General Steps in a Chemical Analysis
Introduction
The analytical process often begins with a question that is not phrased in terms of a chemical analysis. The question could be "Does lead in petrol enter our food supply?" or "Is this water safe to drink?" or "Does emission testing of automobiles reduce air pollution?" A scientist translates such questions into the need for particular measurements. An analytical chemist then must choose or invent a procedure to carry out those measurements,When the analysis is complete, the analyst must translate the results into terms that can be understood by others preferably by the general public. A most important feature of any results is its limitations. What is the statistical uncertainty in reported results? If you took samples in a different manner, would you obtain the same results? Is a tiny amount (a trace) of analyte found in a sample really there or is it contamination? Once all interested parties understand the results and their limitations, then they can draw conclusions and reach decisions.
The Process
Formulating the question
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1.
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Translate general questions into specific questions
amenable to being answered through chemical measurements.
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Selecting analytical procedures
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2.
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Search the chemical literature to find appropriate
procedures or, if necessary, develop original procedures to make the required
measurements.
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Sampling
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3.
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Obtain a representative bulk sample from the lot.
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4.
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Extract from the bulk sample a homogeneous laboratory
sample.
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Sample preparation
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5.
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Convert the laboratory sample into a form suitable for
analysis, which usually means dissolving the sample. Samples with a low
concentration of analyte may need to be concentrated prior to analysis.
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6.
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Remove or mask species that interfere with the chemical
analysis.
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Analysis
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7.
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Measure the concentration of analyte in several aliquots.
The purpose of replicate measurements (repeated measurements) is to assess
the variability (uncertainty) in the analysis and to guard against a gross
error in the analysis of a single aliquot. The uncertainty of a measurement
is as important as the measurement itself, because it tells us how reliable a
measurement is. If necessary, use different analytical methods on similar
samples to make sure that each method gives the same result and that the
choice of analytical method is not biasing the result. You may also wish to
construct and analyse several different bulk samples to see what variations
arise from your sampling procedure.
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Reporting and interpretation
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8.
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Deliver a clearly written, complete report of your
results, highlighting any special limitations that you attach to them. Your
report might be written to be read only by a specialist (such as your
instructor), or it might be written for a general audience (such as your
mother). Be sure the report is appropriate for its intended audience.
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Drawing conclusions
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9.
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Once a report is written, the analyst might or might not
be further involved in what is done with the information, such as modifying
the raw material supply for a factory or creating new laws to regulate food
additives. The more clearly a report is written, the less likely it is to be
misinterpreted by those who use it. The analyst should at least have the
responsibility to ensure that conclusions drawn from his or her data are
consistent with the data.
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