Steps and Tools in A Typical Quantitative Analysis
Steps and Tools in A Typical Quantitative Analysis
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.
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.
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).
· 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.
· 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.
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.
· 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.
Examples:
a. pH is adjusted
b. reagent is added to mask
interference
c. analyte is converted to a form
suitable for measurement or
separation
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.
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).