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How reliable are our data?

Data of unknown quality are useless!

Analyse accurately known standards

Perform statistical tests on data

Mean

Defined as follows:

x =

xi

i=1

measurements

Median

The middle result when data are arranged in order of size (for even

numbers the mean of middle two). Median can be preferred when

there is an outlier - one reading very different from rest. Median

less affected by outlier than is mean.

Precision

Relates to reproducibility of results..

How similar are values obtained in exactly the same way?

Useful for measuring this:

Deviation from the mean:

d i xi x

Accuracy

Measurement of agreement between experimental mean and

true value (which may not be known!).

Measures of accuracy:

Absolute error: E = xi - xt (where xt = true or accepted value)

Relative error:

x x

t 100%

E i

r

x

t

Data

Three types:

(1) Random (indeterminate) Error

Data scattered approx. symmetrically about a mean value.

Affects precision - dealt with statistically (see later).

(2) Systematic (determinate) Error

Several possible sources - later. Readings all too high

or too low. Affects accuracy.

(3) Gross Errors

Usually obvious - give outlier readings.

Detectable by carrying out sufficient replicate

measurements.

1. Instrument Error

Need frequent calibration - both for apparatus such as

volumetric flasks, burettes etc., but also for electronic

devices such as spectrometers.

2. Method Error

Due to inadequacies in physical or chemical behaviour

of reagents or reactions (e.g. slow or incomplete reactions)

Example from earlier overhead - nicotinic acid does not

react completely under normal Kjeldahl conditions for

nitrogen determination.

3. Personal Error

e.g. insensitivity to colour changes; tendency to estimate

scale readings to improve precision; preconceived idea of

true value.

constant (e.g. error in burette reading less important for larger values of reading) or

proportional (e.g. presence of given proportion of

interfering impurity in sample; equally significant

for all values of measurement)

Minimise instrument errors by careful recalibration and good

maintenance of equipment.

Minimise personal errors by care and self-discipline

Method errors - most difficult. True value may not be known.

Three approaches to minimise:

analysis of certified standards

use 2 or more independent methods

analysis of blanks

The equation for must be modified for small samples of data, i.e. small N

N

2

(

x

x

)

i

i 1

N 1

1.

2.

Reason is that in working out the mean, the sum of the

differences from the mean must be zero. If N - 1 values are

known, the last value is defined. Thus only N - 1 degrees

of freedom. For large values of N, used in calculating

, N and N - 1 are effectively equal.

(suitable for calculators)

N

( xi ) 2

i 1

( xi 2 )

i 1

N 1

Note: NEVER round off figures before the end of the calculation

VARIANCE:

N

s2

2

2

(

x

x

)

i

i 1

N 1

(or RELATIVE STANDARD DEVIATION):

Divide the standard deviation by the mean value and express as a percentage:

s

CV ( ) 100%

x

the % of selenium in foods. 9 measurements

were made on a single batch of brown rice.

Sample

1

2

3

4

5

6

7

8

9

0.07

0.07

0.08

0.07

0.07

0.08

0.08

0.09

0.08

xi

0.69

Standard deviation:

xi2

0.0049

0.0049

0.0064

0.0049

0.0049

0.0064

0.0064

0.0081

0.0064

xi2=

0.0533

0.0533 0.0529

0.00707106 0.007

9 1

CONFIDENCE LIMITS

CONFIDENCE INTERVAL

the magnitude of the confidence limits

CONFIDENCE LEVEL

fixes the level of probability that the mean is within the confidence limits

DetectionofGrossErrors

Asetofresultsmaycontainanoutlyingresult

outoflinewiththeothers.

Shoulditberetainedorrejected?

Thereisnouniversalcriterionfordecidingthis.

OnerulethatcangiveguidanceistheQtest.

Considerasetofresults

TheparameterQexpisdefinedasfollows:

Qexp x q xn /w

wherexq = questionableresult

xn = nearestneighbour

w = spreadofentireset

QexpisthencomparedtoasetofvaluesQcrit:

Qcrit (reject if Qexpt > Qcrit)

No. of observations

90%

95%

99% confidencelevel

3

0.941

0.970

0.994

4

0.765

0.829

0.926

5

0.642

0.710

0.821

6

0.560

0.625

0.740

7

0.507

0.568

0.680

8

0.468

0.526

0.634

9

0.437

0.493

0.598

10

0.412

0.466

0.568

RejectionofoutlierrecommendedifQexp>Qcritforthedesiredconfidencelevel.

Note:1.

Thehighertheconfidencelevel,thelesslikelyis

rejectiontoberecommended.

2.Rejectionofoutlierscanhaveamarkedeffectonmean

andstandarddeviation,esp.whenthereareonlyafew

datapoints.Alwaystrytoobtainmoredata.

3.Ifoutliersaretoberetained,itisoftenbettertoreport

themedianvalueratherthanthemean.

of Outliers

the concentration of nitrite ions in a sample

of river water: 0.403, 0.410, 0.401, 0.380 mg/l.

Should the last reading be rejected?

But Qcrit = 0.829 (at 95% level) for 4 values

Therefore, Qexp < Qcrit, and we cannot reject the suspect value.

Suppose 3 further measurements taken, giving total values of:

0.403, 0.410, 0.401, 0.380, 0.400, 0.413, 0.411 mg/l. Should

0.380 still be retained?

But Qcrit = 0.568 (at 95% level) for 7 values

Therefore, Qexp > Qcrit, and rejection of 0.380 is recommended.

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