Engineering and Mining Experiment Station (EMES)

Helios 5-CX dual beam

EMES houses a Thermo Fisher Scientific Helios 5-CX focused ion beam – scanning electron microscope (FIB-SEM), which is capable of both imaging and manipulating materials down to the single nanometer scale. The SEM portion of the instrument accelerates a focused beam of electrons at the surface of a material, generating signal electrons and x-rays which are used for imaging and microanalysis. The FIB portion of the system accelerates ionized gallium atoms at the surface of the sample to ablate material, allowing for micro to nanoscale machining of surfaces. In tandem, the FIB-SEM can be used to sequentially remove material and image subsurface features, allowing for 3D rendering of microstructure and chemistry.

The SEM is equipped with a field emission gun source and is capable of 1 nm resolution at 1kV accelerating voltage. Detectors include ET, retractable backscatter, retractable STEM, and several in-lens detectors. Further, the system is equipped with an Oxford UltimMax 100 EDS detector, and Oxford Symmetry S3 EBSD.

The FIB is equipped with a Ga+ source capable of ~4 nm resolution at 30kV. Along with manual user layouts for milling, the system has automated TEM sample prep and in-situ lift-out capabilities through AutoTEM 5 and TF nanomanipulator, and automated serial sectioning with Auto Slice and View.

Axia ChemiSEM

EMES also houses a Thermo Fisher Scientific Axia ChemiSEM scanning electron microscope. The Axia is equipped with ET, retractable backscatter, EDS, and cathodoluminescence detectors enabling a wide range of applications.

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X-ray diffraction (XRD) is a method for probing the space between atomic planes that make up crystalline materials. In doing so, the technique allows for identification of materials based on their crystal structure and lattice spacings. XRD is primarily used for phase identification of minerals and metals, and also finds some applications with polymers, thin films, and nanomaterials. The EMES is equipped with a Malvern Empyrean (3rd Gen.) XRD that is equipped with a cobalt source, automated optics, a Pixcel3D detector, and 3-axis cradle stage.

Measurements are primarily done in powder mode but can also include grazing incidence measurements of thin films and residual stress by chi-tilting.

The system also has an Anton Parr DCS500 stage capable of in-situ measurements from –180 °C to 500 °C, with electrical connections for simultaneous in-situ electrical measurements. This stage mounts to the 3-axes cradle, allowing for in-situ residual stress measurements as well.

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Facility Overview

Inductively coupled plasma mass spectrometry (ICP-MS) can be utilized for both quantitative and semi-quantitative analysis of most elements in the periodic table and is commonly employed in a wide range of geologic, environmental, biological, and industrial applications. The primary strengths of ICP-MS lie in its ability to provide rapid, sensitive, and precise multi elemental analyses across a high dynamic range enabling measurement of elemental concentrations ranging from sub parts per billion to hundreds of parts per million in a single run. The EMES is equipped with an Agilent 7900 quadrupole ICP-MS for determination of trace, minor, and major elements in aqueous solutions and acid digestions.

Sample Preparation

Sample preparation for ICP-MS is dependent upon the sample type and users analytical needs. Preparation procedures should be discussed with EMES personnel during experimental design to ensure their suitability for analysis on our instrument. Sample preparation facilities, including an Anton Paar Multiwave 5000 Microwave System, are available to lab users and can be utilized to prepare a wide range of sample types. The following are some general guidelines to consider when preparing samples to be analyzed in the EMES:

• All reagents used in sample preparation for ICP-MS should be high purity and certified for trace metal analysis (for ppb level analyses most commonly performed in our lab Fisher TraceMetal grade or equivalent is required and Optima grade may be ideal if analyzing near detection limits).
• A procedural blank should be prepared following the same process as unknown samples to ensure no contamination during sample preparation.
• Samples must be free of particulates as the presence of any particulates may clog the sample introduction system. If necessary, particulates can be removed from the sample through filtration or centrifugation and decanting.
• Samples should preferably have less than 200 parts per million total dissolved solids (TDS) although higher TDS concentrations may be possible if discussed with EMES personnel prior to submission. Samples with TDS above this range may be diluted to the appropriate range.
• Samples should ideally be in a 2% HNO3- matrix. In some cases, other matrices may need to be utilized, but total acid contents must remain below 5% and cannot include hydrofluoric acid.
• Estimated elemental concentrations for the samples should be provided to enable selection internal standards and calibration concentrations. If elemental concentrations are unknown, they can be determined using a semi-quantitative analysis on the ICP-MS.
• While most elements are stable in dilute acid solutions it is generally better to analyze samples quickly after collection or preparation.
• Samples should ideally be stored and submitted in 15 mL polypropylene test tubes (Falcon tubes are a good option, but other brands will also work).
• A sample volume of 10 mL is preferred. Smaller sample volumes may be possible if necessary but should be discussed with EMES staff prior to submission.

User Fees

Analysis fees for the ICP-MS are charged at an hourly rate to cover instrument maintenance and consumable costs. User fees for the ICP-MS are charged at the following rates:

	User Provided Labor	EMES Provided Labor
Research	$89.58/hr	$132.56/hr
Commercial	$172.19/hr	$251.28/hr

 

Run times are dependent upon the type of samples analyzed and the analytes of interest. Approximately 45 minutes of instrument startup and tuning time is needed at the beginning of each analytical run. After tuning and optimization each sample or standard takes approximately 1-2 minutes. An estimate of sample run times for specific applications can be provided upon request.

To be eligible for the User Provided Labor rate users must have been trained by the EMES staff and judged to be able to independently run the analyses from start to finish. Until a user is proficient in utilization of the ICP-MS the EMES Provided Labor charge will apply. Sample preparation using a variety of standard protocols may also be performed by EMES staff for a fee. Contact EMES staff for information regarding available preparation methods and fees. Samples submitted to the EMES that require filtration or dilution prior to analysis will also be charged a sample preparation fee.

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Facility Overview

Ion chromatography (IC) is a method for separation of ionic species in aqueous solutions according to their affinity to a stationary phase within a chromatographic column whose concentrations are then quantified using a conductivity or other detector. IC can be utilized to measure a variety of species including major and minor anions, major and minor cations, and organic acids. IC is primarily used to assess water chemistry in natural or artificial systems but can also be used to analysis extracts of solid samples such as soils. The EMES is equipped with a Dionex ICS-6000 Dual Channel High Pressure Ion Chromatography system configured to enable concurrent analysis of cations and anions using conductivity detection. The standard setup utilizes a CS-16 column for analysis of Li, Na, K, Mg, Ca, and NH4 and an AS-11 column for analysis of Cl, F, Br, NO2, NO3, SO4, and PO4. Other analytes such as organic acids, amines, or other metals may also be analyzed using the system but may require system reconfiguration. Please contact EMES staff if you are interested in performing nonroutine analyses.

Sample Preparation

Samples should be submitted in either 1.5 mL or 10 mL plastic vials with split septa caps that are compatible with the AS-AP autosampler. Thermo Scientific vial kits (Item #’s 055427 and 055058) are preferred although other brands may be utilized if approved by EMES. All samples should be filtered to at least 0.45 micron to remove any particulate matter. Failure to filter samples resulting in damage to columns or other instrument hardware will incur additional charges. Samples should be diluted such that all analytes of interest are within the appropriate calibration range (typically between 0.1 and 50 ppm). Samples containing high concentrations of organic compounds such as humic acids or transition metals may require additional sample preparation steps prior to analysis. EMES staff can provide assistance into sample preparation procedures; however, it is ultimately the responsibility of the user to ensure that samples are prepared to meet their analytical needs and do not result in contamination and/or loss of analytes.

User Fees

Analysis fees for the IC are charged at an hourly rate to cover instrument maintenance and consumable costs. User fees for routine cation (Li, Na, K, Mg, Ca, and NH4) and anion (of Cl, F, Br, NO2, NO3, SO4, and PO4) analyses are charged at the following rates:

	Anions	Cations	Labor
Research	$26.10/hr	$13.05/hr	$47.24/hr
Commercial	$84.56/hr	$42.28/hr	$86.92/hr

 

Typical run times are 30 minutes per sample for cation analyses and 15 minutes per sample for anion analyses. A minimum charge two hours is required for both cation and anion analyses.

Primary Contact:

Dr. Scott Beeler
Research Scientist II - Analytical Chemistry
Email: Scott.Beeler@sdsmt.edu
Office: Mineral Industries 212B
Phone: (605) 394-2380

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Facility Overview

The total organic carbon (TOC) analyzer enables quantification of the amount of total organic carbon (TOC), total inorganic carbon (IC), and total carbon in aqueous samples (TC). The EMES operates a Shimadzu TOC-L CSN Total Organic Carbon Analyzer within the Shimadzu Environmental Research Laboratory. The TOC-L utilizes a combustion catalytic oxidation method paired with a nondispersive infrared (NDIR) gas analyzer enabling complete oxidation of difficult to decompose samples and detection limits as low as 4 ug/L. Total organic carbon can be analyzed utilizing the non-purgeable organic carbon (NPOC) or the total carbon minus inorganic carbon (TC-IC) method. Total carbon and inorganic carbon may also be analyzed using standalone methods. The TOC-L is equipped with an OCT-L 8-port auto-sampler allowing continuous measurement of up to eight samples.

Sample Preparation

Samples should be collected and submitted in 40 mL glass amber vials with no headspace. Vials should be cleaned, triple-rinsed with deionized water, and baked at 550oC for a minimum of two hours prior to use. Samples should be refrigerated as soon as possible following collection and remain chilled until analyzed. If dissolved organic carbon (DOC) is to be analyzed samples should filtered at the time of collection. If filtration is not possible in the field sample should be filtered as soon as possible after collection.

User Fees

Analysis fees for the TOC analyzer are charged on an hourly basis. Routine analysis using the NPOC method takes approximately 15 minutes per sample. Calibration standard must be analyzed at the beginning of each day and typically requires 1 – 1.5 hours of instrument time. User fees for the TOC analyzer are charged at the following rates:

	User Provided Labor	EMES Provided Labor
Research	$17.25/hr	$49.25/hr
Commercial	$31.74/hr	$11.74/hr

 

To be eligible for the User Provided Labor rate users must have been trained by the EMES staff and judged to be able to independently run the analyses from start to finish. Until a user is proficient in utilization of the GC-MS the EMES Provided Labor charge will apply. Samples not submitted in an analysis ready form will be charged a sample preparation fee.

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Facility Overview

Gas chromatography mass spectrometry (GC-MS) enables the identification and quantification volatile and semi-volatile organic compounds at trace concentrations from complex mixtures. The technique pairs separation of compounds using gas chromatography with sample identification and quantification via mass spectrometry. GC-MS is a critical technique in a variety of disciplines including environmental science, biology, geology, and materials sciences. The EMES operates a Shimadzu QP2010 Ultra GC-MS within the Shimadzu Environmental Research Laboratory. 

The GC-MS is a single quadrupole system equipped with a dual inlet system with a PTV injector allowing for split/spitless injections of soluble samples and a Frontier pyrolizer enabling analysis of insoluble samples. Standard setup utilizes the PTV injector with a Rtx-5 (USP 27) column enabling analysis of a wide range of compounds. Use of the pyrolizer or other column types are also possible but require special consideration. If your samples require an alternate setup, please contact EMES staff prior to sample submission.

Sample Preparation

Sample preparation for GC-MS is sample and analyte dependent. It is recommended that sample preparation and analytical needs are discussed with EMES personnel during experimental design to ensure that the necessary analyses can be performed using our instrument. Sample preparation facilities for some sample types are available through EMES. Samples should be prepared in an appropriate organic solvent and submitted in standard screw top GC vials (2 mL volume) with PTFE/red silicone septa. For low volume samples glass inserts may be used allowing analysis of sample volumes as low as 30 microliters.

User Fees

Analysis fees for the GC-MS are charged on an hourly basis. Analysis times vary depending on the method utilized and will typically range from thirty to seventy-five minutes per sample. User fees for the GC-MS are charged at the following rates:

	User Provided Labor	EMES Provided Labor
Research	$66/hr	$108/hr
Commercial	$122/hr	$202/hr

 

To be eligible for the User Provided Labor rate users must have been trained by the EMES staff and judged to be able to independently run the analyses from start to finish. Until a user is proficient in utilization of the GC-MS the EMES Provided Labor charge will apply. Samples not submitted in an analysis ready form will be charged a sample preparation fee.

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Ultraviolet-visible (UV-Vis) spectroscopy measures the absorbance spectra of liquid and solid samples across the UV-visible region of the electromagnetic spectrum. UV-vis can be utilized for the quantitative and qualitative analysis of a wide range of materials making it a valuable tool in a variety of disciplines. The EMES operates a Shimadzu UV-2600 spectrophotometer within the Shimadzu Environmental Research Laboratory. For more information about the UV-Vis and its capabilities please contact EMES staff.

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Location: MI 128C 
Primary Contact: Dr. Bill Cross

The facility features a MicroXCT-400 high-resolution 3D X-ray microscope system from Xradia Inc. 3D X-ray microscopy is commonly referred to as Micro X-Ray Computed Tomography or MicroXCT. The system has a 150 kV X-ray source and six available detector magnifications for X-ray spatial resolution down to about 1 micron. It is also equipped with a tensile/compression stage capable of maximum loading of 500 newton. For tomographic reconstruction and advanced visualization, the facility has a dedicated high-performance workstation featuring Avizo Fire advanced visualization software.

The MicroXCT system supports research and training in a range of projects including direct write printing, paleontology, membrane bio-fouling, concrete characterization, blast and impact personal protective equipment, soil and rock core evaluation, nanoenergetics, metallic foams, friction stir joining, cold spray deposition, and examination of various composite materials.

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Location: EP 112
Primary Contact: Vanessa Kee

 The JEOL JEM-2100 LaB6 transmission electron microscope (TEM) is equipped with the high-resolution (HR) style objective-lens pole piece to achieve point resolution as small as 0.23 nm ― small enough to observe lattice structure in many crystalline materials. The instrument operates at a high tension of up to 200 kV, corresponding to an electron wavelength of 2.5 pm. Image acquisition is performed with a Gatan Orius bottom-mount, 14-bit, 11-megapixel CCD camera. An Oxford Inca energy-dispersive silicon-drift X-ray (EDX) spectrometer is provided for compositional analysis and mapping at high count rates. The instrument has scanning-TEM (STEM) capability, with both bright-field and dark-field imaging modes, as well as both secondary-electron and back-scattered electron imaging modes. Scan control is achieved through a Gatan DigiScan II image acquisition system. A hollow-cone illumination feature is available for conical dark-field imaging.

A standard JEOL double-tilt specimen holder and a second JEOL low-background double-tilt holder are provided for crystallographic and EDX analysis. A high-tilt specimen retainer is also available for electron tomography. A Gatan Model 628 single-tilt heating holder allows thermal treatments to temperatures over 1000 °C with in-situ observation.

The instrument is used by several departments on the SDSM&T campus, including Nanoscience and Nanoengineering, Chemistry, Chemical and Biological Engineering, and Materials and Metallurgical Engineering for a range of projects involving topics such as energy generation and storage, functional composite materials for space applications, and friction-stir-processed metals.. A suite of equipment is provided for standard TEM sample-preparation methods, including specimen grinding/polishing/dimpling, electrochemical thinning, ion milling, and ultramicrotomy. Access is available with appropriate training for off-campus users to meet academic and industrial needs. For training materials, scheduling, and other policies, visit http://ahrenkiel.sdsmt.edu/JEM2100_TEM/.

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The AFM facility features a Bruker Nanoscope MultiMode 8, capable of contact, non-contact, and Bruker’s Peak Force Tapping imaging modes, along with STM imaging. For a full list of capabilities and instrument training, please contact Dr. Jacob Petersen or Dr. William Cross.

AFM can be used to image surface morphology of materials ranging from micron to atomic scales. The combination of probe and samples stage selection can allow for simultaneous 3D topography with spatially resolved mechanical, electrical, magnetic, and other material properties. These capabilities make the AFM a versatile materials characterization instrument that can bridge length scales between SEM and TEM, with the added benefit of surface sensitive measurements.

The AFM facility is used extensively for faculty and graduate and undergraduate research in SDSM&T programs including: Civil and Environmental Engineering, Chemical and Biological Engineering, and Materials and Metallurgical Engineering, Nanoscience and Nanoengineering, and Mechanical Engineering.

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Location: MI 234
Primary Contact:  Dr. Edward Duke

The EMES maintains several instruments that can be used in a laboratory setting, but which are specifically designed for field portability. These instruments are particularly well suited for collection of field data in support of geological, ecological, or environmental studies. They also can be used to perform analyses on-site if a customer does not have the option of sending a sample for laboratory examination.

Visible and Near Infrared (Vis/NIR) Spectrometer

The Analytical Spectral Devices FieldSpec FR Pro portable visible and near infrared spectroradiometer records reflected radiation between 350 nm and 2500 nm. The system can use reflected solar radiation or an internal light source. A wide variety of organic and inorganic materials have diagnostic absorption features in this wavelength range (e.g., minerals, plants, polymers). This is also the principal spectral region of solar irradiance and corresponds with the spectral range of earth-observing satellite systems. For this reason, the portable Vis/NIR spectrometer is used extensively to provide ground-truth data for research in geological and environmental remote sensing. A second field spectrometer was acquired in 2014. It is a PANalytical TerraSpec Halo with similar capabilities to the FieldSpec Pro, but it is lighter and more compact and has an on-board GPS and mineral identification software.

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Raman Spectrometer

The DeltaNu Rockhound handheld Raman spectrometer provides a portable solution for rapid, non-destructive analysis. Raman spectrometry has a wide range of applications on organic and inorganic materials including mineral identification and hazardous material identification (solid and liquid). The instrument uses a 120 mW laser source (785 nm) and operates in the spectral range 200– 2000 cm-1with a resolution of 8 cm-1. The handheld unit links via wireless blue tooth or USB connections to a laptop PC for spectral display and processing. The software includes a spectral reference library of over 500 minerals.

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X-Ray Fluorescence (XRF) Spectrometer

The Bruker AXS Tracer IV-SD handheld XRF system provides rapid analysis of elements from magnesium through uranium. The handheld unit contains a rhodium X-ray source (maximum voltage of 45kV; beam current 2−25μA) and a silicon drift detector. It can be controlled through Windows CE based software on a PDA or with full lab based spectral analysis software on a laptop PC. The system includes a vacuum pump for improved detection of light elements such as magnesium and aluminum; this technology was developed in partnership with NASA for the Space Shuttle program. 

X-ray fluorescence is a widely used analytical method in the geological and material sciences. The instrument can identify hundreds of standard alloys, and can detect low levels of many hazardous elements such as lead, mercury, chromium, cadmium, and bromine, which makes it valuable for screening consumer products and paint or for mapping soil and sediment contamination from industrial or mining activity.

 

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