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You are on page 1of 25

ANALYTICAL CHEMISTRY

CCB 2073

Sept 2013

M Azmi Bustam

Learning Outcomes

Students should be able to:

1. Understand the principle of analytical chemistry, analytical

methodology and apply the statistic method in data handling

for reliability and significant derived results.– PO 1 and PO2

2. Describe the procedures and applications of analytical

techniques within the area of gravimetric. PO 1 and PO2

3. Explain the basic principles and analyze the data generated by

using spectrophotometric, spectroscopic and chromatographic

method of analysis. PO 1 and PO2

4. Apply the knowledge of analytical and associated data handling

and processing skills in a series of laboratory experiments. PO

1 and PO 2

M Azmi Bustam

Chapter Outcomes

Students should be able to:

1. Understand the principle of analytical chemistry, analytical

methodology and apply the statistic method in data handling

for reliability and significant derived results.– PO 1 and PO2

M Azmi Bustam

Chapter 1(cont….)

Calibration

Introduction

M Azmi Bustam

Calibration

- Method to determine the relationship

between the analytical response and the

analyte concentration.

Introduction

M Azmi Bustam

Calibration

- Method to determine the relationship

between the analytical response and the

analyte concentration.

Calibration Techniques

1. Calibration Curve Method

2. Standard Additions Method

3. Internal Standard Method

Calibration Curve Method

1. Most convenient when a large

number of similar samples are to be

analyzed.

2. Most common technique.

3. Facilitates calculation of Figures of

Merit.

Calibration Curve Procedure

1. Prepare a series of standard solutions

(analyte solutions with known

concentrations).

2. Plot [analyte] vs. Analytical Signal.

3. Use signal for unknown to find

[analyte].

Example: Pb in Blood by

GFAAS

[Pb] Signal

(ppb) (mAbs)

0.50 3.76

1.50 9.16

2.50 15.03

3.50 20.42

4.50 25.33

5.50 31.87

Results of linear regression:

S = mC + b

m = 5.56 mAbs/ppb

b = 0.93 mAbs

0

5

10

15

20

25

30

35

0 1 2 3 4 5 6

Pb Concentration (ppb)

m

A

b

s

y = 5.56x + 0.93

Standard Addition Method

1. Most convenient when a small

number of samples are to be

analyzed.

2. Useful when the analyte is present

in a complicated matrix and no ideal

blank is available.

Standard Addition

Procedure

1. Add one or more increments of a standard

solution to sample aliquots of the same

size. Each mixture is then diluted to the

same volume.

2. Prepare a plot of Analytical Signal versus:

a) volume of standard solution added, or

b) concentration of analyte added.

Standard Addition

Procedure

3. The x-intercept of the standard addition

plot corresponds to the amount of analyte

that must have been present in the sample

(after accounting for dilution).

4. The standard addition method assumes:

a) the curve is linear over the concentration range

b) the y-intercept of a calibration curve would be

0

Example: Fe in Drinking Water

Sample

Volume

(mL)

Standard

Volume

(mL) Signal (V)

10 0 0.215

10 5 0.424

10 10 0.685

10 15 0.826

10 20 0.967

The concentration

of the Fe

standard solution

is 11.1 ppm

All solutions are

diluted to a final

volume of 50 mL

-0.2

0

0.2

0.4

0.6

0.8

1

1.2

-10 -5 0 5 10 15 20 25

Volume of standard added (mL)

S

i

g

n

a

l

(

V

)

-6.08 mL

[Fe] = ?

x-intercept = -6.08 mL

Therefore, 10 mL of sample diluted to 50 mL

would give a signal equivalent to 6.08 mL of

standard diluted to 50 mL.

V

sam

x [Fe]

sam

= V

std

x [Fe]

std

10.0 mL x [Fe] = 6.08 mL x 11.1 ppm

[Fe] = 6.75 ppm

Internal Standard Method

1. Most convenient when variations in

analytical sample size, position, or

matrix limit the precision of a

technique.

2. May correct for certain types of

noise.

Internal Standard Procedure

1. Prepare a set of standard solutions

for analyte (A) as with the calibration

curve method, but add a constant

amount of a second species (B) to

each solution.

2. Prepare a plot of S

A

/S

B

versus [A].

Notes

1. The resulting measurement will be

independent of sample size and

position.

2. Species A & B must not produce

signals that interfere with each

other. Usually they are separated by

wavelength or time.

Example: Pb by ICP Emission

Each Pb solution contains

100 ppm Cu.

[Pb]

(ppm) Pb Cu Pb/Cu

20 112 1347 0.083

40 243 1527 0.159

60 326 1383 0.236

80 355 1135 0.313

100 558 1440 0.388

Signal

No Internal Standard Correction

0

100

200

300

400

500

600

0 20 40 60 80 100 120

[Pb] (ppm)

P

b

E

m

i

s

s

i

o

n

S

i

g

n

a

l

0.000

0.050

0.100

0.150

0.200

0.250

0.300

0.350

0.400

0.450

0 20 40 60 80 100 120

[Pb] (ppm)

P

b

E

m

i

s

s

i

o

n

S

i

g

n

a

l

Internal Standard Correction

Results for an unknown sample after

adding 100 ppm Cu

Run Pb Cu Pb/Cu

1 346 1426 0.243

2 297 1229 0.242

3 328 1366 0.240

4 331 1371 0.241

5 324 1356 0.239

mean 325 1350 0.241

σ 17.8 72.7 0.00144

S/N 18.2 18.6 167

Signal

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