Water Sampling Techniques

Wu et al. [388] carried out measurements of the enrichment of Atrazine on the micro surface water of an estuary. These authors used a micro surface water sampling technique with a 16 mesh stainless steel screen collecting bulk sampled from the top 100-150 pm of the surface. Atrazine concentration in the actual micro surface was estimated to vary in the range 150-8850 pg/1. 

Bufflap, S. E., and Allen, H. E. (1995b). Comparison of pore water sampling techniques for trace metals. Water Res. 29(9), 2051—2054. 

The improvement in water sampling techniques such as the development of the Kiel in-situ Pump (KISP) [122] and high resolution gas chromatography (such as MDGC-ECD) has resulted in a series of papers on the concentration of di-, mono-, and occasionally non-ortho CB levels in world waters. This is detailed in Table 4. 

The choice of the correct sampling point can depend on the depth of a lake [19]. These authors have compared different water sampling techniques in a series of lakes. 

Preparation of soil—sediment of water samples for herbicide analysis generally has consisted of solvent extraction of the sample, followed by cleanup of the extract through Uquid—Uquid or column chromatography, and finally, concentration through evaporation (285). This complex but necessary series of procedures is time-consuming and is responsible for the high cost of herbicide analyses. The advent of soUd-phase extraction techniques in which the sample is simultaneously cleaned up and concentrated has condensed these steps and thus gready simplified sample preparation (286). 

Ethylene oxide is sold as a high purity chemical, with typical specifications shown ia Table 14. This purity is so high that only impurities are specified. There is normally no assay specification. Proper sampling techniques are critical to avoid personal exposure and prevent contamination of the sample with trace levels of water. A complete review and description of analytical methods for pure ethylene oxide is given ia Reference 228. 

Mercury generally is found in low and trace concentrations. So there is need to determine Hg in ranges corresponding to various types of water samples. Detection levels of Hg can be improved by the use of vapour generation technique. This technique allows to sepai ate the analyte from the sample matrix and so to overcome the matrix interference. The fluorescence technique, with its high sensitivity and linearity, in combination with vapour generation, provides for a possibility to detect Hg in parts per trillion per liter regions. 

The recent development and comparative application of modern separation techniques with regard to determination of alkylphosphonic acids and lewisite derivatives have been demonstrated. This report highlights advantages and shortcomings of GC equipped with mass spectrometry detector and HPLC as well as CE with UV-Vis detector. The comparison was made from the sampling point of view and separation/detection ability. The derivatization procedure for GC of main degradation products of nerve agents to determine in water samples was applied. Direct determination of lewisite derivatives by HPLC-UV was shown. Also optimization of indirect determination of alkylphosphonic acids in CE-UV was developed. Finally, the new instrumental development and future trends will be discussed. 

Lead and copper are regulated by a Treatment Technique that requires systems to control the corrosiveness of their water. If more than 10% of tap water samples exceed the action level, water systems must take additional steps. For copper, the action level is 1.3 mg/L, and for lead is 0.015 mg/L. 

Water sample collection techniques differ depending on the source being tested. The minimum number of water samples collected from a distribution system which are examined each month for coliforms is a function of the population. For example, the minimum number required for populations of 1,000 and 100,000 are 2 and 100, respectively. To ascertain compliance with the bacteriological requirements of drinking water standards, a certain number of positive tests must not be exceeded. When 10-ml standard portions are examined, not more than 10 percent in any month should be positive (that is, the upper limit of coliform density is an average of one per 100 ml). 

When determining the bacterial content of, for example, foods, clinical material and even water, elaborate techniques are required to eliminate non-bacterial ATP. Also, the sample being tested has to undergo an extraction process to remove ATP from any bacteria present. The problem of non-microbial ATP is not likely to be met in the examination of pharmaceuticals and toilet goods, however. 

Analytical methods for parent chloroacetanilide herbicides in soil typically involve extraction of the soil with solvent, followed by solid-phase extraction (SPE), and analysis by gas chromatography/electron capture detection (GC/ECD) or gas chromatog-raphy/mass spectrometry (GC/MS). Analytical methods for parent chloroacetanilides in water are similarly based on extraction followed by GC with various detection techniques. Many of the water methods, such as the Environmental Protection Agency (EPA) official methods, are multi-residue methods that include other compound classes in addition to chloroacetanilides. While liquid-liquid partitioning was used initially to extract acetanilides from water samples, SPE using... 

The most widely employed techniques for the extraction of water samples for triazine compounds include liquid-liquid extraction (LLE), solid-phase extraction (SPE), and liquid-solid extraction (LSE). Although most reports involving SPE are off-line procedures, there is increasing interest and subsequently increasing numbers of reports regarding on-line SPE, the goal of which is to improve overall productivity and safety. To a lesser extent, solid-phase microextraction (SPME), supercritical fluid extraction (SEE), semi-permeable membrane device (SPMD), and molecularly imprinted polymer (MIP) techniques have been reported. 

Table 3 Summary of solid-phase extraction techniques applied to the preparation of water samples for the determination of triazine pesticides...

Specifically for triazines in water, multi-residue methods incorporating SPE and LC/MS/MS will soon be available that are capable of measuring numerous parent compounds and all their relevant degradates (including the hydroxytriazines) in one analysis. Continued increases in liquid chromatography/atmospheric pressure ionization tandem mass spectrometry (LC/API-MS/MS) sensitivity will lead to methods requiring no aqueous sample preparation at all, and portions of water samples will be injected directly into the LC column. The use of SPE and GC or LC coupled with MS and MS/MS systems will also be applied routinely to the analysis of more complex sample matrices such as soil and crop and animal tissues. However, the analyte(s) must first be removed from the sample matrix, and additional research is needed to develop more efficient extraction procedures. Increased selectivity during extraction also simplifies the sample purification requirements prior to injection. Certainly, miniaturization of all aspects of the analysis (sample extraction, purification, and instrumentation) will continue, and some of this may involve SEE, subcritical and microwave extraction, sonication, others or even combinations of these techniques for the initial isolation of the analyte(s) from the bulk of the sample matrix. 

Sample preparation techniques vary depending on the analyte and the matrix. An advantage of immunoassays is that less sample preparation is often needed prior to analysis. Because the ELISA is conducted in an aqueous system, aqueous samples such as groundwater may be analyzed directly in the immunoassay or following dilution in a buffer solution. For soil, plant material or complex water samples (e.g., sewage effluent), the analyte must be extracted from the matrix. The extraction method must meet performance criteria such as recovery, reproducibility and ruggedness, and ultimately the analyte must be in a solution that is aqueous or in a water-miscible solvent. For chemical analytes such as pesticides, a simple extraction with methanol may be suitable. At the other extreme, multiple extractions, column cleanup and finally solvent exchange may be necessary to extract the analyte into a solution that is free of matrix interference. 

F.D. Wilde, D.B. Radtke, J. Gibs, andR.T. Iwatsubo, Collection of Water Samples , in National Field Manual for the Collection of Water-Quality Data , US Geological Survey Techniques of Water Resource Investigations, US Geological Survey, Reston, VA, Book 9, Chapter A4, (1999). 

From a technical standpoint, this article emphasizes recent advances in sample preparation and instrumentation. A brief history of modern sample preparation techniques is covered, together with the impact of modern instrumentation on water sample analysis. 

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