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Elemental Analysis

ICP-OES Analysis

Major, minor, and trace elemental analysis by inductively coupled plasma optical emission spectrometry is offered using a Jarrell Ash IRIS High Resolution ICP-OES. The ICP-OES technique uses a plasma at 8000°C to energize ions to emit lights, an optical filter to separate emitted light according to wavelength, and a CID detector to measure ion concentration. This technique was developed in 1970’s and has matured since then into a reliable, quick and inexpensive simultaneous measurement of elemental concentrations in various geological, biological, biomedical and environmental samples. Compared to the ICP-MS technique, this ICP-OES technique lacks the ability to measure isotopic concentrations and isotope ratios or ion concentrations at very low levels. It does, however, offer the option for more routine analysis.

We offer the following ICP-OES services. Please contact the Madison lab for specialized analysis/method development. Solutions should be stabilized in 1% HNO3 (or 1% HClO4) and be at least 10 mL. Solid samples will be digested with mineral acids at high temperature.

Many elements in the periodic table can be analyzed simultaneously with a wide dynamic range (ng L-1 to mg L-1). Samples that have been analyzed include soils and soil extracts, plant tissues and plant sap, animal bones and tissues, foodstuffs, proteins, solutions, biological fluids, and water/waste water. Elements can be grouped as follows:

• Essential plant elements, Major and secondary: P, K, Ca, Mg and S; Minor: Fe, Mn, Cu, Zn, B, Al and Na.
• Nonessential metals: Cd, Cr, Co, Ni, Mo and Ba.
• Other elements can be included in the above groups on request or be combined in different groups.

ICP-MS Analysis

The inductively coupled plasma mass spectrometry (ICP-MS) is one of the latest advancement in determining isotopic concentrations, isotopic ratios and elemental concentrations in various geological, biological, biomedical and environmental samples. Coupled with different sample pretreatment, and/or with different sample introduction devices, the ICP-MS can be used for ultra-trace (e.g. As and Se at sub µg L-1 level), micro-sized sample (25 µL), or speciation analysis. The ICP-MS uses a plasma at 8000°C to ionize analytes, a mass filter to separate analytes according to their mass-to-charge ratios, and an electron multiplier to measure ion concentration.

The following services are offered with a VG PlasmaQuad PQ2 Turbo Plus ICP-MS. Solution samples should be prepared in 1% HNO3 acid to preserve trace metals and be more than 10 mL, and “homogenous” dried solid samples should be more than 1 gram. Solid samples are routinely digested with mineral acids at high temperature(150°C). Please contact the Madison lab for specialized analysis/method development.

• Elemental analysis of 73 elements in the periodic table quasi-simultaneously with a wide dynamic range (pg L-1 to µg L-1). Samples that have been analyzed include soils, plant tissues, animal tissues, foodstuffs, alloys, proteins, solutions, and water.
• Isotopic concentration and isotopic ratio analysis: The mass spectrum produced is analogous to an emission spectrum but tremendously simpler than that, and can be used as a “finger print” to identify unknown samples and impurities.
• Stable isotope dilution(SID) technique: Stable isotope dilution techniques(SID) using an enriched isotope spiked to a sample can be used for the SID calibration. Compared to conventional external calibration methods, SID is not affected by the problems such as matrix effect, physical interference, chemical interference, or instrument instability. The result by using SID is usually the most accurate and precise among several calibration methods or several analytical methods.
• Hydride generation for As, Se, Sn, Sb, Te, Ge, Pb and Bi: The hydride generation technique is used to separate analytes from the matrix and increase the sample introduction efficiency. Selenium at 0.004 mg g-1 in plant tissue is reliably determined.
• Gaseous sample introduction to determine iodine speciation in water samples.
• Micro-sample introduction: A CETAC MICRONEB 2000 system is used to introduce micro-size samples(as little as 25 µL) into the ICP-MS system for analysis.