Introduction Introduction
Analytical Chemistry. Analytical chemistry can be broken down in to
two general areas of analysis:
The branch of chemistry that deals with the
separation, identification and determination of Qualitative analysis
components in a sample. Attempting to identify what materials are
present in a sample.
It also traditionally includes coverage of
Quantitative analysis
chemical equilibrium and statistical treatment
of data. Determining how much of a material is
present in a sample.
Introduction Types of methods
As we review the various methods, we’ll see that Many approaches can and have been taken.
some are primarily qualitative tools and others
Gravimetry
are used for quantitative work.
Methods based on a measured weight.
Many methods offer both types of information.
Titrimetry
Example - GC/MS (qual and quant info) Methods based on a measured volume.
This method includes both a separation tool Electrochemical
(Gas Chromatography) and a spectral method Approaches that rely on measurement of
(Mass Spectrometry). The combination is a potential, current, resistance, charge, ...
very powerful method.
Types of methods Quantitative analysis
Spectral methods A large portion of this course deals with methods
Interaction of an analyte with EM radiation. that are used to determine how much of a
material is present.
Chromatography
Separation of a material due to its interaction We need to review the general steps that are
with two different phases. taken for any quantitative method.
Chemometrics These steps are taken to insure an accurate
The statistical treatment of data. and reliable answer.
Quantitative analysis Quantitative analysis
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What type of information do you need? Partial analysis
Determining one or a limited number of
Complete analysis species in a sample.
The goal is to determine the amount of each
component in a sample. This is the most common approach.
Examples
Ulitmate analysis Iron in an ore sample
The amount of each element present without Electrolyte levels in blood
regard to actual composition Presence of lead in a water sample
Basic steps in an analysis Technique to be used
Prior to even starting an assay, one must Factors to consider
consider several factors. Accuracy and sensitivity
Technique to be used Cost
Number of samples to be assayed
Sampling and sample preparation
Number of components in a sample.
Proper application of the method
Data analysis and reporting The approach you take must produce the results
you require in a timely, cost effect manner -
All of these together are what comprise an primarily determined by the type of sample you
analytical method. have.
Samples Samples
Must be representative. Sample selection
Steps must be taken to insure that your results Requires some knowledge as to sample
reflect average composition. source and history.
Example - Determination of iron in an ore.
One common approach is to select several
Minerals and ores are heterogeneous. To random samples for analysis.
assay any single sample may not yield valid
Powder the samples
results for an entire sample ‘lot.’
Blend the powders
Proper sample selection and preparation can
Select a fraction for assay
help minimize this problem.
Sample preparation Sample replicates
One must then convert the sample to a form All methods have errors associated with them.
suitable for the method of analysis.
Using multiple samples and replicates helps
Based on the method, this may include: track and identify this error.
Drying to insure an accurate weight. Multiple samples
Sample dissolution. - identically prepared from another source.
- used to verify if your sampling was valid.
Elimination or masking of potential
interferences. Replicate samples
Conversion of analyte to a single or - splits ofthe same sample.
measurable form. - helps track and identify errors in method.
We must establish the relationship between
For most methods, we measure a response that measured response and concentration of our
is proportional to the concentration of our analyte.
analyte. Canalyte = f(x)
Gravimetric - Weight of a precipitate. where
Canalyte = concentration
Titration - Volume of a titrant required. X = technique response.
Spectrophotometric - light absorbed. Most methods attempt to make f(x) a linear relationship
Canalyte = mX + b
Chromatographic - peak area.
Calibration Results
To establish this relationship, we must use one or Once your response has been obtained, the final
more standards - calibration. step is to calculate your results.
Standards should be
Prepared identically to the sample This will include
Application of you standard curve.
Have a similar composition I matrix
Prepared over the range that is expected for Estimation of error based on replicates.
our samples.
The number and type of standards is method
Reporting in a standard, usable format.
dependent.
Each method includes many steps that one must
consider before doing even one analysis.
Each is dependent on the technique to be used,
the type of sample and the desired results.
As we discuss each method, we’ll consider these
factors and how to best address them.