Research and Development of New Analytical Methods

Project Home Tasks Products Contacts Links

Task Objectives

One of the primary goals of this task is to provide for the development and performance of analytical protocols for difficult-to-analyze samples that are beyond the routine capabilities of commercial laboratories. This development tries to anticipate and meet future analytical needs of USGS projects, so that state-of-the-art analytical methods will be available to users as they are needed.

Another objective of this task is to develop new analytical methods that meet the specific needs of USGS scientists, and then make these methods available to outside commercial labs for their use as routine methods.

It should be emphasized that the method development capability of this task is not directed specifically to assist the projects of any particular Geologic Discipline program. Rather it is meant to be a valuable resource that is available to any project within the Geologic Discipline that may need the services of expert, highly experienced, analytical chemistry research and development personnel employing state-of-the-art instrumentation.

Statement of Work

Under a Cooperative Research And Development Agreement (CRADA) agreement with PerkinElmer, Inc., an analytical instrumentation manufacturer, a new endeavor will be undertaken to cooperatively develop a completely new Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) system which will improve our laboratory's capabilities. Research chemistry staff will have the opportunity to test prototype instruments under development and help make improvements based on the needs of the geochemical analysis community. Once the new instrumentation is introduced to the general public, Research Chemistry will be allowed to use the test unit for methods development and sample analysis free of charge for one year after the CRADA agreement has ended.

This task will further develop novel in-situ microanalytical techniques aimed at determining trace concentrations of heavy metals in surface water environments. The focus of this development will be to analyze aqueous environments for metals such as zinc, copper, and lead in a virtual real-time mode using field deployable instrumentation that operates in an unattended mode.

With the development of a Cr speciation method for Cr(III) and Cr(VI) using High Performance Liquid Chromatographic separation and High Resolution ICP-MS detection for waters completed, we plan to extend this method for use on soil extracts. Efforts in 2007 will focus on completing the method validation using appropriate soil extraction techniques and isotope dilution methods. This method will also be used to support the production of a speciated Cr reference material for NIST (National Institutes for Standards and Technology).

We plan to utilize the capabilities of our new Dynamic Reaction Cell ICP-MS to extend the current analytical capabilities of research chemistry. Once the instrument is installed, we plan to develop a rapid, sensitive method for the SIMULTANEOUS determination of sub-ppb concentrations arsenic, chromium, and selenium species in aqueous samples. This method will be based on the use of a new liquid chromatographic column to simultaneously separate As, Cr, and Se species prior to their determination using a quadrupole ICP-MS instrument. Existing quadrupole ICP-MS methods will be updated in order to take advantage of the interference eliminating capabilities of the Dynamic Reaction Cell ICP-MS in support of general USGS mission goals and projects. Specifically, methods for the ultra-trace detection of difficult elements like As, Se, Cr, Fe, Ag, Au, and others in geologic samples will be developed.

We plan to continue to develop the capabilities of the High Resolution ICP-MS to analyze samples that require either high-resolution to resolve interferences or samples that would benefit from the superior sensitivity of the high resolution ICP-MS. Specific projects to be completed include the development of methods for ultra-trace levels of gold in both solutions and solids, the development of isotope dilution methods in support of the USGS Reference Materials Project and the Geochemical Landscapes Project, as well as the analysis of specific samples for isotopic concentration information.

We also aim to develop a multi-acid digestion procedure for the dissolution of municipal biosolids. This procedure will replace the more time-consuming microwave digestion procedure. The testing of various types of digestion vessels is currently underway.

We will update the 4-acid and ICP-MS REE sinter methods to streamline them and improve their performance, including running a variety of QA standards to validate the revised methods. We will also modify the calibration routines for the ICP-MS methods in order to improve the method's accuracy for differing matrices.

Efforts will also be undertaken to update and validate the methods currently used on the ICP-OES instrumentation to improve their accuracy and performance for varying sample matrices and to streamline the data entry process into Laboratory Information Management System (LIMS).

Return to top of this page | Next Task | Task List


Mineral Resources	Eastern / Central / Western / Alaska / Minerals Information
Mineral Resources	Crustal Imaging & Characterization / Spatial Data