This Guide is concerned with the practice of qualitative analysis and contains invaluable advice for laboratories undertaking such work. It is designed to assist laboratories in establishing and maintaining a working regime that will minimise the risk of error and maximise the quality of the analytical information they produce. It is aimed primarily at laboratory managers and those responsible for any part of the analysis process from designing qualitative tests or deciding which tests to apply in particular cases to those performing the requisite experimental work. Qualitative Analysis has been developed using the knowledge and experience of an advisory panel drawn from a representative cross-section of practising analytical scientists. It was produced as part of the VAM Programme, and will be a useful guide for laboratory staff, government agencies, researchers and professionals in industry and academia alike.
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This guide is concerned with the practice of qualitative analysis and contains invaluable advice for laboratories undertaking such work. It is designed to assist laboratories in establishing and maintaining a working regime that will minimise the risk of error and maximise the quality of the analytical information they produce. It is aimed primarily at laboratory managers and those responsible for any part of the analysis process from designing qualitative tests or deciding which tests to apply in particular cases to those performing the requisite experimental work. Qualitative Analysis: A Guide to Best Practice has been developed using the knowledge and experience of an advisory panel drawn from a representative cross-section of practising analytical scientists. It was produced as part of the VAM Programme, and will be a useful guide for laboratory staff, government agencies, researchers and professionals in industry and academia alike.
1 This Document, 1,
2 The VAM Principles, 1,
3 Scope, 2,
4 Health and Safety, 3,
5 Establishing the Requirements, 3,
6 The Sample, 7,
7 The Analytical Process, 12,
8 Quality Assurance, 16,
9 Interpretation of Results, 20,
10 Analysis Report, 20,
11 Field Testing, 21,
12 Further Information, 21,
Appendix A: Requirements and Design Model, 22,
Appendix B: Bibliography, 23,
Qualitative Analysis: A Guide to Best Practice
1 This Document
This document is about principles of good practice in qualitative analysis. These principles are themselves related to one or more of the six VAM principles. In order to highlight this point, relevant VAM principles are indicated within square brackets at the beginning of each numbered section e.g. [VAM principle #1]. To assist the reader in locating the "Best Practice" principles, they are presented in italic with each one being further indicated by a finger sign in the left margin. Each statement of a principle is followed by some explanatory text which elaborates on the theme and may provide examples of why it is important.
The document as a whole is structured to follow the logical sequence of issues surrounding: health and safety; initial customer contact; samples; the analytical process; and quality assurance. A section on field testing is included to cover the important area of out of laboratory analyses.
2 The VAM Principles
The VAM Programme was set up with the aim of assisting analysts to obtain reliable analytical measurements. To facilitate this a set of six principles has been formulated and is widely publicised. The main focus of these principles, listed below, is on quantitative measurement but it is, of course, crucially important for the analyst to know the identity of whatever it is that he or she has measured. The word 'identity' in this context has a somewhat broad meaning; it could be the name of a single substance but equally it could be a descriptor for a recognised mixture of substances e.g. kerosene or lavender oil.
Apart from being a necessary prerequisite to quantitation, the determination of identity is also frequently the sole purpose of an analysis. The VAM principles are equally applicable whether analysis is being performed for quantitation or for identification.
The VAM principles are:
(1) Analytical measurements should be made to satisfy an agreed requirement.
(2) Analytical measurements should be made using methods and equipment which have been tested to ensure that they are fit for their purpose.
(3) Staff making analytical measurements should be both qualified and competent to undertake the task.
(4) There should be regular independent assessment of the technical performance of a laboratory.
(5) Analytical measurements made in one location should be consistent with those made elsewhere.
(6) Organisations making analytical measurements should have well defined quality control and quality assurance procedures.
Each of the following section headings contains, where appropriate, numbered references to one or more of the above six principles. These references are intended to be indicative only, pointing to the more obvious principles which apply. Some sections could be considered to be covered by several of the principles and, in any given case, the referenced principles should not necessarily be taken to deny the relevance of any of the principles not cited.
3 Scope
The Guide has been developed as a generic document and is intended to cover a broad area of application ranging from traditional analytical chemistry/clinical chemistry to the more subjective assessments arising from activities such as organoleptic testing and document examination. For the purpose of the Guide therefore, qualitative analysis is loosely defined as follows:
Definition Qualitative Analysis: The classification of objects against specified criteria to meet an agreed requirement.
In order to classify an object, in the present context, a sample of it must be made available to an analyst. The methods of classification are taken to consist of the determination of chemical or physical properties or inspection by visual or other sensory means. Some examples of classification methods are:
• Chemical tests involving colour changes, e.g. addition of Schiff's reagent to aliphatic aldehydes.
• Chemical tests involving production of precipitates, e.g. BaSO4 in testing for SO42-.
• Measurement of specific gravity.
• Observation of crystalline form or other morphological features.
• Observation of particular absorption bands in an IR spectrum.
• Limit tests in which the magnitude of a measured parameter is compared to a predetermined boundary value.
Where analysis is by reference to chemical species, all concentration levels are covered from macro to trace level.
4 Health and Safety
[VAM Principle #2, 3]
laboratory staff should be made aware of any potential dangers associated with the collection, analysis or storage of sample materials.
The health and safety of laboratory staff is of paramount importance and where samples are sent to a laboratory for analysis, the laboratory should ensure that it is aware of any relevant Health & Safety information connected with the sample material. This could include extracts from hazard information sheets supplied by the customer for example.
Laboratories should have a hazard assessment policy to cover all materials received; this should cover reagents as well as sample materials. All material entering a laboratory should be assigned to a predefined hazard/toxicity class upon arrival. Materials of unknown or partially known composition should automatically be assigned to high hazard/toxicity classes.
When laboratory staff collect their own samples the host organisation has a duty to ensure that such visitors are aware of any hazards connected with the environment from which the samples are collected. That is to say, from other chemicals, biological organisms or sources of electrical, kinetic, or radiative energy.
For their part, laboratory field personnel have an obligation to inform a responsible person in the host organisation if they discover, whether as a result of their tests or otherwise, that a toxic threshold has been exceeded or that a hazard or potential hazard exists in the area in which they have been working (see Section 8 on Field Testing).
5 Establishing the Requirements
5.1 An Agreed Requirement
[VAM Principle #1]
The analyst and customer should agree on the business requirement and the technical solution.
The kind of information (chemical/physical/observational) to which this Guide relates will usually be required in order to enable the user to decide between alternative courses of action. For example:
• An industrial customer may wish to know if an impurity is present in a process feed stock so that he can avoid using it if it might poison a catalyst.
• In order to direct the course of an investigation, a police officer may wish to know if samples taken at the scene of a crime match those associated with a...
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