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Speciation analysis is defined as the separation and quantification of different oxidation states or chemical forms of a particular element. In the past, the determination of total element concentrations was considered to be sufficient for clinical and environmental considerations. Although the total concentration of an element is still useful to know and essential in many areas, the determination of each species is an important task. The concentration of a toxic species is more relevant in the setting of environmental and ecological standards than is the total elemental concentration. The collection, treatment and preservation of samples for quantitative analysis of species require careful consideration and planning. This separates speciation studies from procedures for "total" element determinations, and analytical chemists are faced with very difficult problems in the acquisition of accurate data. Speciation analysis is essential for predicting and modeling fate, risk, and effects while it's a must have for designing custom - tailored treatment strategies. Wastewater treatment failures are often results of not understanding the individual chemistry at different stages of treatment. The speciation of an element can directly affect the efficiency of the treatment process. Unfortunately, speciation analysis is not as common as traditional total elemental analysis because while speciation data is accepted by some regulators, there are no set laws or regulations on this matter. We believe that the lack of species-specific regulations is due to the absence of methods that can reliably measure the analytes of interest at the regulatory levels. For instance, the analytical methods currently available for elements such as arsenic and chromium are either not selective enough or do not provide sufficiently low detection limits.

Another important issue for speciation analysis is its cost. Even though it has been shown time after time that speciation analysis can save time and money with respect to remediation and risk assessment, it is usually more expensive than routine elemental analyses. One of the most important aspects of speciation analysis is the issue of preservation. In the ideal world, we would be able to perform speciation analysis in the field. Unfortunately, this is still not possible for most analytes of interest so even the most sophisticated analytical methods for the determination of an element's speciation are “useless” if it cannot be assured that the species distribution in the sample remains unchanged between sample collection and analysis.

Therefore, choosing the right preservation techniques for the right matrix is obligatory to ensure that the speciation information in the sample remains intact during shipping and storage until the analysis is performed. Analytical speciation procedures require experienced personnel who understand proper sampling and analytical protocols. As a result, most commercial full-service environmental laboratories do not provide this service. Applied Speciation and Consulting, LLC has been instituted to fill this gap providing routine and non-routine analytical speciation services and consulting to the scientific community. Our experience with a variety of matrices allow us to choose the right sampling protocols and right analytical methods depending on the target species and the sample environment

Ion chromatography (IC) is based on the differences in the attraction of the solute ions to the charged sites on the chromatographic column (stationary phase). It provides tremendous separation power and by changing the pH and ionic strength of the eluant (mobile phase), a variety of ionic species can be separated in a single run. The most common detectors for ion chromatography is conductivity and UV spectrophotometry. Even though these detectors are useful for some species, they can not provide enough sensitivity and selectivity especially for metal(loid)s. Inductively coupled plasma - mass spectrometry (ICP-MS) has been the choice for the determination of total metals and metal(loid)s because it's a mature technique with incredible sensitivity and selectivity. As with every analytical technique, it is prone to interferences but most of these interferences have been well documented. In fact, with the introduction of second generation ICP-MS instruments that are equipped with dynamic reaction cells, almost interference-free analysis at trace levels is becoming reality.

Coupling the separation power of ion chromatography to the detection power of ICP-MS is extremely beneficial for the determination of metals and metalloids. Although, it has been an “old” analytical technique with hundreds of scientific articles in the literature, it has not been utilized in regulatory methods. To our knowledge, the only accepted method that acknowledges and utilizes IC-ICP-MS is ASTM Method D6994-04 for cyanide speciation analysis. This specific method was developed by our senior scientist, Dr. Hakan Gürleyük as part of a joint ASTM and EPA Inter-Laboratory Collaborative for the validation of a Cyanide Speciation Analysis method. IC-ICP-MS can not only provide detection limits in the range of 1-10 ppt (ng/L) for various analytes, it can also eliminate false positives since most analytes are identified according to their isotopic ratios in addition to retention time matching.

Determination of a variety of analytes simultaneously is also possible in some circumstances since many mass-to-charge ratios can be monitored in a single run. In fact, in our laboratory, this feature has been routinely used to monitor interfering species to provide the most accurate results. In our laboratory, we utilize a Dionex ion chromatography system and couple it to a Perkin Elmer ICP-MS system equipped with a Dynamic Reaction Cell. We have developed various methods for the speciation analysis of a variety of analytes including arsenic, selenium, chromium, metal-cyanide complexes and transition metals. Each of these methods are described in following sections.

If you have any questions regarding services or would like a quotation, please feel free to email us at info@appliedspeciation.com or call (425) 483-3300. Feel free to visit our website on a regular basis as we will be providing scientific discussions and useful links to save you time and money.