STKK1702

Kimia Analisis Asas

Dr Sharina Abu Hanifah
Bilik 2132 Paras 2, Bangunan Kimia
03-89213902
sharina@ukm.edu.my

 Everything is made of chemicals.

Analytical chemists determine what and how much!

 Concern with the chemical characterization of matter and

the answer to two important questions:
1) What is it (qualitative)
2) How much is it (quantitative)

 Applications:
nitrogen content of a fertilizer determines its value.
Food must be analyzed for contaminants (pesticide
residue) and for essential nutrients (vitamin content).
Blood glucose must be monitored in diabetics.
The presence of trace elements from gun powder on
a murder defendants hand will prove a gun was
fired.

What is Analytical Chemistry?

The Division of Analytical Chemistry of the American
Chemical Society (ACS) provides a comprehensive
definition of analytical chemistry, which may be found on
their website.
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Analytical Chemistry seeks ever improved means of measuring the

chemical composition of natural and artificial materials.
The techniques of this science are used to identify the substances
which may present in a material and to determine the exact amounts
of the identified substance.
Analytical chemists work to improve the reliability of existing
techniques to meet the demands for better chemical measurements
which arise constantly in our society.

 They adapt proven methodologies to new kinds of materials or to

answer new questions about their composition and their reactivity
mechanisms.
Needs of many fields:
Medicine: basis for clinical laboratory tests which help physicians
diagnose disease and chart progress in recovery.
Industry: means of testing raw materials and for assuring the quality
of finished products whose chemical composition is critical.
Household products such as fuels, paints, pharmaceuticals etc are
analyzed by the procedures developed by analytical chemists before
being sold to the consumer.
Environmental quality is often evaluated by testing for suspected
contaminants using the techniques of analytical chemistry.
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 Nutritional value of food is determined by chemical analysis for

major components such as protein and carbohydrates and trace
components such as vitamins and minerals.

Qualitative and Quantitative Analysis: What

does each tell us?

 Discipline of analytical chemistry consists of qualitative analysis and

quantitative analysis.
Deals with the identification of elements, ions, or compounds
present in a sample then latter deals with the determination of how
much of one or more constituents is present.
Sample may be solid, liquid, gas or mixture.
The presence of gunpowder residue on a hand generally requires
only qualitative knowledge not of how much is there but the price of
coal will be determined by the percent of sulfur impurity present.

Qualitative tests
May be performed by selective chemical reactions or with the use of
instrumentation.
Certain chemical reactions will produce colors to indicate the
presence of classes of organic compounds for example ketones.
Infrared spectra will give fingerprints of organic compounds of their
functional groups.
Terms (selective vs specific):
a selective reaction or test is one that can occur with other
substances but exhibits a degree of preference for the substance of
interest.
A specific reaction or test is one that occurs only with the substance
of interest.
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Qualitative tests
** unfortunately few reactions are specific but many exhibit
selectivity. Selectivity may be achieved by a number of strategies.

Sample preparation (e.g extractions, precipitation)

Instrumentation (selective detectors)
Target analyte derivatization
Chromatography, which provides powerful separation

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Quantitative analysis
A history of the sample composition will often be known.
- it is known that blood contains glucose or else the analyst will have
performed a qualitative test prior to performing the more difficult
quantitative analysis.
Modern chemical measurement systems often exhibit sufficient
selectivity that a quantitative measurement can also serve as a
qualitative measurement.
However simple qualitative tests are usually more rapid than
quantitative procedures.

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Analytical process in general

Define the problem

Select a method

Obtain a representative
sample

Prepare the sample for

analysis

Calculate the results and report

Perform the measurement

Perform any necessary

chemical separations

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Define the problem

what do we really need to know (not necessarily everything).

Information: by whom?
For what purpose?
What type of sample?

The analyst must have good communication with the client.

The client may be the Environmental Protection Agency (EPA), an
industrial client, an engineer etc.
Each will have different criteria or needs and different understanding
of what a chemical analysis involves or means.
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 Analyte is the substance analyzed for. Its

concentration is determined.

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Define the problem

** The concept of safe or zero/nothing is one that is hard to define or
understand by many people.
Telling someone their water is safe is not for the analyst to say.
All you can do is present the analytical data. The client must decide
whether it is safe to drink, perhaps relying on other experts.

Also never report an answer zero but as less than the detection
limit which is based on the measurement device/instrument (ppm,
ppb, ppt).
We are limited by our methodology and equipment and that is all
that can be reported.
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 A law may be passed that there should be zero concentration of

chemical effluent in water.
In practice, the acceptable level is defined by how low a
concentration can be detected; and the very low detectability may be
far below the natural occurrence of the chemical or below the levels
to which it can be reasonably reduced.

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 Once the problem is defined:

- how much is needed?
- how sensitive the method must be?
- how accurate and precise?
- what separations may be required to eliminate
interferences?
The analytical method to be used will depend on factors such as:
1) analysts skills and training in different techniques
instruments
2) facilities, equipments and instruments available
3) sensitivity and precision required
4) cost and budget available
5) time for analysis and how soon results are needed.

and

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Obtaining sample is it solid, liquid or gas?

This process can be the most critical aspect of an analysis.
The significance and accuracy of measurements can be limited by
the sampling process.
Many professional societies have specified definite instructions for
sampling given materials. [American Society for Testing and
Materials (ASTM), American Public Health Association (APHA)].

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Drainage water sampling

Collecting water samples
Blood sample

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 The problem involves obtaining a sample that is representative of

the whole. This sample is called gross sample.
Once a representative gross sample is obtained, it may have to be
reduced to a sufficiently small size to be handled. This is called
sample.
Once the sample is obtained, an aliquot or portion of it will be
analyzed. This aliquot is called the analysis sample. Several
replicate analyses on the same sample may be performed by taking
separate aliquots.

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 1) Solids
2) Liquids

3) Gases

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 In the case of biological fluids, the conditions under which the

sample is collected can be important, for example whether a patient
has just eaten.
Composition of blood varies considerably before and after meals, for
many analyses a sample is collected after the patient has fasted for
a number of hours.
** certain precautions should be taken in handling and storing samples
to prevent or minimize contamination, loss, decomposition or matrix
change.

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Precautions!
In general must prevent contamination or alteration of the sample
by:
1) container
2) atmosphere
3) light
** the sample may have to be protected from atmosphere or from light.

Alkaline substance for example, will react with CO2 in the air.
Blood samples to be analyzed for CO2 should be protected from the
atmosphere.

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Precautions!
The stability of the samples must be considered.
Example:
Glucose is unstable and a preservative such as sodium flouride is
added to blood samples.
The preservation must not interfere in the analysis.
Proteins and enzymes tend to denature on standing and should be
analyzed without delay.
Urine samples are unstable and calcium phosphate precipitates out,
entrapping metal ions or other substances of interest.
Precipitation can be prevented by keeping urine acidic (pH 4.5)
usually by adding 1 or 2 ml glacial acetic acid per 100-ml sample.
Store under refrigeration.
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Performing necessary chemical separations

In order to eliminate interferences, to provide suitable selectivity in
the measurement or to preconcentrate the analyte for more sensitive
or accurate measurement, the analyst must often perform one or
more separation steps.
It is preferable to separate the analyte away from the sample matrix,
in order to minimize losses of the analyte.
Separation steps: precipitation, extraction, into an immiscible
solvent, chromatography, dialysis and distillation.

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Performing the measurementselect a method

Analytical Chemistry. Gary D. Christian. Page 10-13

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Calculating the results and

reporting data
Once the concentration of analyte in the prepared sample solution
has been determined, the results are used to calculate the amount
of analyte in the original sample.
Either an absolute or a relative amount may be reported.
Replicate analyses can be performed (three or more) and a
precision of the analysis may be reported, standard deviation.
Acknowledge of the precision is important gives degree of
uncertainty in the result.

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As analyst, it is important to have good communication and

interaction with the customer about what the analysis
represents.

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