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Sample preparation
In analytical chemistry, sample preparation refers to the ways in which a sample is treated prior to its analyses. Preparation is a very important step in most analytical techniques, because the techniques are often not responsive to the analyte in its original form, or the results are distorted by interfering species. Sample preparation may involve:
(a) Dissolution,
(b) Extraction,
(c) Reaction with some chemical species,
(d) Pulverizing,
(e) Treatment with a chelating agent (e.g. EDTA)
(f) Masking,
(g) Filtering,
(h) Dilution,
Sub-sampling or many other techniques.
Treatment is done to prepare the sample into a form ready for analysis by specified analytical equipment. Sample preparation could involve:
(a) Crushing and dissolution,
(b) Chemical digestion with acid or alkali,
(c) Sample extraction,
(d) Sample clean up
(e) Sample pre-concentration.
SAMPLE TREATMENT PROCEDURES
Sample preparation includes all of the steps taken in the laboratory to render a sample into a form that is suitable for chemical analysis. Correct sample preparation results in sub-samples that are representative of the total sample.
Many of the samples received in laboratories are not in a form that can readily be analyzed i.e. are either not fine or wet ad may require subsequent treatment before they can be analyzed. The most common sample treatment methods include
Crushing and Grinding Samples
A certain amount of crushing and grinding is usually required to decrease the particle size of solid samples. However, some crushing or grinding operations tend to alter the composition of the sample, therefore care be taken not to reduce them no more than is required for homogeneity and ready attack by reagents.
Several factors can cause significant changes in sample composition as a result of grinding. The heat inevitably generated can cause losses of volatile components. In addition, grinding increases the surface area of the solid and thus increases its susceptibility to loss of its moisture and reactions with the atmosphere.
Differences in hardness of the component can also introduce errors during crushing and grinding. Softer materials are ground to fine particles more rapidly than are hard ones and may be lost as dust as the grinding proceeds. In addition, flying fragments tend to contain a higher fraction of the harder components.
Intermittent screening often increases the efficiency of grinding. Screening involves shaking the ground sample on a wire or cloth sieve that will pass particles of a desired size. Grinding must be continued until every particle has been passed if the screened sample is to have the same composition as it had before grinding and screening.
A serious contamination error can arise during grinding and crushing due to mechanical wear and abrasion of the grinding surfaces.
Several different tools can be used for reducing the particle size of solids, including jaw crushers and disk pulverizers for large samples containing large lumps, ball mills for medium-sized samples and particles, and various types of mortars for small amounts of material
Organic samples can be reduced in size with a macerating hammer mill. This makes organic material easier to homogenize and makes representative sub-sampling easier.
Once selected, a sample that represents the properties of the whole population must be prepared for analysis in the laboratory. The preparation of a sample for analysis must be done very carefully in order to make accurate and precise measurements.
Mixing
Mixing of the laboratory sample is another critical operation. If the particle size is reduced in a series of steps, generally each step is followed by an interval of mixing. The effectiveness of any given mixing operation will be related to the particle size, shape, and density, as well as to external influences such as electrostatic or magnetic fields and air turbulence. If the material at a given stage represents a broad range of particle sizes and shapes, mixing must circumvent the tendency for fine particles to collect in the center of a pile while rounded particles collect at a pile’s edge.
Liquid samples, even gases, require thorough blending. Liquids can be stirred or otherwise agitated. Gases can be mixed by gently warming one end of the storage vessel.
Making Samples Homogeneous
The material within the sample selected from the population is usually heterogeneous, i.e., its properties vary from one location to another. Sample heterogeneity may either be caused by variations in the properties of different units within the sample (inter-unit variation) and/or it may be caused by variations within the individual units in the sample (intra-unit variation). For this reason, it is usually necessary to make samples homogeneous before they are analyzed, otherwise it would be difficult to select a representative laboratory sample from the sample.
Drying
Many of the samples received in the laboratories are wet. They must be dried before they can be crushed or pulverized for analysis. Laboratory staff uses drying procedures that avoid contamination and ensure that the drying temperature is suitable for your sample and the analysis that you want to perform on it.
Reducing Sample Size
Once the sample has been made homogeneous, a small more manageable portion is selected for analysis. This is usually referred to as a laboratory sample, and ideally it will have properties which are representative of the population from which it was originally selected.
Reducing the volume of the ground and mixed laboratory sample while keeping the sample representative is another concern. The sample can be poured through a set of riffles that uniformly splits it into two (or more) streams. One is selected for further processing, with the other(s) discarded or archived for future reference. If the laboratory sample is very large, the riffling process may be repeated several times. At the end of this process, the final selected stream is the test sample.