CCQM Activities in the Organic Analysis Working Group

Summary

NIST's Chemical Sciences Division has participated in over 50 Consultative Committee for Amount of Substance - Metrology in Chemistry (CCQM) Organic Analysis Working Group (OAWG) studies since 1997 and coordinated numerous studies over this long history. The CCQM conducts international comparisons to establish equivalence among measurements made by national metrology institutes (NMIs). Recent OAWG studies included a direct comparison of CRMs for vitamin B3 (niacin) in milk powders and infant/adult nutritional formulas, polycyclic aromatic hydrocarbons (PAHs) in olive oil, purity assessments of folic acid and bisphenol A. 

Description

Key comparison data demonstrating NMI performance measuring moisture by Karl Fisher titration in folic acid at varying relative humidity.

Credit: CCQM-K55.d (Folic acid) Final Report: April 2018

The results from these studies will be used to demonstrate the capabilities of participating NMIs for their similar measurement services, and eventually benchmark the appropriate Calibration and Measurement Capabilities (CMCs) that summarizes this capability.  NIST CMCs that directly support SI traceability (e.g., pure chemical standards, calibration solutions) are also benchmarked by this process. 

Major Accomplishments

• CCQM-K55c Purity assignment of L-valine
• CCQM-K55d Purity assignment of folic acid
• CCQM-K131 Low-polarity analytes in a multicomponent organic solution: PAHs in acetonitrile
• CCQM-K142 Comparison of CRMs and value-assigned quality controls: urea and uric acid in human serum or plasma
• CCQM-K146 PAHs in olive oil
• CCQM-K147 Comparison of value-assigned CRMs for niacin (vitamin B₃) in milk powder and infant formula matrices

ASSOCIATED PUBLICATIONS

• 1. Li, X. M., Li, H. M., Zhang, Q. H., Lu, X. H., Li, S. Q., Koch, M., Polzer, J., Hackenber, R., Moniruzzaman, M., Khan, M., Kakoulides, E., Pak-Wing, K., Richy, Chi-Shing, N., Lu, T., Gui, E. M., Cheow, P. S., Teo, T. L., Rego, E., Garrido, B., Carvalho, L., Leal, R., Violante, F., Baek, S. Y., Lee, S., Choi, K., Kim, B., Bucar-Miklavcic, M., Hopley, C., Nammoonnoy, J., Murray, J., Wilson, W., Toman, B., Itoh, N., Gokcen, T., Krylov, A., and Mikheeva, A., "CCQM-K146 low-polarity analyte in high fat food: benzo[a]pyrene in olive oil," Metrologia, 57, (2020). 

  2. Arzate, C. M. S., Burdette, C. Q., Aragon, H. G., Lippa, K. A., Osuna, M. A., Contreras, L. R., Lee, J., Lee, S., Baek, S. Y., Kim, B., Huang, T., Guo, Z., Li, H. M., Zhang, Q. H., Phillips, M. M., Toman, B., and Duewer, D. L., "CCQM-K147 Comparison of value-assigned CRMs for niacin (vitamin B-3) in milk powder and infant formula matrices," Metrologia, 56, (2019). 

  3. Duewer, D. L., Murray, J. A., Wood, L. J., Wise, S. A., Sander, L. C., Lippa, K., Hein, S., Koch, M., Philipp, R., Werneburg, M., Hackenberg, R., Polzer, J., Avila, M. A., Serrano, V., Kakoulides, E., Alexopoulos, C., Giannikopoulou, P., Gui, E. M., Lu, T., Teo, T. L., Hua, T., Chen, D. Z., Li, C. X., Ye, C. J., Li, H. M., Nammoonnoy, J., Quinn, L., Swiegelaar, C., Fernandes-Whaley, M., Goren, A. C., and Gokcen, T., "CCQM-K95.1 Low-polarity analytes in a botanical matrix: polycyclic aromatic hydrocarbons (PAHs) in tea," Metrologia, 56, (2019). 

  4. Duewer, D. L., Sander, L. C., Wise, S. A., Lippa, K., Philipp, R., Hein, S., Hackenberg, R., Polzer, J., Avila, M. A., Serrano, V., Kakoulides, E., Alexopoulos, C., Giannikopoulou, P., Chan, P. K., Lee, H. M., Tang, H. S., Tang, P. O., Yip, Y. C., Lu, T., Cheow, P. S., Teo, T. L., do Rego, E. C. P., Violante, F. G. M., de Carvalho, L. J., Leal, R. V. P., Sega, M., Rolle, F., Baek, S. Y., Kim, B., Lee, S., Cabillic, J., Fallot, C., Hua, T., Chen, D. Z., Ye, C. J., Li, C. X., Li, H. M., Itoh, N., Quinn, L., Prevoo-Franzsen, D., Fernandes-Whaley, M., Goren, A. C., Gokcen, T., Gunduz, S., Krylov, A., Mikheeva, A., Baldan, A., van der Hout, J. W., and van der Veen, A. M. H.,  "CCQM-K131 Low-polarity analytes in a multicomponent organic solution: polycyclic aromatic hydrocarbons (PAHs) in acetonitrile," Metrologia, 56, (2019). 

  5. Lippa, K. A., Duewer, D. L., Nelson, M. A., Davies, S. R., and Mackay, L. G., "The role of the CCQM OAWG in providing SI traceable calibrators for organic chemical measurements," Accreditation and Quality Assurance, 24, 407-415 (2019). 

  6. Liu, Q. D., Liu, H., Chen, Y. Z., Yong, S. R., Teo, H. L., Wong, L. K., Teo, T. L., Vamathevan, V., do Rego, E. C. P., Wollinger, W., Fernandes, J. L. N., Monteiro, T. M., Garrido, B. C., Violante, F. M., Shi, L. H., He, H. H., Quan, C., Xu, B., Li, H. M., Dai, X. H., He, Y. J., Lo, M. F., Yip, Y. C., Cabillic, J., Delatour, V., Ohlendorf, R., Henrion, A., Kawaguchi, M., Kang, D., Lee, H., Osuna, M. A., Serrano, V., Arzate, C. M. S., Krylov, A., Lopushanskaya, E., Nammoonnoy, J., Goren, A. C., Gunduz, S., Yilmaz, H., Mussell, C., Warren, J., Pritchett, J. S., Lippa, K., Nelson, M. A., Toman, B., Sniegoski, L. T., and Duewer, D., "High polarity analytes in biological matrix: determination of urea and uric acid in human serum (CCQM-K109)," Metrologia, 56, (2019). 

  7. Teo, T. L., Liu, Q. D., Cheow, P. S., Duewer, D., Lippa, K., Toman, B., Osuna, M. A., Serrano, V., Arzate, C. M. S., Wong, L. K., Chen, Y. Z., Yong, S., Teo, H. L., Liu, H., Tong, B., Kang, D., Lee, H., Dai, X. H., Quan, C., Shi, L. H., Li, H. M., and Pritchett, J. S., "Comparison of CRMs and value-assigned quality controls: urea and uric Acid in human serum or plasma (CCQM-K142)," Metrologia, 56, (2019). 

  8. Teo, T. L., Lippa, K. A., Mackay, L., Yong, S., Liu, Q. D., Camara, J. E., Delatour, V., Lee, T. K., Lalere, B., O'Connor, G., Henrion, A., Kato, M., Numata, M., Kwon, H. J., Jeong, J. S., Xu, B., Song, D. W., Nammoonnoy, J., and Wollinger, W., "Enhancing the accuracy of measurement of small molecule organic biomarkers," Analytical and Bioanalytical Chemistry, 411, 7341-7355 (2019). 

  9. Westwood, S., Josephs, R., Choteau, T., Daireaux, A., Wielgosz, R., Melanson, J., Thibeault, M. P., Meija, J., Quan, C., Hongmei, L., Huang, T., Zhang, W., Song, D., Martos, G., Delatour, V., Ohlendorf, R., Henrion, A., Kakoulides, E., Giannikopoulou, P., Alexopoulos, C., Chan, K., Lam, W. H., Fung, W. H., Yamazaki, T., Krylov, A., Lopushanskaya, E., Kharitonov, S., Belyakov, M., Sokolova, O., Liu, Q. D., Liu, H., Yong, S., Prevoo-Franzsen, D., Fernandes-Whaley, M., Kim, B., Jeong, J. S., Kwon, H. J., Yang, I., Nammoonnoy, J., Goren, A. C., Gunduz, S., Un, I., Bilsel, G., Biesenbruch, S., and Lowenthal, M., "Mass fraction assignment of Amino Acids in acidic aqueous solution (CCQM-K78.a)," Metrologia, 56, (2019). 

  10. Wise, S. A., Phinney, K. W., Duewer, D. L., Sniegoski, L. T., Welch, M. J., Pritchett, J., Pabello, G., Calderon, M. A. A., Balderas, M., Liu, Q. D., Kooi, L. T., Rego, E., Garrido, B., Allegri, G., de La Cruz, M., Barrabin, J., Monteiro, T., Lee, H., Kim, B., Delatour, V., Peignaux, M., Kawaguchi, M., Bei, X., Can, Q., Nammoonnoy, J., Schild, K., Ohlendorf, R., Henrion, A., Goren, A. C., Yilmaz, H., Bilsel, M., Konopelko, L., Krylov, A., and Lopushanskaya, E., "CCQM-K11.2 Determination of Glucose in Human Serum and CCQM-K12.2 Determination of Creatinine in Human Serum," Metrologia, 55, (2018). 

  11. Wise, S. A., Phinney, K. W., Duewer, D. L., Sniegoski, L. T., Welch, M. J., Pabello, G., Caldero, M. A. A., Liu, Q. D., Kooi, L. T., Rego, E., Garrido, B., Allegri, G., de La Cruz, M., Barrabin, J., Puglisi, C., Lopez, E., Lee, H., Kim, B., Delatour, V., Heuillet, M., Nammoonnoy, J., Goren, A. C., Bilsel, G., Konopelko, L., Krylov, A., and Lopushanskaya, E., "CCQM-K6.2 Determination of Total Cholesterol in Human Serum," Metrologia, 55, (2018). 

  12. Wise, S. A., Tai, S. S. C., Duewer, D. L., Bedner, M., Camara, J. E., Lippa, K. A., Qinde, L., Kang, D., Kim, B., and Quan, C., "CCQM-K132: low-polarity analytes in a biological matrix: vitamin D metabolites in human serum," Metrologia, 54, (2017). 

  13. Wise, S., "CCQM activities and impact in food safety and nutrition," Abstracts of Papers of the American Chemical Society, 250, (2015). 

  14. Westwood, S., Josephs, R., Choteau, T., Daireaux, A., Wielgosz, R., Davies, S., Moawad, M., Chan, B., Munoz, A., Conneely, P., Ricci, M., do Rego, E. C. P., Garrido, B. C., Violante, F. G. M., Windust, A., Dai, X. H., Huang, T., Zhang, W., Su, F. H., Quan, C., Wang, H. F., Lo, M. F., Wong, W. F., Gantois, F., Lalerle, B., Dorgerloh, U., Koch, M., Klyk-Seitz, U. A., Pfeifer, D., Philipp, R., Piechotta, C., Recknagel, S., Rothe, R., Yamazaki, T., Bin Zakaria, O., Castro, E., Balderas, M., Gonzalez, N., Salazar, C., Regalado, L., Valle, E., Rodriguez, L., Laguna, L. A., Ramirez, P., Avila, M., Ibarra, J., Valle, L., Perez, M., Arce, M., Mitani, Y., Konopelko, L., Krylov, A., Lopushanskaya, E., Lin, T. T., Liu, Q. D., Kooi, L. T., Fernandes-Whaley, M., Prevoo-Franzsen, D., Nhlapo, N., Visser, R., Kim, B., Lee, H., Kankaew, P., Pookrod, P., Sudsiri, N., Shearman, K., Goren, A. C., Bilsel, G., Yilmaz, H., Bilsel, M., Cergel, M., Coskun, F. G., Uysal, E., Gunduz, S., Un, I., Warren, J., Bearden, D. W., Bedner, M., Duewer, D. L., Lang, B. E., Lippa, K. A., Schantz, M. M., Sieber, J. R., and Westwood, S., "Final Report on Key Comparison CCQM-K55.c (L-(+)-Valine): Characterization of Organic Substances for Chemical Purity," Metrologia, 51, (2014). 

  15. Camara, J. E., Duewer, D. L., Gasca-Aragon, H., Lippa, K. A., and Toman, B., "CCQM-K80 Comparison of value-assigned CRMs and PT materials: creatinine in human serum Final Report," Metrologia, 50, (2013). 

  16. Hein, S., Philipp, R., Duewer, D. L., Gasca-Aragon, H., Lippa, K., and Toman, B., "CCQM-K79 Comparison of value-assigned CRMs and PT materials: Ethanol in Aqueous Matrix Final Report," Metrologia, 50, (2013). 

  17. Urquiza, M. P., Torres, M. M., Mitani, Y., Schantz, M. M., Duewer, D. L., May, W. E., Parris, R. M., Wise, S. A., Kaminski, K., Philipp, R., Win, T., Rosso, A., Kim, D. H., Ishikawa, K., Krylov, A. I., Kustikov, Y. A., and Baldan, A., "CCQM Key Comparison - Organic Solutions CCQM-K47 Volatile Organic Compounds in Methanol Final Report," Metrologia, 50, (2013). 

  18. Camara, J. E., Lippa, K. A., Duewer, D. L., Gasca-Aragon, H., and Toman, B., "An international assessment of the metrological equivalence of higher-order measurement services for creatinine in serum," Analytical and Bioanalytical Chemistry, 403, 527-535 (2012). 

  19. Westwood, S., Josephs, R., Choteau, T., Daireaux, A., Mesquida, C., Wielgosz, R., Rosso, A., de Arechavaleta, M. R., Davies, S., Wang, H. J., do Rego, E. C. P., Rodrigues, J. M., Guimaraes, E. D., Sousa, M. V. B., Monteiro, T. M., Valente, L. A. D., Violante, F. G. M., Almeida, R. R. R., Quaresma, M. C. B., Nogueira, R., Windust, A., Dai, X. H., Li, X. M., Zhang, W., Li, M., Shao, M. W., Wei, C., Wong, S. K., Cabillic, J., Gantois, F., Philipp, R., Pfeifer, D., Hein, S., Klyk-Seitz, U. A., Ishikawa, K., Castro, E., Gonzalez, N., Krylov, A., Lin, T. T., Kooi, L. T., Fernandes-Whaley, M., Prevoo, D., Archer, M., Visser, R., Nlhapo, N., de Vos, B., Ahn, S., Pookrod, P., Wiangnon, K., Sudsiri, N., Muaksang, K., Cherdchu, C., Goren, A. C., Bilsel, M., LeGoff, T., Bearden, D., Bedner, M., Duewer, D., Hancock, D., Lang, B., Lippa, K., Schantz, M., and Sieber, J., "Final report on key comparison CCQM-K55.b (aldrin): An international comparison of mass fraction purity assignment of aldrin," Metrologia, 49, (2012). 

  20. Westwood, S., Josephs, R., Daireaux, A., Wielgosz, R., Davies, S., Wang, H. J., Rodrigues, J., Wollinger, W., Windust, A., Kang, M., Su, F. H., Philipp, R., Kuhlich, P., Wong, S. K., Shimizu, Y., Perez, M., Avila, M., Fernandes-Whaley, M., Prevoo, D., de Vos, J., Visser, R., Archer, M., LeGoff, T., Wood, S., Bearden, D., Bedner, M., Boroujerdi, A., Duewer, D., Hancock, D., Lang, B., Porter, B., Schantz, M., Sieber, J., White, E., and Wise, S. A., "CCQM-K55. a (Estradiol) Final Report: August 2012 CCQM-K55. a Key Comparison on the Characterization of Organic Substances for Chemical Purity," Metrologia, 49, (2012). 

  21. Westwood, S., Josephs, R., Choteau, T., Mesquida, C., Daireaux, A., Wielgosz, R., Davies, S., Windust, A., Kang, M., Ting, H., Kato, K., Frias, E., Perez, M., Apps, P., Fernandes-Whaley, M., Wiangnon, K., Ruangrittinon, N., Wood, S., LeGoff, T., Duewer, D., Schantz, M., Siekmann, L., and Esker, J., "An international comparison of mass fraction purity assignment of digoxin: The Comite Consultatif pour la Quantite de Matiere (CCQM) Pilot Study CCQM-P20.f (Digoxin)," Metrologia, 48, (2011). 

  22. Kipphardt, H., Matschat, R., Vogl, J., Gusarova, T., Czerwensky, M., Heinrich, H. J., Hioki, A., Konopelko, L. A., Methven, B., Miura, T., Petersen, O., Riebe, G., Sturgeon, R., Turk, G. C., and Yu, L. L., "Purity determination as needed for the realisation of primary standards for elemental determination: status of international comparability," Accreditation and Quality Assurance, 15, 29-37 (2010). 

  23. Sharpless, K. E., Rimmer, C. A., Phinney, K. W., Nelson, B. C., Duewer, D. L., Wise, S. A., Kim, B., Liu, J., Huang, T., and Zhang, W., "Final report on CCQM-K62: Nutrients in infant/adult formula-vitamins," Metrologia, 47, (2010). 

  24. Tai, S. S. C., Duewer, D. L., Urquiza, M. P., Lee, H., Mussell, C., Dai, X. H., Phinney, K. W., Welch, M. J., Wise, S. A., Murby, J., Kawaguchi, M., and Henrion, A., "Final report on CCQM-K63.a,b: Non-peptide hormones in serum: cortisol and progesterone," Metrologia, 47, (2010). 

  25. Schantz, M. and Wise, S., "CCQM-K25: Determination of PCB congeners in sediment," Metrologia, 41, (2004).