H&M Analytical Services Equipment

Here at H&M, we have a wide range of analytical testing equipment to meet customer needs and requirements ranging from XRD to particle size analysis to high resolution imaging.  Utilizing our state-of-the-art equipment, we strive to apply our experience and knowledge to solve your most challenging problems. We pride ourselves on fast turn-around of routine diffraction tests, often within 2 to 3 days at no additional charge.

XRD Equipment

Panalytical X’Pert MPD Pro – H&M employs multiple X’Pert MPD Pro diffractometers in various configurations in order to cover all of your XRD requirements.  We have multiple machines so that we can handle the high sample throughput and provide our customers with results faster than other XRD laboratories, with turnaround times of 2-3 days for most moderately sized sample sets.  The use of high speed detectors (PixCel and X’celerator) and robotic sample changers provide improved throughput without sacrificing scan quality for standard powder samples.

While providing the fast turnaround, the multiple diffractometers also allows us the flexibility to meet the more specialized needs of challenging samples.  Utilizing the Panalytical Prefix concept, these units have numerous options and configurations for addressing both powder and bulk sample needs.  H&M is capable of running scans with fixed divergence, anti-scatter, and receiving slits or where preferred, using programmable and variable slit optics as well as Soller slits for improved scan and peak resolution where desired.  For samples where fluorescence is an issue, we have diffracted beam monochromators available to reduce the background and provide quality scans where the detection of trace phases is possible.  Large bulk samples, odd shapes, and coated wafers, coupons, etc. can easily be accommodated using the multi-purpose sample stage or other sample holders.

 

 

 

 

 

 

 

These versatile diffractometers, when coupled with the expertise of H&M’s staff, allow us to perform multiple types of XRD analyses, providing valuable materials properties and data such as: phase identification and quantification, percent crystallinity, residual stress, retained austenite, domain size, preferred orientation, rocking curves, lattice parameters, and pharmaceutical polymorph identification.

Particle Size Analyzers

The particle size of a material influences many of its properties and subsequent performance and can be an important measurement in fields like pharmaceuticals, geology, and materials science.  As an example, understanding the particle size distribution of a pharmaceutical powder can be vital in ensuring the proper rate of dissolution of a drug substance.  H&M provides a wide range of analytical methods for interrogating the size, shape, and aspect ratio of your materials, including laser scattering, high resolution microscopy, and laboratory scale sieve analysis.  Whether interested in true particle size, evaluating agglomeration behavior, or determining the crystallite size, H&M has the tools to appropriately measure your sample.

Horiba LA-950V2 – This is a state of the art particle size analyzer utilizing laser scattering to measure the particle size distribution over a wide range of sizes from 10 nanometers to 3,000 microns.  By measuring the intensity and angle of the scattered light and applying the Mie scattering theory, the dual wavelength system provides fast and accurate measurements over the entire range.   The Horiba system is equipped with both wet and dry dispersion systems and can also handle a limited number of solvents if required.

 

 

 

 

 

Scanning Electron Microscopes –Scanning electron microscopy (SEM) is a powerful method of investigating the size and shape of particles and agglomerates by imaging the regions of interest.  This can be particularly useful in evaluating materials with acicular particles, irregular morphologies, facets, or just do not disperse or measure properly in the particle sizer.  SEM is also very useful for bulk samples where grains or grain boundaries can be imaged measured in polished samples of metals or mounted geological specimens.  For additional information on H&M’s SEM capabilities, please visit the High Resolution Imaging tab.

X-ray Diffraction – For some applications, the features of interest are finer than the particles you can see with your eyes, or can easily image in an SEM.  Particles can, in fact, be made up of even smaller grains or crystals and knowing their size can be important for many applications.  Crystallite or domain size measurements can be simply performed using X-ray Diffraction (XRD) methods.  This method is limited to the range of 1 – 100 nm, however.

Thermal Analysis

There is a well-known paradigm in the field of materials science that you can only fully categorize a material’s performance and properties if you understand both its structure and its processing.  As a compliment to H&M’s suite of tools for evaluating structure, H&M offers two methods of thermal analysis testing to provide insight into the thermal processing history and relevant materials properties that are essential for performance.

Q50 TGA, Thermal Gravimetric Analysis – This technique measures the weight loss or gain behavior of a material as a function of increasing temperature or time.  These weight changes can be attributed to physical and chemical changes in the sample such as decomposition, oxidation, dehydration, volatilization, organic phase content, Curie temperature, and many other materials properties.  Our Q50 TGA system operates over a temperature range from ambient to 1000°C and can handle sample sizes from 10 mg to 1 gram while providing accurate and repeatable results.

 

 

 

 

 

 

 

 

Q20 DSC, Differential Scanning Calorimetry – DSC measures the difference in heat flow between the sample of interest and a reference sample during a controlled heating process.  This an excellent analytical technique for interrogating many useful material properties such as melting and crystallization temperatures, phase and polymorph transitions, glass transition temperatures, curing temperature, specific heats, and many other thermal and material properties.  H&M performs DSC testing on a Q20 DSC that provides accurate thermal data on small samples (0.5 to 100 mg) and has a working temperature range of -40°C to 400°C.

 

 

 

 

 

 

 

 

Chemical Analysis

Whereas XRD is an excellent tool for evaluating the phases present in a sample, the determination of chemical constituents and trace level impurities is often of equal interest to the customer.  Whether performing basic quality control, research and development, reverse engineering, or looking for a sense of the composition of a coating, scale, or a small sample area, H&M offers the quantitative chemical testing methods to meet your testing needs.

Panalytical PW2403 Wavelength Dispersive XRF with PW2540 Sample Changer – This instrument is a wavelength dispersive x-ray spectrometer capable of analyzing the elements between Na and U with high precision and accuracy, and detection down to O.  It has an automatic sample changer that can handle up to 120 samples, ensuring H&M can meet the high throughput demands of QC and large sample sets.  This versatile machine can test solids, powders, and liquid samples, and is supported by traditional powder sample preparation methods including pressed pellets, as well as glass beads with the use of a Katanax K1 Prime Fluxer.  Semi-quantitative analysis is quickly available using a fundamental parameters approach.  For more accurate and stringent projects, full quantitative analysis is available through the preparation of calibration standards.

Energy Dispersive XRF –The lab also offers a second approach to chemical analysis through the use of EDXRF.  This system is mounted to one of our SEM units and offers the ability to detect elements from carbon to uranium.  As the system is associated with the SEM, this technique differs from the standalone WDXRF by allowing a quick and nondestructive way to perform elemental mapping and line scans on a specific sample area.  This is a quick and useful tool for aiding in failure analysis or providing spot chemical compositions on bulk samples that are not suitable for alternative sample preparation.

High Resolution Imaging

In many scientific fields, high resolution imaging can provide valuable insights into the grain structure, surface morphology, fracture surfaces, corrosion behavior, particle size and shape, and a myriad of other properties and features of materials.  H&M offers scanning electron microscopy (SEM) as a quick and cost-effective imaging tool which when coupled with energy dispersive spectroscopy, provides both quality imaging and elemental composition.  We are equipped to meet the sample preparation and coating needs to support the high resolution imaging.   H&M can deliver these services to customers on an hourly basis and with two different instruments to meet a customer’s specific project needs.

Topcon ABT-32 – This unit offers reasonable images at low and mid-range magnifications of up to 20,000.  The large depth of field of SEM imaging permits excellent focusing on irregular surfaces such as fracture surfaces or textured samples.  It is equipped with both secondary and backscattered electron detectors and can therefore provide imaged with enhanced compositional contrast where necessary.  The Topcon also has an energy dispersive x-ray (EDX) spectroscopy system to measure elemental concentrations.

 

 

 

 

 

 

 

Zeiss Sigma FESEM – The Sigma is a field emission scanning electron microscope (FESEM) that delivers even higher quality images when compared to a standard SEM like the Topcon.  With potential resolutions of 1.5 nm @ 30 kV and magnifications up to 1,000,000, this microscope permits us to tackle the most challenging material problems for our customers.  It also has an energy dispersive x-ray (EDX) spectroscopy system for analyzing and mapping chemical composition of individual regions or particles.  Electron backscatter diffraction (EBSD), used for detailing crystallographic and texture features in microstructures, is also available.

 

 

 

 

 

 

 

 

Support Equipment

H&M has all of the necessary support equipment for properly preparing samples in order to provide the best results to our customers.  While this equipment is utilized internally in support of the testing we perform, the equipment and techniques are also available to support customer projects as needed.  Our additional equipment includes:

  • Jaw crushers for pulverizing rocks / geological samples    
  • Ball mills / micronizing mills for particle size reduction
  • Cryomilling
  • Motorized & conventional mortal and pestles
  • Sieves for material selection
  • Low speed saws for cutting & sectioning samples
  • Mounting, grinding, and polishing equipment
  • High temperature ovens (1100°C max) for drying, thermal treatments, LOI testing, etc.