Analytical Services Laboratory of ICET

 

The Analytical Services Laboratory, part of the Institute for Clean Energy Technology (ICET) of Mississippi State University (MSU), has extensive state-of-the-art capabilities for materials analysis.   The laboratory is managed by ICET personnel and supports all of the projects within the ICET. Here are a few examples:

 

*      Mercury analysis for phytoremediation and bioavailability studies

*      Chemical characterization of glass and ceramic waste forms for radioactive waste immobilization

*      Analytical support and chemical analyses of saltcake dissolution studies (non-radioactive)

*      Capable of analyzing uranium and other radioactive materials

*      Thermal analysis of materials

*      Inorganic/organic carbon content of materials

*      Anion analysis

*      Analysis of solutions from durability tests such as the Product Consistency Test (PCT) and the Toxicity Characteristic Leaching Procedure (TCLP)

*      Resource Conservation and Recovery Act (RCRA) metals analysis

*      Optical microscopy of glass and ceramic waste forms for radioactive waste immobilization

 

The laboratory is primarily supported by the funding and projects generated by the ICET.   The laboratory facilities are available to other members of the MSU community depending on their various needs, capabilities, and possibilities for joint funding.  Appropriate training may also be necessary for new users of the equipment.  (Requests for access will be evaluated on a case-by-case basis.)

 

The services of the laboratory are also open to the general public.  Costs are negotiable and depend on the number of samples, type and complexity of analysis, and expected turn-around time.

 

The laboratory technical staff includes two analysts, Ms. Yunju Xia and Mr. Dean Patterson, having over 45 years of cumulative experience in the field. Ms. Xia has two master’s degrees, one in Chemical Engineering and another in Chemistry. Mr. Patterson has a master’s degree in Analytical Chemistry. Both chemists design the analyses, perform the sample preparation with the help of a student worker if needed, program and operate the instruments, and perform a preliminary examination of the data.

 

Standards, blanks, and instrument calibration are applied according to the needs of the sample or project.  For instance, because the ICET works closely and extensively with the Department of Energy (DOE), some projects have been required to conform to their strict Quality Assurance (QA) guidelines.  (The governing document for DOE QA is OCRWM DOE/RW-0333P Rev. 14.)  Ms. Teresa Leone is our QA officer.  Depending on the customer’s requirements, a “graded approach” is used in applying the most appropriate level of QA to assure an accurate analysis.


The analytical laboratory operates under MSU's radioactive materials Educational Broad Scope License and can accept various radioactive isotopes including uranium and uranium-bearing materials.  Responsible for all of ICET are Ms. Donna Rogers as Health & Safety Officer and Mr. Michael Parsons as Environmental Compliance specialist. ICET health and safety compliance is managed by Donna Rogers, CIH and environmental compliance for the institute is managed by Michael Parsons, CHMM

 

The point of contact for the Analytical Services Laboratory is:

 

Dr. Jeff S. Lindner

ICET – Mississippi State University

205 Research Boulevard

Starkville, MS 39759

Phone: (662) 325-7641

Fax: (662) 325-8465

Email:  lindner(at)icet.msstate.edu

 


Analytical Instrumentation

 

Laser Ablation – Inductively Coupled Plasma –Mass Spectrometer

(LA-ICP-MS)

 

 

The newest addition to the laboratory (through an instrumentation grant from the NSF) is a Laser Ablation – Inductively Coupled Plasma –Mass Spectrometer (LA-ICP-MS). The instrument is comprised of a New Wave UP213 Laser Ablation unit and a Perkin Elmer Elan DRC II Mass Spectrometer. This instrument is capable of analyzing materials down to an accuracy of 1 part per trillion with little or no sample preparation required and substantially no damage to the sample. The spectrometer is also equipped with an ADS-500 Autodilutor and an ASX-502 Autosampler.  The system uses ELAN v.3.3 software.  Both microstructural analysis and bulk analysis can be performed.  It is estimated that the instrument will be operational in the second half of 2006.

 

The addition of the LA-ICP-MS brings a new and exciting capability to our laboratory and should lead to new sources of projects and funding.  Two of our initial focus areas will be the examination of archeological materials and the study of the surface of materials especially with respect to material degradation (corrosion).

 

Inductively Coupled Plasma Atomic Emission Spectrometer (ICP-AES)

 

 

The Perkin Elmer Optima 4300 DV has both axial and radial viewing modes and is equipped with an AS90plus autosampler and uses WinLab 32 software.   It can detect a wide range of elements with a sensitivity in the ppb range. The exact sensitivity depends on the specific element.

 

The ICP-AES is the workhorse of our laboratory.  Cation analysis is critical to our understanding and characterization of waste forms and other materials. 

 

 Total Inorganic Carbon – Total Organic Carbon (TIC/TOC) Analyzer

 

 

 

 

The Tekmar Dohrman Phoenix 8000 wet oxidation TIC/TOC system can measure the amount of carbon that is associated with organic or inorganic compounds in aqueous samples, or the total carbon, as low as 0.5ppm.  It is equipped with an autosampler that can be configured for 24 positions (125mL bottles), 140 positions (40mL vials), or 154 positions (23mL test tubes) and uses TOC Talk 3.0 software.  This instrument is routinely used for the analysis of drinking waters, wastewaters, and samples from saltcake dissolution studies to determine the levels of carbonate and total organic carbon present.

 


High Performance Liquid Chromatography (HPLC)

 

This system is composed of multiple Dionex components. It includes a Dionex LC chromatography enclosure, a GP50 gradient pump, a PC10 post-column pneumatic delivery system, and a PDA-1000 photodiode array detector with a wavelength range of 100 to 800 nm.

 

The system is used to monitor the concentration of organic compounds and cationic species including Cr6+, Cr3+, Fe2+, and Fe3+.

 

 

 

Ion Chromatograph (IC)

 

The Dionex DX-500 Chromatography system includes an EG40 Eluent Generator, an AS40 autosampler, a GP 50 gradient pump, an ED40 electrochemical detector, a PDA-100 photodiode array detector, PC10 pneumatic controller, and PeakNet 6.2 software.  This system is used to monitor the concentration of anions in aqueous samples.

 

 

 

 

Gas Chromatograph/Mass Spectrometer (GC/MS)

 

The Varian system has an autosampler comprising a Varian Saturn 2000 GC/MS/MS with 8200 CX Autosampler, Archon purge trap autosampler, and Tekmar 300 purge and trap concentrator.  It uses a Saturn 2000 GC/MS workstation.  This instrument can be used to analyze VOCs, semi-VOCs, and other organics.

 

Cold Vapor Atomic Absorption (CVAA) for Mercury Analysis

 

The Perkin Elmer FIMS-100 CVAA is an EPA-approved method for mercury analysis with detection limits down to the 0.1 ppb level.  The instrument is equipped with an AS90plus Autosampler and uses WinLab 32 software.  The technique uses the classical cold vapor atomic absorption (CVAA) method for mercury (EPA methods 7470A and 7471A); however, reduction of mercury post-digestion/oxidation is achieved on-line by use of a flow-injection system.

 

 

Differential Scanning Calorimeter (DSC)

This system is comprised of a Netzsch Pegasus 404 with a platinum furnace and is capable of achieving temperatures up to 1500°C.  It employs Proteus software for data analysis.  The DSC can be used for the determination of specific heat, melting temperatures, transition enthalpies, phase transformations, phase diagrams, crystallization temperatures, glass transition temperatures, decomposition effects, reaction kinetics, and purity, as a function of temperature or time.  Atmospheric control can be done with one or two purge gases which may flow separately or concurrently during analysis.

 


Thermo-Gravimetric/ Differential Thermal Analysis (TG/DTA)

 

 

 

The Perkin Elmer TG/DTA 6300 has a temperature range from room temperature to 1200°C.  The TG/DTA monitors the mass loss of a material during thermal processing as a function of temperature or time. It can pinpoint water or solvent evaporation, phase changes, and thermal decomposition of components, measuring the rate at which the mass loss occurs.


 

Analytical Support Equipment

And Miscellaneous Capabilities

 

 

The laboratory is also furnished with a chemical hood, a deionized water station, several precision balances, sieves with a variety of mesh sizes, grinders, constant-temperature baths, shakers, an ultrasonic cleaner, a pH meter, and other standard laboratory equipment.

 

For some materials, an aggressive method of dissolution is necessary.  The laboratory has Perkin Elmer/Anton Paar Multiwave (shown with carrousel resting on top) is used for aggressive digestion of samples for compositional analyses.  The instrument is provided with Teflon vessels and high-pressure quartz vessels.

 

Microwave Digestion System – Perkin Elmer/Anton Paar Multiwave

 

 


 

The Olympus BX50 optical microscope system is fitted with 100x, 200x, and 400x objectives and has polarized light capabilities. The system also includes software for image capture and topological analysis.

 

 

Optical Microscope

 

 

 

 


A variety of furnaces of various sizes can be used for different processes. The larger furnace, with a liftable top, can reach 1600°C and is programmed with a Thermaltek controller.  The smaller ones are programmable and have a maximum temperature of 1200°C.  Platinum crucibles are available for glass melting at the higher temperatures and other special projects.

 

Furnaces

 

EPA SW-846 is typically followed for all inorganic and organic analyses when appropriate.  Digestion methods for solid samples have been developed for microwave preparation and alkali fusion preparation.   Product performance tests including ASTM C-1285 “The Product Consistency Test for Waste Glass” and EPA method 1311 “Toxic Characteristic Leaching Procedure (TCLP)” are performed routinely.

 

Stainless Steel Vessels for the Product Consistency Test