Institute of South Africa (NMISA); Sudáfrica Fil: Ahn, S. Korea Research Institute of Standards and Science (KRISS); Corea del Sur Fil: Pookrod, P. National Institute of Metrology of Thailand (NIMT); Tailandia Fil: Wiangnon, K. National Institute of Metrology of Thailand (NIMT); Tailandia Fil: Sudsiri, N. National Institute of Metrology of Thailand (NIMT); Tailandia Fil: Muaksang, K. National Institute of Metrology of Thailand (NIMT); Tailandia Fil: Cherdchu, C. National Institute of Metrology of Thailand (NIMT); Tailandia Fil: Gören, A. C. National Metrology Institute (TUBITAK UME); Turquía Fil: Bilsel, M. National Metrology Institute (TUBITAK UME); Turquía Fil: LeGoff, T. LGC Limited; Reino Unido Fil: Bearden, D. National Institute of Standards and Technology (NIST); Estados Unidos Fil: Bedner, M. National Institute of Standards and Technology (NIST); Estados Unidos Fil: Duewer, D. National Institute of Standards and Technology (NIST); Estados Unidos Fil: Hancock, D. National Institute of Standards and Technology (NIST); Estados Unidos Fil: Lang, B. National Institute of Standards and Technology (NIST); Estados Unidos Fil: Lippa, K. National Institute of Standards and Technology (NIST); Estados Unidos Fil: Schantz, M. National Institute of Standards and Technology (NIST); Estados Unidos Fil: Sieber, J. National Institute of Standards and Technology (NIST); Estados Unidos |
| description |
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. |
| publishDate |
2012 |
| dc.date.none.fl_str_mv |
2012 |
| dc.type.none.fl_str_mv |
info:eu-repo/semantics/article info:eu-repo/semantics/publishedVersion http://purl.org/coar/resource_type/c_6501 info:ar-repo/semantics/articulo |
| format |
article |
| status_str |
publishedVersion |
| dc.identifier.none.fl_str_mv |
Rosso2012CCQM.pdf https://app.inti.gob.ar/greenstone3/sites/localsite/collect/nuevadc/index/assoc/Rosso201.dir/doc.pdf |
| identifier_str_mv |
Rosso2012CCQM.pdf |
| url |
https://app.inti.gob.ar/greenstone3/sites/localsite/collect/nuevadc/index/assoc/Rosso201.dir/doc.pdf |
| dc.language.none.fl_str_mv |
eng |
| language |
eng |
| dc.rights.none.fl_str_mv |
info:eu-repo/semantics/openAccess https://creativecommons.org/licenses/by/3.0/ openAccess |
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openAccess |
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https://creativecommons.org/licenses/by/3.0/ openAccess |
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application/pdf |
| dc.publisher.none.fl_str_mv |
IOP Publishing |
| publisher.none.fl_str_mv |
IOP Publishing |
| dc.source.none.fl_str_mv |
Metrología, 49 reponame:Repositorio Institucional del Instituto Nacional de Tecnología Industrial (INTI) instname:Instituto Nacional de Tecnología Industrial |
| reponame_str |
Repositorio Institucional del Instituto Nacional de Tecnología Industrial (INTI) |
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Repositorio Institucional del Instituto Nacional de Tecnología Industrial (INTI) |
| instname_str |
Instituto Nacional de Tecnología Industrial |
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Repositorio Institucional del Instituto Nacional de Tecnología Industrial (INTI) - Instituto Nacional de Tecnología Industrial |
| repository.mail.fl_str_mv |
pfalcato@inti.gob.ar |
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1846147090632146944 |
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12.712165 |