Uncertainty quantification in material

characterization
Arvind Sharma and Manoj Kumar Singh
M.Tech Students(Transportation Engineering)
Department of Civil Engineering, IIT Delhi
30th April 2016

Overview

Introduction
Uncertainty quantification (UQ)
Materials Characterization
Experimental Methodology
o
o

Sample Material Collection and Preparation

Measurement of Purity
DSC method
Mass Balance (MB) method
Coulometric titration (CT) method

Measurement of uncertainty
DSC Method
Mass Balance (MB) method
CT method

Result and Discussions

Conclusion

Introduction

Uncertainty defined as the situation where the person is unknown of the

state of particular event
Some definitions:

a degree of ignorance (Beven, 2009),

a state of incomplete knowledge (Cullen and Frey, 1999)
Insufficient information (Murray, 2002)
a departure from the unattainable state of complete determinism (Walker et al., 2003).

Generally, the measurements are reported in the range of actual value

achieved from the experiment
Most common way to report a result is best value uncertainty as weight
of sample may be reported as 10 g 0.02 g, Which assumed that the weight
lies between 9.98 g to 10.02 g
Uncertainties generally arise due to the model assumptions and experiment
conducted which depends on nature of apparatus in experiment and theory
used
Four major sources of uncertainty

Limitations of model
Limited accuracy of measurements i.e presence of human errors in data collection
Uncertainty in input due to initial experimental conditions,
Numerical errors in boundary conditions
Measurements uncertainty.

Uncertainty quantification (UQ)

The science of identifying, quantifying, and reducing uncertainty associated
with the assumed model in experiment, numerical algorithm applied and
predicted outcomes or quality of interest in result
It tries to predict the response of an input of certain unknown parameters
It determining the confidence level of the predicted result
It determines the output on the basis of decisions or algorithms applied which
may be having errors.
UQ plays a significant role in Validation of results
Uncertainties may arise during mathematical formulations into numerical
algorithms and computational coding for feeding into computational
applications.
UQ
broadly involves in quantitative characterization, management, and
reduction of uncertainty in applications.
National Academy of Sciences has recognized the necessity of uncertainty in
computational estimates of reality and the necessity for its quantification

Materials Characterization

Material Characterization, defined as the materials that are used for

experimentation for achieving the result to understand the
properties of the study material

Characterization assumed to be the basis for understanding the

composition of a particular material to be used as medicine & other
scientific purpose

Its potential for an adverse effect if any.

Material characterization also serves as a means to ensure

standardization of study materials

Cont.

Figure 1: Modeling, Numerical and experimental components

(Source: Internet)

Figure show the terms play an important role for algorithm of any experiment
Input: used to designate the initial parameters, trial & boundary conditions and the constraints
that exhibit uncertainties

Verification: the checking of accuracy of results by simulation to mathematical models

Validation: to quantify the accuracy of results of simulation codes in mathematical model to
achieve desired level of confidence

Quality of Interest: the output in form of necessary information required for concluding the
experiment

Cont.

Figure shows the systematic approach for characterizing the material

The procedures that are meteorologically valid

for one or more specified properties
Two characteristics of any material are
Homogeneity and stability with its associated
uncertainties
In the process of material characterization,
homogeneity testing associated with two types
of stability testing (Van der Vann 2001)
long term stability of the material
short term stability of the material

The evaluation of uncertainties by following 1. Differential scanning calorimetry (DSC),

2. Mass balance method (MB),
3. Coulometric titration (CT).

Figure 2: Process of uncertainty evaluation

(Source: Shiying Yang,2015)

DSC and CT, both methods were used to obtain information about the purity
of Characterized Reference Material.
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Experimental Methodology

Sample Collection and Preparation

Measurement of Purity
DSC method
Mass Balance (MB) method
Coulometric titration (CT) method

Measurement of uncertainty
DSC Method
Mass Balance (MB) method
CT method

Sample Collection and Preparation

Ferulic acid was obtained from Institute of Materia Medica, Chinese

Academy of Medical

Honokiol raw material was obtained from the Guanyu Biotechnology

Co., Ltd.

Six hundred bottle samples were prepared in a batch

Stored at 25 C for homogeneity and stability determination

Baicalein raw material obtained from Mansite Botanical Development

Co., Ltd,

2.8 L 95% ethanol added in and dissolves Heated, filtrated and mixed with 0.8
L deionized water

The mix was dried over 24 h at 0.01 mbar pressure at constant temperature of
40C

Crystals were crushed into powder and sealed into dark glass bottles containg
50mg each.

Measurement of Purity
Shiying Yang & Ningbo Gonga (2014) performed Homogeneity studies using
DSC method.
One in each of 15 randomly selected bottles was analyzed for homogeneity
Stability studies performed by using DSC method for the short-term stability
Sample divided into six groups, each group contains 6 samples
Stored for 0, 1 ,2, 4, 6 and 12 months at 25 C.
Linear Regression was used to estimate the slope and standard standard
deviation in the stability
Microbubble characteristics through fitting experimental data in theoretical
model

Figure 4: Example of micro bubble image captured by high speed

video microscopy
(Source: Caroline Harfield, 2016)

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Purity by DSC method

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Purity by Mass Balance (MB) method

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Purity by Coulometric titration (CT) method

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Measurement of uncertainty

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uncertainty by DSC Method

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Uncertainty by Mass Balance (MB) method

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Uncertainty by CT method

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Result and discussions

Homogeneity test of samples
For honokiol material was examined using an F test and no outliers were
detected where F value was 1.36 which was lower than the critical F value of
2.04.
For the Baicalein raw material, No significant differences were found in the
purity of baicalein and honokiol
Stability test of samples
For honokiol material, short-term stability test data was examined by t tests,
and no significant differences were found even after stored at high
temperature, humidity and under strong light for 2 weeks.
For Baicalein material, long-term stability test, data was examined by slope
was obtained to be 0.000003, which is statistically indistinguishable from
zero. Thus, the overall the samples were stable even when stored at 25C for
one year.

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Cont.
Purity determination by HPLC
The purity of Baicalein material was P HPLC value achieved is 99.720% with an SD of
0.00392% after deduction of volatile impurity, moisture and ash.
Purity determination by DSC
for ferulic acid, The heat flow temperature curve was plot between T f vs 1/F and
the purity was obtained to be 99.81%.
For honokiol raw material, mean of purity was 99.34 % with an SD of 0.0288 %,
For baicalein mean of purity was calculated to be 99.725% with an SD of 0.0106%.
Purity determination by MB methods
The purity of the ferulic acid sample determined was 99.79%.
Purity determination by CT
The purity of the ferulic acid sample determined was 99.81%.
for honokiol raw material, the purity was 99.34 % with an SD of 0.0825 %.
The mean purity of baicalein was 99.722% with an SD of 0.0158%.
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Evaluation of uncertainty
Uncertainty of homogeneity
The uncertainty of homogeneity for baicalein and ferulic acid are 0.0000134
and 0.0000465 respectively.
Uncertainty of stability
The uncertainty of stability for baicalein and ferulic acid are 0. 0000590 and 0.
0006612 respectively.
Uncertainty of mass balance
The standard uncertainty of mass balance for baicalein and ferulic acid are
0.000818 and 0.00211 respectively.
Uncertainty of DSC
The standard uncertainty of DSC for baicalein and ferulic acid are 0.00035
and 0. 00051 respectively.
Uncertainty of CT
The standard uncertainty of CT for baicalein and ferulic acid are 0. 00087 and
0. 00098 respectively.
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conclusion
Three methods: The mass balance, Differential Scanning Calorimetry,
and Coulometric titration methods were studied and was found that
the purity of baicelin, honokiol materials for consistent results.
These

methods

have

advantages

as

small

sample

amount

requirement, quick measurement, and high accuracy can be used as

alternative methods for testing
Methods not have narrow working range
In the study, it was concluded that consistent result can be obtained
with confidence in the purity assessment.
The studies of homogeneity and stability showed that materials can be
stable for one year or more

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Thankyou

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