MODULE 2

Lesson 1: Steps and tools in a typical quantitative

analysis

Introduction

A quantitative analytical process follows different steps and procedures. In this module
you will learn about the steps in conducting analysis, sampling techniques and statistical
treatment of your data.

Module Learning Outcomes

● Be familiar with the different steps in a typical quantitative analysis.

● Be aware of different protocols in sampling and of factors that must be
considered in selecting an analytical method.
● Identify possible sources of errors associated with the different steps in
quantitative analysis.

In the previous module you learned the definition, divisions, scope and
importance of analytical chemistry. In this subject our main focus is quantitative
analytical chemistry thus in this module we will focus our discussion on quantitative
analysis.

What are the steps in a typical quantitative analysis?

A quantitative analysis, involves several steps and procedures. These are:

1. Selecting a method of analysis

The first step in any quantitative analysis is the selection of an appropriate method for
the analysis. The choice of method is based on the complexity and the number of
components in a sample. The following are also given consideration when choosing a
method:
a. Skills and training of the analyst
b. Availability of equipment, instruments and facilities
c. Required sensitivity and precision of analysis
d. Cost and budget
 e. Time for analysis/how soon are the results needed
2. Sampling
Sampling is a procedure whereby a part of a substance, material or product is taken
to provide for testing or calibration a representative sample of the whole (ISO / IEC
17025).

Considerations during sampling:

· Analysis is usually performed on only a small portion of the material to be

characterized.

· If the amount of the material is very small and it is not needed for future use, then
the entire sample maybe used for analysis.

· More often, the characterized materials must be altered as little as possible in

sampling.

· Materials to be sampled maybe liquid, solid or gas.

· For samples with homogeneous composition- a sample “grab sample” taken at

random will suffice for analysis.

· For samples with heterogeneous composition- may be interested in the variation

throughout the sample, hence several individual samples may be required.

· If gross composition is needed, need to obtain a gross sample that will be later
reduced to a laboratory sample.

· In case of biological liquids, conditions under which the sample is collected can be
important; preservative added to it like anticoagulants may affect a particular analysis.

· Certain precaution could be taken in handling in storing samples to prevent or

minimize contamination, loss, decomposition, or matrix change.

· Stability of samples is affected by light, atmosphere, and container.

Example:
1. Blood samples to be analyzed for CO2 must be protected from the
atmosphere.
 2. Glucose is unstable, thus preservative such as NaF must be added
to blood sample.
3. Urine samples are unstable, calcium phosphate precipitates out
entrapping metals or ions of interest, hence urine should be kept acidic
(pH=4.5) by adding 1 or 2ml of glacial acetic acid.
4. Corrosive sample will often react with the container.

3. Preparing a laboratory sample for analysis

· In preparing the samples, the first thing that must be done is to measure the amount
(volume or weight) of the sample.

· Solid samples are often analyzed on a dry basis and must be dried in an oven, and
cooled in a dessicator prior to weighing.

· Organic materials that are to be analyzed for inorganic substituents maybe

destroyed by dry ashing, or wet digestion by heating with oxidizing agent.

Examples:
a. pH is adjusted
b. reagent is added to mask
interference
c. analyte is converted to a form
suitable for measurement or
separation

4. Defining replicate samples

Replication is important since it improves the quality of results and measures the
reliability. Since solvent and reagent used for dissolution may contain trace impurities, it
is important to prepare and analyze replicate blanks. A blank consist of all chemicals
used in an analysis in the same amounts; run though the entire analytical procedure.
The blank result is subtracted from the analytical sample result.
 5. Preparing solutions of the sample
Most quantitative analyses are conducted using solutions thus in preparing solutions
of the sample, the chosen solvent should dissolve the sample completely and
rapidly.

6. Performing necessary chemical separation and eliminating interferences:

Separation steps are necessary to:

a. Eliminate interference
b. Provide suitable selectivity in the measurement
c. Preconcentrate the analyte for more sensitive or
accurate measurement.
Separation steps may include:
a. Precipitation
b. Extraction into an immiscible solvent
c. Chromatography
d. Dialysis
e. Distillation

7. Performing the measurement

8. Calculation and interpretation of the result

· The result obtain from the final measurements are used to calculate
the amount of analyte in the original sample.
· Analyte should be critically evaluated whether the result are
reasonable and relate to the analytical problem as original stated.

References

1. Holler, Skoog and Crouch. (2007) Principles of Instrumental Analysis, 6th ed.,
Brooks Cole.
2. Handbook of Instrumental Techniques for Analytical Chemistry. (1997) Ed. Settle,
F., Prentice-Hall.
3. Kealy, D. and Haines, P.J. (2002) Instant Notes in Analytical Chemistry. BIOS
Scientific Publishers Limited.
4. Skoog, West, Holler and Crouch. (2003) Fundamentals of Analytical Chemistry,
8th ed., Brooks Cole (or latest edition).