Routine analysis, requirements

In experiments where a higher degree of sensitivity and selectivity is required, fluorescence and mass-selective detectors have been applied. Picomole limits of detection offered by fluorescence makes it ideal for routine analysis requiring high sensitivity. Mass spectrometry has also proven to be both a sensitive and efficient way to identify numerous chlorophyll derivatives (unitf4.s). van Breemen et al. (1991) utilized both fast atom bombardment (FAB) and tandem mass spectrometry (MS/MS) for the structural characterization and mass determination of numerous deriva-... 

Routine analysis requires a short analysis time, especially when sample preparation is simple. In fact, the instrumental requirements are demanding but commercially available. Three categories can be distinguished ... 

The utilization of commercially available finite element packages in the simulation of routine operations in industrial polymer processing is well established. However, these packages cannot be usually used as general research tools. Thus flexible in-house -created programs are needed to carry out the analysis required in the investigation, design and development of novel equipment and operations. 

Time, Cost, and Equipment Automated chemical kinetic methods of analysis provide a rapid means for analyzing samples, with throughputs ranging from several hundred to several thousand determinations per hour. The initial start-up costs, however, may be fairly high because an automated analysis requires a dedicated instrument designed to meet the specific needs of the analysis. When handled manually, chemical kinetic methods can be accomplished using equipment and instrumentation routinely available in most laboratories. Sample throughput, however, is much lower than with automated methods. 

Total acidity and total chlorides can be deterrnined by conventional techniques after hydrolysing a sample. Satisfactory procedures for determining hydrogen chloride and free-sulfiir trioxide are described in the Hterature (18,41). Small amounts of both hydrogen chloride and sulfur trioxide can be found in the same sample because of the equiUbrium nature of the Hquid. Procedures for the direct deterrnination of pyrosulfuryl chloride have also been described (42,43), but are not generally required for routine analysis. Small concentrations of sulfuric acid can be deterrnined by electrical conductivity. 

Multidimensional ehromatography is a very powerful teehnique whieh ean help solve eomplex problems in environmental analysis. Sinee it requires more eomplex instrumentation, it has not been widely used in routine analysis, although some of the eoupled teehniques may beeome important in eontrol laboratories in the future. 

Repetitive routine analysis of a specific sample (e.g., for Quality Control) will usually require a dedicated instrument. Therefore, the chromatograph and, in particular, the detector will be chosen for that specific analysis. Consequently, only one detector will be necessary and the purchase of an armory of detectors on the basis that they might be needed in the nebulous future is not advised. An alternative detector can always be obtained if and when the demand arises. The same argument applies to multi-solvent reservoirs and multi-solvent gradient programmers and other accessories that are not immediately required for the specific analysis in mind. 

Desorption of an analyte from the SPME fibre depends on the boiling point of the analyte, the thickness of the coating on the fibre, and the temperature of the injection port. The fibre can immediately be used for a successive analysis. Some modifications of the GC injector or addition of a desorption module are required. It is possible to automate SPME for routine analysis of many compounds by either GC-MS or HPLC. A significant advantage of SPME over LLE is the absence of the solvent peak in SPME chromatograms. SPME eliminates the separate concentration step from the SPE and LLE methods because the analytes diffuse directly into the coating of the SPME device and are concentrated there. 

There are two main types of routine analysis carried out, i.e. those required for screening purposes, where one is testing a large number of individual unrelated samples, e.g. work-place drugs screening, and those for surveillance activities, e.g. monitoring foodstuffs for the level of toxic metals. 

If no method exists for the analysis required, then either an existing method has to be adapted or a new method developed. The adapted or developed method will need to be optimized and the controls required identified, hence ensuring that the method can be used routinely in the laboratory. Evidence is then collected so as to demonstrate that the method is fit for purpose . The extent of validation, i.e. the amount of effort that needs to be applied, depends on the details of the problem and the information already available. Figure 4.3 indicates an approach that can be used to decide on the extent of validation required. The answer to DQ 4.2 has already mentioned that the customer may request a particular method. If... 

Certainly, a vast amount of experience has been gained by the widespread use of conventional amino acid analysers. They offer high reliability, accuracy, reproducibility and can separate complex samples. Because conventional analysers can be fully automated, they are widely used in routine analysis. However, the method is limited by the sensitivity which can be achieved using ninhydrin as the derivatizing agent. Sensitivity can be increased by using ortho-phthaldialdehyde (OPA) instead, but where extremely high sensitivity is required, HPLC is the method of choice. 

Packed columns are still used extensively, especially in routine analysis. They are essential when sample components have high partition coefficients and/or high concentrations. Capillary columns provide a high number of theoretical plates, hence a very high resolution, but they cannot be used in all applications because there are not many types of chemically bonded capillary columns. Combined use of packed columns of different polarities often provides better separation than with a capillary column. It sometimes happens that a capillary column is used as a supplement in the packed-column gas chromatography. It is best, therefore, to house the capillary and packed columns in the same column oven and use them selectively. In the screening of some types of samples, the packed column is used routinely and the capillary column is used when more detailed information is required. 

The technique is fairly suitable for routine analysis because its operation and related calculations do not require highly skilled personnel, and... 

The use of dansyl derivatives is not recommended for routine analysis of free amino acids but is very suitable in the identification of an unknown amino acid that has been selectively extracted from the original sample and is present in small quantities. Both kinds of derivative can be easily separated by chromatography or electrophesis and no locating reagent is required for either because the DNP derivatives are themselves yellow in colour and the dansyl derivatives are fluorescent. 

When developing a CE method for routine analysis of samples in our laboratory, the first three parameters to be checked are reproducibility, sensitivity, and throughput. There is little use for any analytical method that does not meet these three requirements. 

However, only common and inexpensive reagents are used. They are rapid and do not require ai r expensive or sophisticated apparatus, in contrast with chromatographic methods. So, the proposed methods can be used for the routine analysis of caffeine in energy drinks. 

The accuracy of an analysis can be determined by several procedures. One common method is to analyze a known sample, such as a standard solution or a quality control check standard solution that may be available commercially, or a laboratory-prepared standard solution made from a neat compound, and to compare the test results with the true values (values expected theoretically). Such samples must be subjected to all analytical steps, including sample extraction, digestion, or concentration, similar to regular samples. Alternatively, accuracy may be estimated from the recovery of a known standard solution spiked or added into the sample in which a known amount of the same substance that is to be tested is added to an aliquot of the sample, usually as a solution, prior to the analysis. The concentration of the analyte in the spiked solution of the sample is then measured. The percent spike recovery is then calculated. A correction for the bias in the analytical procedure can then be made, based on the percent spike recovery. However, in most routine analysis such bias correction is not required. Percent spike recovery may then be calculated as follows ... 

Other eluent systems in suppressed ion chromatography are typically chosen based on specific separation requirements. For routine analysis of monovalent and divalent anions, carbonate-based eluents represent a reasonable alternative to hydroxide-based eluent systems. Carbonate eluents are simple to prepare and can be useful in cases where anion analysis is only occasionally performed. It must be kept in mind, however, that carbonate lowers the detection sensitivity for anionic species and introduces significant nonlinearity into the analysis. ... 

Those parameters that are not directly evaluated by system suitability testing during routine analysis must be checked periodically or the risk mitigated in some other way to ensure that the instrument is maintained in a qualified state. However for some critical parameters evaluation as part of the system suitability testing may not be sufficient and specific periodic testing may also be required. 

However, the major limitations of instrumental analysis for marine biotoxins are, first sometimes the lack of standards, second the required time of analysis, are expensive techniques to be applied in routine analysis but the main limitation is the lack of information about the possible presence of other nontarget marine biotoxins. 

---