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Preparation and characterization of phosphate rock as quality control material

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Abstract

A quality control material for inorganic constituents present in a phosphate-bearing rock used to manufacture phosphate fertilizers was produced and characterized according to the ISO Guide 80. The evaluation of the estimated minimum mass, homogeneity, and stability of the material was performed using microwave-assisted digestion and inductively coupled plasma optical emission spectrometry (ICP-OES) as an in-house validated technique for determination of Al, As, Ca, Cd, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, V, and Zn. Phosphorus mass fraction determination was done by laser-induced breakdown spectroscopy. The accuracy of the measurement results was confirmed by analyzing the certified phosphate rock and fertilizer certified reference materials according to NIST SRM 694 and SRM 695. One-way analysis of variance (ANOVA) was applied to the measurement data, and the homogeneity and stability of the material presented averages within the 95 % confidence interval. The results from the preparation and with collaborative trial allowed the calculation and estimation of the consensus value and its expanded measurement uncertainties, obtained by combining the uncertainty contributions from characterization (u char), between-bottle homogeneity (u bb), short-term stability (u sts), and long-term stability (u lts) for each evaluated analyte mass fraction.

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References

  1. MAPA—Ministério da Agricultura, Pecuária e Abastecimento. http://www.brasil.gov.br/economia-e-emprego/2016/12/agronegocio-deve-ter-crescimento-de-2-em-2017. Accessed 28 July 2017

  2. United Nations Conference on trade and development (UNCTAD). http://www.unctad.org. Accessed 6 Feb 2017

  3. http://www.portaldoagronegocio.com.br/index.php. Accessed 6 Feb 2017

  4. EURACHEM/CITAC (2012) Quantifying Uncertainty in Analytical Measurement, 3ª ed. http://www.eurachem.org/images/stories/Guides/pdf/QUAM2012_P1.pdf. Accessed July 28 2017

  5. Santana MAA (2003) Requisitos técnicos para competência de laboratórios de calibração e ensaios aplicados em P&D. ENQUALAB, São Paulo

    Google Scholar 

  6. JCGM 200:2012. International vocabulary of metrology—basic and general concepts and associated terms (VIM 3rd ed) BIPM, Sèvres. http://www.bipm.org/en/publications/guides/vim.html. Accessed on Aug 2 2017

  7. ISO 17034 (2016) General requirements for the competence of reference material producers. International Organizational for Standardization, Geneva

  8. De Bièvre P, Lamberty A (1998) An enriched 6Li isotopic reference material. Int J Mass Spectrom Ion Processes 83:135–145

    Google Scholar 

  9. Caroli S, Spagnoli M, Forte G, Alessandrelli M, Cresti R, D’Ilio S, Pauwels J, Kramer GN, Z’aray G (2000) Trace elements in bovine muscle: an ongoing project for a new certified reference material. Microchem J 67:235–243

    Article  CAS  Google Scholar 

  10. Cardoso MHWM, Nobrega AW, Vital HC, Abrantes S (2010) Preparação de um material de referência certificado para controle de agrotóxicos em hortifrutigranjeiros: estudo da homogeneidade. Ciênc Tecnol Aliment 30-2: 429–438, ISSN: 0101-2061

  11. Nogueira ARA, Souza GB, Bossu CM, Bianchi SR, Verhalen TR, Silva PT, Peixoto AMDJ, Silva CS (2016) Embrapa’s experience in the production and development of agriculture reference materials. J phys Conf Ser 733:012005

    Article  Google Scholar 

  12. ISO Guide 80 (2014) Guidance for the in-house preparation of quality control materials (QCMs). International Organization for Standardization, Geneva

    Google Scholar 

  13. ISO Guide 34 (2009) General requirements for the competence of reference materials producers. International Organization for Standardization, Geneva

    Google Scholar 

  14. ISO Guide 35 (2006) Reference materials—general and statistical principles for certification. International Organization for Standardization, Geneva

    Google Scholar 

  15. Brasil. Ministério da Agricultura, Pecuária e Abastecimento (2017). Manual de métodos analíticos oficiais para fertilizantes e corretivos/Ministério da Agricultura, Pecuária e Abastecimento. Secretaria de Defesa Agropecuária. Brasília: MAPA, p 240

  16. Kane PF, Hall WL (2006) Determination of arsenic, cadmium, cobalt, chromium, lead, molybdenium, nickel, and selenium in fertilizers by microwave digestion and inductively coupled plasma-optical emission spectrometry detection: collaborative study. J AOAC Int 89–6:1447–1466

    Google Scholar 

  17. ISO Guide 30 (2015) Reference materials—selected terms and definitions. International Organization for Standardization, Geneva

    Google Scholar 

  18. Moreira EG, Vasconcellos MBA, Catharino MGM, Maihara VA, Saiki M (2009) Perna perna mussel reference material: short term stability assessment. J Radioanal Nucl Chem 282:957–962

    Article  CAS  Google Scholar 

  19. ISO Guide 33 (2015) Reference materials—good practice in using reference materials. International Organization for Standardization, Geneva

    Google Scholar 

  20. Gandra RLP, Santos ALS, Santos PPB, Alvarenga RL, Junqueira RG, Labanca RA, Souza SVC (2016) Production and evaluation of a reference material for moisture, ash, and total fat mass fractions, and titratable acidity in whole milk powder. Accred Qual Assur 21:47–55

    Article  CAS  Google Scholar 

  21. ISO/IEC 17043 (2010) Conformity assessment—general requirements for proficiency testing. International Organization for Standardization, Geneva

    Google Scholar 

  22. Grubbs FE (1969) Procedures for detecting outlying observations in sample. Technometrics 11:1–21

    Article  Google Scholar 

  23. Horwitz W (1982) Evaluation of analytical methods used for regulation of food and drugs. Anal Chem 54:67A–76A

    Article  CAS  Google Scholar 

  24. Thompson M (2000) Recent trends in inter-laboratory precision at ppb and sub-ppb concentrations in relation to fitness for purpose criteria in proficiency testing. Analyst 125:385–386

    Article  CAS  Google Scholar 

  25. Uhrovcik J (2014) Strategy for determination of LOD and LOQ values—some basic aspects. Talanta 119:178–180

    Article  CAS  Google Scholar 

Download references

Acknowledgements

We are grateful for grants and fellowships provided by Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP - 2015/14488-0), Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq), and Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES).

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Authors and Affiliations

  1. Embrapa Pecuária Sudeste, P.O. Box 339, São Carlos, SP, 13560-970, Brazil

    Caroline Santos da Silva, Gilberto Batista de Souza & Ana Rita Araujo Nogueira

  2. Group of Applied Instrumental Analysis, Department of Chemistry, Federal University of São Carlos, P.O. Box 676, São Carlos, SP, 13560-970, Brazil

    Caroline Santos da Silva

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  1. Caroline Santos da Silva
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  2. Gilberto Batista de Souza
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  3. Ana Rita Araujo Nogueira
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Corresponding author

Correspondence to Caroline Santos da Silva.

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da Silva, C.S., de Souza, G.B. & Nogueira, A.R.A. Preparation and characterization of phosphate rock as quality control material. Accred Qual Assur 23, 39–45 (2018). https://doi.org/10.1007/s00769-017-1295-3

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