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Temperature calibration of differential scanning calorimeters

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Abstract

A procedure for calibrating the temperature scale of a DSC is described. A different calibration trend was obtained using the transition points of organic compounds compared to that found using the melting points of highly pure metals. The crystal-crystal transitions of three ammonium salts were studied by this method; ammonium dihydrogen phosphate and ammonium sulphate were found to be suitable reference materials in the region −150 to 0°C, but ammonium nitrate was found to be unsuitable due to poorly defined transition points and inconsistent thermal behaviour.

Zusammenfassung

Es wird ein Vorgehen für die Kalibration der Temperaturskale bei DSC beschrieben. Vergleicht man die Verwendung von Umwandlungstemperaturen organischer Verbindungen mit den Schmelztemperaturen von hochreinen Metallen, erhält man unterschiedliche Kalibrationstendenzen. Mittels vorliegender Methode wurde die Kristall-Kristall-Umwandlung dreier Ammoniumsalze untersucht; Ammoniumdihydrogenphosphat und Ammoniumsulfat wurden im Bereich von −150 bis 0°C für geeignete Referenzsubstanzen befunden, Ammoniumnitrat ist hierzu jedoch wegen des nicht genau definierten Umwandlungspunktes und seines inkonsistenten thermischen Verhaltens nicht geeignet.

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References

  1. H. G. McAdie, Thermochim. Acta, 1 (1970) 325.

    Article  CAS  Google Scholar 

  2. E. M. Barrall II, Thermochim. Acta, 5 (1973) 377.

    Article  CAS  Google Scholar 

  3. Standard Practice for Temperature Calibration of Differential Scanning Calorimeters and Differential Thermal Analyzers, ASTM E967-92.

  4. E. L. Charsley, Anal. Proc. (London), 17 (1980) 223

    CAS  Google Scholar 

  5. P. A. Barnes, E. L. Charsley, J. A. Rumsey and S. B. Warrington Anal. Proc. (London), 21 (1984) 5.

    CAS  Google Scholar 

  6. A. D. Barker, J. Thermal Anal., 40 (1993) 799.

    Article  CAS  Google Scholar 

  7. Council Regulation (EEC) No. 2455/92 (23rd July 1992), Official J. of Europ. Com. No. L251/13 (29.8.92).

  8. M. Jarratt, MSc Dissertation, University of Warwick, 1993.

  9. G. W. H. Höhne, H. K. Cammenga, W. Eysel, E. Gmelin and W. Hemminger, Thermochim. Acta, 160 (1990) 1.

    Article  Google Scholar 

  10. H. Preston-Thomas, Metrologia, 27 (1990) 3.

    Article  Google Scholar 

  11. R. L. Rusby, R. P. Hudson, M. Durieux, J. F. Schooley, P. P. M. Steur and C. A. Swenson, Metrologia, 28 (1991) 9.

    Article  Google Scholar 

  12. H. Preston-Thomas, Metrologia, 12 (1976) 7.

    Article  CAS  Google Scholar 

  13. E. L. Charsley, J. P. Davies, E. Glöggler, H. Hawkins, G. W. Höhne, T. J. Lever, K. Peters, M. J. Richartdson, J. Rothemund and A. Stegmeyer, J. Thermal Anal., 40 (1993) 1405.

    Article  CAS  Google Scholar 

  14. H. K. Cammenga, W. Eysel, E. Gmelin, W. Hemminger, G. W. Höhne and J. M. Sarge, Thermochim. Acta, 219 (1993) 337.

    Article  Google Scholar 

  15. J. G. Aston, G. J. Szasz and H. L. Finke, J. Am. Chem. Soc., 65 (1943) 135.

    Google Scholar 

  16. G. T. Furukawa, J. L. Riddle, W. R. Bigge and E. R. Pfeiffe, Natl. Bur. Std. (US) Special Publication, 260–77 (1982)

  17. H. L. Finke, M. E. Gross, G. Waddington and H. M. Huffman, J. Am. Chem. Soc., 76 (1954) 333.

    Article  CAS  Google Scholar 

  18. M. J. Richardson and N. G. Savill, Thermochim. Acta, 1 (1975) 213.

    Article  Google Scholar 

  19. H. P. Klug and W. W. Johnson, J. Am. Chem. Soc., 59 (1937) 2061.

    Article  CAS  Google Scholar 

  20. C. C. Stephenson and A. C. Zettlemeyer, J. Am. Chem. Soc., 66 (1944) 1405.

    Article  CAS  Google Scholar 

  21. D. Hogg and L. A. K. Staveley, unpublished (in Ref. 25). J. Chem. Soc., (1951) 2572.

  22. C. C. Stephenson and J. G. Hooley, J. Am. Chem. Soc., 66 (1944) 1397.

    Article  CAS  Google Scholar 

  23. C. C. Stephenson and A. C. Zettlemeyer, J. Am. Chem. Soc., 66 (1944) 1402.

    Article  CAS  Google Scholar 

  24. C. C. Stephenson and H. E. Adams, J. Am. Chem. Soc. 66 (1944) 1409.

    Article  CAS  Google Scholar 

  25. D. G. Thomas and L. A. K. Staveley, J. Chem. Soc., (1951) 2572.

  26. A. G. Kennan, J. Am. Chem. Soc., 77 (1955) 1379.

    Article  Google Scholar 

  27. C. N. R. Rao, B. Prakash and M. Natarajan, Crystal Structure Transitions in Inorganic Nitrates, Nitrates and Carbonates, NSRS-NBS publication 53, 1975.

  28. K. Tanaka and I. Fukuyama, J. Phys. Soc. Japan, 8 (1953) 428.

    Article  CAS  Google Scholar 

  29. J. Whetstone, Acta Cryst., 7 (1954) 697.

    CAS  Google Scholar 

  30. M. Nagatani, Kogyo Kaguka Zasshi, 68 (1965) 424.

    CAS  Google Scholar 

  31. S. I. Vol’fkovich, S. M. Rubinchik and V. M. Kozhin, Izv. Akad. Nauk SSSR, Otdel Kim. Nauk, (1954) 209.

  32. R. N. Brown and A. C. McLaren, Proc. Roy. Soc., 266 (1962) 329.

    CAS  Google Scholar 

  33. R. R. Sowell, M. M. Karnowsky and L. C. Walters, J. Thermal Anal. 3 (1971) 119.

    Article  CAS  Google Scholar 

  34. C. C. Stephenson, D. R. Bentz and D. A. Stevenson, J. Am. Chem. Soc., 77 (1955) 2161.

    Article  CAS  Google Scholar 

  35. R. G. Early and T. M. Lowry, J. Chem. Soc., 115 (1919) 1387.

    CAS  Google Scholar 

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  1. Courtaulds Research & Technology, Lockhurst Lane, PO Box 111, CV6 5RS, Coventry, UK

    D. M. Price

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Price, D.M. Temperature calibration of differential scanning calorimeters. Journal of Thermal Analysis 45, 1285–1296 (1995). https://doi.org/10.1007/BF02547423

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