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Group 3

Andi Tenri Nurwahidah

Nining Sintia Dewi

Dewi Puspita

Hamdan Hidayat

CHEMISTRY DEPARTMENT

MATH AND NATURAL SCIENCE FACULTY

HALU OLEO UNIVERSITY

KENDARI

2015

Analytical Standards and Calibration

Curves

that require some form of calibration

before use in quantitative analysis.

Although not the only way, a very

important and popular method for

this calibration is by means of a

graph

6.1 Simple Linear

Function

The general equation for a linear function, expressed in

concentration terms is given by Eq. 6.1a.

Y mC b

(6.1a)

C = concertration of analyte

m = proportionally constant

b = a constant term (often considered as the

experimental blank value)

sample, following an estabilished procedur, but where the

analyte was not added to the sample.

Fig.6.1a shows Eq.6.1a in graphical terms

function

The proportionalty constant m is goven by the slope

of the graph illustrated in Fig. 6.1a and ca be

calculated as below.

m tan MN LM

(6.1b)

relate these the scale on youre axes, and do not

measure purely in terms of distance.

mC b plot for an

analytical method obeying the equation

Calculate the slope of the line.

From Fig. 6.1b as labelled

definite value and which can be allowed for during the analysis. They may be

caused by the analyst, the instrument, or the method.

In a colorimetric determination of formaldehyde (methanal) the following

result were used to construct a calibration graph :

(g)

0 0.036

20.0 0.154

40.0 0.273

60.0 0.389

80.0 0.507

100.0 0.626

In order to see if there a determinate error the blank value must be subtraced

from all the sample values and then a graph of corrected absorbance against

mass of formaldehyde should be constructed.

(g)

20.0 0.118

40.0 0.237

60.0 0.353

80.0 0.471

100.0 0.590

Fig.6.1c identification of determinate error

As all of the points lie on straight line which can be extrapolated through the

origin, the method has been shown, within wxperimental error, to have no

determonate error. In fact equation now becomes that originally shown in Eq.

5.3b.

mC a

Ie

It should be obvious that a positive intercept may arise from the presence of

the analyte in the reagents used in the analytical method. It may be less

obvious how a negative intercept can be occur. One way, is in

spectrophotometric measurment on solutions, when unmatchedd cells are

used the reference cell absorbs more rediation than the sample cell.

SAQ 6.1a

Indeterminate error is errors that arise from uncertainties in a

measurement, they are unknown and cannot be cntrolled by the

analyst. The effect will produce a scatter of result for replicate

measurements which can be assesed only by statistical test.

comprehensive description and discussion

6.1.1. Linear Regression Analysis

The simplest procedure for linear regeression analysis is

that known as the method of least squares.

It use a mathematical formula to calculate the values of

m and b in our equation, given that we have a set of

data relating Y to C. The two values are calculated by

using Eqs. 6.1c and 6.1d below :

C Y n CY

m ...........(6.1c)

( C ) 2 n C 2

2 Y

C Y C

b ............(6.1d )

( C 2 ) n C 2

= the sum of the designated functions of all of its n

result

When applying the method of least squaresyou will

make a number assumptions

measured parameter Y and the analyte concentration C.

That no significant error exist in the composition of the

standard or in C. Thus the deviation of the points from

an exact straight line are entirely due to the

indeterminate error in the value of Y.

That there are no pieces of data, which fall outside the

normal statistical pattern, included in the calibration.

These pieces of bad data, as they arre sometimes

called, should be rejected, either after visual

examination or after the use of statistical tests (see

ACOL Unit : Measurement, Statistics and Computation).

The accuracy of a least-squares fit is a function of the

number of data-points used in the calibration. A m

inimum of six points is recommended. However in this

unit, to reduce the tedium of the calibration, fewer

result than the recommended number have been used.

The set of data listed in the table below relates to an

analytical method obeying the following linear

relationship.

Y mC b Y C

0.33 4.0

0.50 8.0

For example :

0.75 12.0

093 16.0

Compare the two straight lines

Looking at Eq. 6.1c and 6.1d we see that the values

we need to calculate initially are :

C 2 , CY

and then :

Y C C2 CY

0.33 4 16 1.32

0.50 8 64 4.00

0.75 12 144 9.00

0.93 16 256 14.88

2

Y = 2.51 C = 40 C = 480 CY = 29.2

( C 2 ) 1600

n4

(40 x 2.51) (4 x 29.2) (40 x 29.2) (480 x 2.51)

m b

1600 (4 x 480) 1600 (4 x 480)

100.4 116 .8 1168 1204.8

1600 1920 1600 1920

16.4 36.8

320 320

0.115

0.051

In order to construct the best straight line by using

these values we return to the equation for that

line, ie Y mC b

We select the maximum value of C used in the

calibration (ie C = 16), and calculate the value of Y

which corresponds to this value

We now have wo point through which we can

construct our straight line.

Y = 0.115, C = 0

Y = 0.93, C = 16

6.2 Non-Linear Calibration

Plots

Though most comparative obey a linear

relationship as ready described iin section 6.1. this

obedience to linearity is often own only over a

relatively small concentration range. Go outside

range and negative deviation may accur as

ilustrated in fig.

From zero concentration to concentration (X) the linearity iis

obeyed, but above concentration (X) the system is

showing negative deviation.

Curvature does not affect the validity of a calibration plot,

but does mean that more care must be taken in

preparation, by using more standards to predict the

curve accurately.

The effect of curvature in calibration plots is often met in

spectrophotometric methods involving emission or

absorption of radiation.

The curvature arises from instrumental features of from

chemical changes that occur t higher concentration and

will be fully explained in a later unit.

The main problem with analytical methods which exhibit

curved calibration plots is that method are not open to

abriged calibration, standard addition, or internal

standard procedure.

6.2.1 Transformation of Non-linear

into Linear Function

In analytical chemistry there are a number of

useful techniques where the function relating Y to

C is not initially linear,

aC

eg :

Y k10 ............(6.2a )

10 aY kC............(6.2b)

Where : Y =measured parameter

C = concentration

a and k are contants

Eq. 6.2a tell us that there is a reduction in the

parameter Y with increase in concenration, with

the opposite being true for Eq. 6.2b. The equation

are shown graphically in Fig. 6.2b.

Fig. 6.2b. Graphically representation of Eq. 6.2a and

6.2b

We can however, Create a linear relationship

from both of these equations by taking the logs of

both sides. Y k10 aC

Thus , taking logs for gives

log Y log k aC............(6.2c)

aY log k log C

10 aY kC

and taking logs for gives

aY log k log C............(6.2d )

ilustrated in Fig. 6.2c below.

Fig 6.2c. Graphically representation of Eq. 6.2c and

6.2d

The availability of modern scientific calculators has

simplified considerably calibration involving

logarithmic function and their subsequent

application.

The table below gives a set of calibration data for an

analytical method obeying the relationship.

Y k m log C

Concentration of Measured parameter

analyte, C (ppm) Y

100 0/150

200 0.173

300 0.186

400 0.195

If a sample solution gave a value of Y of 0.179, what

was the concentration of the analyte in the sample ?

Page 123

Are told that the relationship is that Y is

proportional to log must first calculate log C

C log C Y

100 2.00 0.150

200 2.30 0.173

300 2.48 0.186

400 2.60 0.195

We can now plot a Y vs log C graph

From our graph we can

now find the log C

value corresponding to

a Y value of 0.179. This

is log C = 2.38(5)

this we can obtain C

Antilog of 2.38(5) = C

= 243

SAQ 6.2a

An analytical method is known to obey the

relationship

Y be mC

Does this method exhibit a relationship where by either

(i) Y increases with increasing concentration

(ii) Y decreases with increasing concentration

thought to obey the experimentalrelationship quoted above

SAQ 6.2a

Y C

2,26 2,00

1,97 4,00

1,67 6,00

1,45 8,00

1,23 10,00

SAQ 6.2a

What are you conclusions regarding this hypothesis ?

s the hypothesis

i)Definitely true

ii)Probably true

iii)Definitely false

iv)Probably false ?

THANK YOU

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