ERRORS IN PHARMACEUTICAL ANALYSIS

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ERRORS IN
PHARMACEUTICAL ANALYSIS
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• Definition
Error is an action which means mistake.
In analytical chemistry error is a difference
between true value or standard value and
observed value.
absolute Error = true value - observed value

(+ or -)
% error = true value - observed value × 100
true value
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• If a tablet contains 500mg of paracetamol

and a analyst observed the value after
analysis is 490 mg, then calculate the error?
True value/standard value = 500mg
Observed value= 490 mg
Absolute error= true value - observed value
= 500-490 =10mg
% error = true value - observed value × 100
true value
= 500- 490
5oo × 100 = 2%
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Source of error
• 1. Sample preparations
2. Error by analyst/ manual error
3. Equipment problem
4. Calibration- error may occur if proper
calibration is not done
5. Reporting error – error occur due to
wrong/improper data 0r observation
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• 6. Calculation error – Due to wrong

calculation
7. Error in method selection
8. Improper Sampling
9. Laboratory environment- Due to unsuitable
laboratory environment
10. Error during transport-Error may occur
due to improper handling of materials during
transport and storage
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Types of errors:-
1. Operational and
personal error
2. Instrumental
and reagent error
3. Error of method
4. Additive
5.proportional
error
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DETERMINATE ERROR/ SYSTEMATIC

ERROR /CONSTAND ERROR
• As the name indicate , the cause of this
type of error may be found out & thus
these error can be either avoided or
corrected
• Determinate error are systematic error
i.e. they are not random
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MINIMISATION OF ERRORS
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1. Calibration of apparatus and

application of corrections
 By calibrating all the instruments, error
can be minimized and appropriate
corrections are applied to the original
measurements.
 In some case errors cannot be eliminated,
apply a correction for that effect.
 Volume, weight and delivery time at
calibration temperature are common
parameter for calibrations.
 Maintain constant temperature during
calibrations
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2. Running a blank determination

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3. Running a control
determination
• By running a control determination parallerly to
the sample by taking standard under same
experimental conditions the error can be
reduced at very possible extent.
• However, a standard should contain same weight
of the constituent present in unknown sample.
The weight of the constituent of unknown sample
can be calculated as follows
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4. Use of independent methods of

analysis
 In that case, the analysis of same sample by totally
different methods is performed and the results obtained
from both methods are compared. If they are identical
then they are considered as reliable.
For example:-
1. Determination of strength of HCl solution.
The strength of HCl solution is performed by titration with
standard NaOH and also by precipitation titration method
with AgCl and results are obtained from both methods are
campared.
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2. Hardness of water
In this case the concentrations of
magnesium and calcium is determined by
both atomic absorption spectroscopy and
EDTA titrations and results are compared.
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5. Running of parallel
determination
• Instead of single determination, duplicate
or triplicate determination is carried out
to minimize the possibilities of accidental
errors.
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6. Standard addition/ recovery

studies
• In this method, small amount of standard of
constituent present in sample is added and
sample is analyzes for the total amount of
constituent present.
• The difference in the results from sample with
and without added standard is calculated.
• Satisfactory recovery gives the confidence of
accuracy of result.
• This procedure is especially appiled to
physicochemical processes, as polarography
and spectroscopy
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7. Internal standards
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8. Isotopic dilution
• It consists in adding a known amount of pure
component containing a radioactive isotope to
the unknown, now the element so isolated is
obtained in pure form usually as a compound
• It activity is determined with help of an
electroscope.
• The activity is compared with the added
element.
• The weight of element in the unknown sample
can than be calculated.
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7. Amplification method
• It is used when a very small amount of
material is to be measured which is
beyond the limit of the apparatus.
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ACCURACY AND PRECISION

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ACCURACY
• Near to the true value or standard value
is known as accuracy.
• Accuracy is the degree of agreement
between the measured value and true
value or its refers to the closeness of a
single measurements to its true value.
• Accuracy express the correctness of a
measurement.
• Accuracy is inversely proportional to
error
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• There are two analyst A and B, who

determine the % of the paracetamol in the
same brand of tablet the standard value
of paracetamol in that tablet is 100% and
observations are given below
Analyst A – 99.80, 99.90,100.O,99.30
Analyst B- 98.5,98.8,98.80,99.0
Who has done more accurate analysis .
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• Methods of determination of accuracy

The 2 methods ways of determining the
accuracy
1. Absolute method
2. Comparative method
Absolute method/ absolute error

The difference between and true value and
measured value is known as absolute error.
absolute Error = true value - observed value
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Comparative method/ relative error

the absolute error or mean error expressed
percentage of true value known as relative
error
Relative error (in pph)= absolute error

×100
true value
Relative error (in ppt)= absolute error
×1000
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• The result of an analysis are found

to be 36.89% compared with the
true value of 36.98% what will be
absolute and relative error.
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PRECISION
• Precision describe the reproducibility of
results.
• It is defined as the concordance of a
series of measurements of the same
quantity.
• It is the repeatability of a result
• So the term precision refers to nearness
between several measurement of the
same quantity.
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• Repeatability-Analyst made the

determinations on the same day would be
defined as repeatability.
• Reproducibility- Analyst made the
determinations on separate day (condition
may vary) defined as Reproducibility.
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• The three terms which are used to

describe the precision of a set of replicate
data.
1. Standard deviation:- it is the root mean
square deviation from mean
2. Variance:- square of standard deviation
3. co-efficient of variation:- standard deviation ×
100%
mean
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Significant figure
• Significant figures are the number of
digits in a value that defines the degree of
accuracy of the value .
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Rule of Significant figure

1. All non zero digits are significant
eg: 1234= 4
1.234= 4
0034544=5
2. Zero between two non zero digits are
significant
eg: 1042= 4
10.02=4
1.0015= 5
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3.Initial zero or leading zero are never
significant
eg: 0412= 3
0.012= 2
0309= 3
0.002 =1
4.Ending zeros or tailing zeros are
significant if they appear after decimal
Eg: 1.0020= 5
200= 1
0200=1
030.00=4
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5. order of magnitude is never significant

eg: 2.0× 103 = 2
2 × 103 = 1
6. Pure numbers or constants have infinite
significant number.
eg : cube area =1cm2 = infinite significant number
gravity on earth 9.8m/s2 = infinite significant
number
7. While changing units, no. of significant figure
remain same.
Eg: 2.0 Km =2
2.0 × 103 m= 2
1.5 m= 2
150 cm=2
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Work
• 800.1=
• 0800.10=
• 800=
• 80=
• 4.0× 103 =
• 200.00=
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1

absolute Error = true value - observed value

• If a tablet contains 500mg of paracetamol

• 6. Calculation error – Due to wrong

DETERMINATE ERROR/ SYSTEMATIC

1. Calibration of apparatus and

2. Running a blank determination

4. Use of independent methods of

6. Standard addition/ recovery

ACCURACY AND PRECISION

• There are two analyst A and B, who

• Methods of determination of accuracy

Absolute method/ absolute error

Comparative method/ relative error

Relative error (in pph)= absolute error

• The result of an analysis are found

• Repeatability-Analyst made the

• The three terms which are used to

Rule of Significant figure

5. order of magnitude is never significant

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