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Complete curve fitting of extraction profiles for estimating uncertainties in recovery estimates.

Date: 01/10/2002 Ref No: LGC/VAM/2002/038 Type: Report
Author(s): Stephen L R Ellison, V J Barwick, P J Norris, M Griffiths
Organisation/Publisher: LGC

The complete submitted paper forming the body of this report forms deliverable MU3 d in the VAM 2000-2003 programme.

The paper incorporates some basic material originally described in report LGC/VAM/2002/016 part 2, but includes very substantial additional work.

The basic work in the previous report described the implementation of full curve fitting of a spherical particle diffusion model to polymer extraction data obtained by pressurised fluid extraction. The additions included in the present paper are:

  • A comparison of the numerical model with the three-point extrapolation reported in earlier published work, showing marked improvement on manually acquired data from Soxhlet extraction.
  • Extension to include plane sheet and cylindrical particle shapes, allowing film and fibre modelling respectively.
  • Implementation of an improved uncertainty estimation method which allows for correlation among residuals; failure to take this effect into account can result in substantial underestimation of uncertainty and also compromise parameter estimates.
  • An approximate implementation of a model based on concentration-dependent diffusion coefficient. This model resulted in a very marked improvement in fit compared to any of the constant diffusion coefficient models.


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