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X-Ray Diffraction

X-Ray Diffraction (XRD)

The Bruker D8 Discover x-ray diffractometer is a non-destructive technique for characterizing crystalline materials. The diffraction pattern contains information on the structure, phase, crystal orientation, crystallinity and strain. The D8 system is equipped with a Cu X-ray source, point and linear detectors, and has both Bragg Brentano and Goebel Mirror optics for divergent or parallel beam applications. The system is designed to analyze powder samples, conduct thin film analysis and analyze capillary contained samples. The ICDD database allows for rapid phase identification of a large variety of samples.     

  • Common Uses: Powder phase and lattice parameter identification,  residual stress analysis, small-angle x-ray scattering, thin film thickness determination, nanoparticle size determination     
  • Strengths: Flexibility and ease-of-use with Bruker DaVinci control system,  snap-Lock x-ray optics of easy alignment     
  • Constraints:     

 

X-Ray Photoelectron Spectroscopy (XPS)

XPS (also called ESCA - Electron Spectroscopy for Chemical Analysis) is a surface sensitive technique that provides elemental and chemical analysis. Depth resolution of 1-10 nm is possible. Organic functional groups can be identified as well as very thin surface layer structures and material interfaces.This custom XPS system features SPECS components in ultra-high vacuum.     

  • Depth Resolution: 1 nm     
  • Elements Detected: Li - U    
  • Common Uses: Material Interfaces, chemical characterization of surface     
  • Strengths:  Surface Sensitive Elemental and Oxidation State Analysis     
  • Constraints: Sample size constraints – usually 1"x1"x 0.25" maximum,  non-conductive samples present additional challenges,  pumping time to introduce sample into UHV analysis chamber

 

Handheld X-Ray Fluorescence (XRF)

The Thermo Niton XL3t 900S GOLDD energy dispersive (ED) handheld XRF is a portable device used to quickly determine the elemental composition of a sample. This analysis tool can identify most alloys in under 30 seconds. It is also used in consumer product safety applications, import/export restrictions, precious metal identification, soil monitoring, QA/QC work, antiquities research, and to check for RoHS/WEEE/CPSIA compliance. Minimal sample preparation also makes this non-destructive technique attractive in screening items. 

  • Elements Detected: Mg to U    
  • Detection Limits: 10 ppm (element specific)    
  • Common Uses: Alloy Identification,  RoHS screening,  lead detection    
  • Strengths:  Generally no sample preparation,  non-destructive, rapid analysis, versatile sample types (plastics, metals, soils, etc.)    
  • Constraints:  Sample Size - should be 3 mm in diameter or greater, elements of interest - cannot detect elements lighter than Mg such as Na, F, etc.

 

X-Ray Fluorescence (XRF)

The Bruker Tiger S8 XRFinstrument can identify major and minor elementsto the part per million (ppm)level in a variety of samples. This wavelengthdispersive (WD) instrument can operate with the sample under vacuum or under heliumand is more sensitive and accurate than an energy dispersive (ED) XRF. Quantificationis obtained with matrix matched standards. Common samples include rocks, sands,and glasses. Traditional vacuum samples are crushed and ground into a powder,which is prepared into fused glass beads or pressed pellets. Some materials(glass) can be analyzed as-is. Using Helium, powder and liquid samples may beanalyzed through a Mylar or polypropylene film.

  • Elements Detected: Na to U
  • Detection Limits: 10 ppm (element specific)
  • Common Uses: Geochemical Analysis, Quality Assurance/Quality Control Functions,
  • Strengths: Quantitative Analysis (with matrix matched standards), Automation of Routine Analyses
  • Constraints: Matrix matched standards required, elements of interest - cannot detect elements lighter than Mg such as Na, F, etc., often a destructive technique due to sample size constraints – samples must be a homogeneous, flat disk about 2 inches in diameter. Powder and liquid samples must be homogeneous and infinitely thick as well as being compatible with the polymer film.

 

High Resolution Inductively Coupled Plasma – Mass Spectrometry (ICP-MS)

The ThermoFinnigan Element2 HR-ICP-MS is used to conduct ultratrace level analyses on a wide variety of samples. One of less than 500 worldwide, this powerful instrument is commonly used for geological studies and water analysis. MSC staff has also studied plastics and catalysts for private sector partners using ICP-MS. Most metals can be detected to the parts per trillion (ppt) level, including many that are often obscured in quadrupole ICP-MS work. The multi-element capabilities of the instrument enable rapid quantitative analysis.

  • Elements Detected: All     
  • Detection Limits: 5 ppt (element specific)    
  • Common Uses: Process Bath Analysis, Geochemical Analysis, Water Studies, Biological Materials     
  • Strengths: Highly Sensitive – part per trillion detection limits for many elements, Quantitative analysis – use of inorganic elemental standards     
  • Constraints:  Sample Introduction – sample must be a liquid (native form or through acid digestion),  Elements of Interest – some elements (F, C, etc.) have much higher detection limits, Sample Matrix – acidified aqueous samples are best.Particulate matter or high total dissolved solids can prohibit analysis.

 

UV-Vis Spectroscopy

The Cary 50 Bio UV – Vis spectrometer provides absorbance measurement for liquid samples in the ultraviolet and visible regimes. Absorbance spectra from the UV-Vis can be used to determine concentrations of components in solution as long as the components absorb in this regime. The Cary 50 utilizes a Xenon flash lamp which produces a narrow and intense light beam allowing for small sample volume analysis (40 µL) with 80% signal intensity remaining. The system software package allows the system to operate with a single wavelength monitor, a scanning module, a Kinetics module or a scanning Kinetics module. This system utilizes a single sample cell and can be used to collect data with ambient light present.      

  • Range of operation: 190 – 1100 nm      
  • Common Uses:     
  • Strengths:     
  • Constraints:

 

Fluorescence Spectrometer (Fluorimeter)

The Perkin Elmer LS 50 Fluorimeter is a spectroscopic technique which induces fluorescence in a compound with exposure to a pulsed Xenon lamp. Compounds which fluoresce will absorb energy leading to an excited state, when they return to the ground state they emit energy in a quantized manner in the form of light. The technique provides excellent selectivity and is sensitive to parameter like pH, viscosity, and thermal effects. The system is equipped with a Peltier thermal cell to allow temperature studies to be conducted on the samples.     

  • Limit of Detection:Part per Trillion     
  • Common Uses:     
  • Strengths:  High specificity     
  • Constraints: Compound must be fluorescent – typically requires aromatic or multiple double bonds

 

Gel Permeation Chromatography (GPC)

The GPC (also known as SEC - Size Exclusion Chromatography) utilizes liquid chromatography to separate polymers in solution based on the size of the polymer. The Waters system consists of a single mobile phase Isocratic Pump (Water 1515), a series of GPC columns (Styragel HR3, HR4 and HR5) a single wavelength UV/Vis Detector (Waters 1489) and a Refractive Index Detector (Waters 2414). The GPC, if properly calibrated for a specific sample is quantitative and provides Molecular Weight information in Mn, Mw and Mz as well as determining the polydispersity index (PDI) of the sample.     

  • Mobile Phase: Dimethylformamide with 0.01 M LiCl, Other solvents are possible but may require separate columns     
  • Calibration: Polystyrene standards: 890 – 2,630,000 Daltons     
  • Common Uses:     
  • Strengths:     
  • Constraints: Columns are solvent specific

 

Scanning Electron Microscopy with Energy Dispersive Analysis (SEM/EDS)

The Hitachi S-3400N Variable Pressure SEM is equipped with an EDS detector and Thermo Noran System Seven software. A variable pressure (VP) option allows for analysis of non-conductive materials.Secondary electron (SE) and backscattered electron (BSE) detectors allow for multiple imaging options.An internal camera provides video feed of the sample during an analysis.This instrument is capable of remote operation of the electron imaging functions.

A Hitachi S510 SEM with an EDS detector and Noran System Six software is also available. These instruments are used for studies of surface morphology and bulk Elemental Analysis and mapping of samples such as electronic components. Images and data are easily captured by the software for rapid electronic distribution. MSC staff has worked with regional businesses to study defects in machined parts and the elemental makeup/distribution of alloys.

  • Resolution: 3.0 nm (SE, high vacuum mode)
  • Elements Detected: Be to U
  • Detection Limits: 1000 ppm (element specific)
  • Common Uses: Electronic Components, Coating Thickness measurements, Biological materials, Geological thin sections, Failure Analysis
  • Strengths: Remote Operation, Elemental Mapping, Feature Measurement Tools
  • Constraints: Sample size constraints – usually a 4"x3"x2", maximum.2 kg weight maximum, Non-conductive samples present additional challenges, Electron beam and vacuum can deform sample

 

Scanning Auger Nanoprobe (SAN)

The Physical Electronics PHI 680 uses Auger Electron Spectroscopy (AES) to determine the elemental content of the top few atomic layers of a sample. It is also equipped with a scanning electron microscope (SEM) and ion sputtering capabilities, allowing for depth profiling of samples.

  • Lateral Resolution: 13 nm
  • Depth Resolution: 0.5 to 10 nm
  • Elements Detected: Li - U
  • Detection Limits: 0.1 – 1 atomic %
  • Common Uses: Electronic Components
  • Strengths: Ultimate in Surface Sensitivity for Elemental Analysis (top 10 nm), Elemental Mapping, Depth Profiling using Argon Sputtering
  • Constraints: Sample size constraints – usually a 3"x3"x2" maximum, Sampling depth is dependent on the material, Samples need to be electrically conductive, Requires sample compatible with ultra-high vacuum

 

Transmission Electron Microscopy (TEM/EDS)

The JEOL 2010 200 kV transmission electron microscope provides high resolution nanoscale images of materials and electron diffraction patterns, which provide crystallographic information. The TEM is capable of magnification up to 1 million times, providing spatial resolution of 1-10 nm.The instrument is also equipped with a Thermo Noran System Seven energy dispersive x-ray analysis (EDS) unit, allowing for elemental analysis.

  • Resolution: 1 nm
  • Elements Detected: Be to U
  • Common Uses: Nanoparticles, Biological materials, Air particulates
  • Strengths: Nanoscale Imaging, Elemental Analysis, Feature Measurement Tools
  • Constraints: Sample size constraints – usually deposited on a 3 mm metal or carbon grid, Non-conductive samples present additional challenges, Electron beam may deform sample

 

Raman Microscope

The Horiba XploRA Raman microscope provides structural characterization of organic and inorganic molecules in solids, liquids and on surfaces by measuring the molecular vibrations induced by a laser beam. The Raman system couples optical images with high resolution chemical mapping allowing the chemical image to be super imposed on the optical image. The system includes polarization optics and a fiber-coupled probe for analysis of objects which do not fit in the enclosure.

  • Spatial Resolution: < 1 um
  • Spectral Resolution: 1.1 cm-1 /pixel
  • Laser Excitation: 532 nm and 785 nm
  • Common Uses:
  • Strengths:
  • Constraints: Samples fluorescence can limit Raman usefulness, Requires standards to be more than qualitative
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