Medical‑Device Defect and Failure Analysis and Metrology Services

Microscopy, SEM, EDX, and ICP‑MS


SEM / EDX / ICP-MS Device Analysis



Microscopic cracks, alloy mix-ups, or trace-metal contamination can derail a 510(k) or spark a costly recall. Our lab pinpoints these issues with high-resolution SEM imaging, elemental EDX maps, and ppb-level ICP-MS quantitation—so you can fix them before the FDA asks


Technique What you get Typical Use-cases
SEM metrology (20 nm resolution) Surface-defect imaging, dimensional checks (± 0.05 µm) Stent strut cracks, catheter balloon wrinkles. Verifying the dimensions and tolerances of critical medical-device components
EDX elemental mapping Alloy verification, plating-thickness, foreign-particle ID Nitinol/titanium homogeneity, solder inclusion
ICP-MS trace-metals
Quantitation to ppb; USP <232>/<233> style

Ni, Cr, Co leachables; contamination audit


Scanning Electron Microscopy (SEM) -

Investigate ultrastructure

Application AND Technique Description
Electron microscopes are used to investigate the ultrastructure of a wide range of biological and inorganic specimens including microorganisms, cells, large molecules, biopsy samples, metals, and crystals. The SEM produces images by probing the specimen with a focused electron beam that is scanned across a rectangular area of the specimen (raster scanning).

Due to the very narrow electron beam, SEM micrographs have a large depth of field yielding a characteristic three-dimensional appearance useful for understanding the surface structure of a sample. A wide range of magnifications is possible, from about 10 times (about equivalent to that of a powerful hand-lens) to more than 500,000 times, about 250 times the magnification limit of the best light microscopes.

Specimens are observed in high vacuum in conventional SEM, or in low vacuum or wet conditions in variable pressure or environmental SEM, and at a wide range of cryogenic or elevated temperatures with specialized instruments.

Our Capabilities:

o High Vacuum
o Low Vacuum
o Cryo
o Energy Dispersive X-ray Analysis (EDX)

Instruments Used Model: Notes:
Thermo Phemom XL Fully integrated EDX and BSE detector
FEI Quanta 3D FEG High and low vacuum, Cryo capability
Oxford INCA PentFEXx3 Energy dispersive X-ray spectroscopy (EDX)
Wiki Reference for SEM

Elemental analysis -

Detection, identification, and quantification:

Elemental analysis and testing includes identification and quantification of elements, elemental compounds and molecular species. Sample types and matrices tested for trace elements include organic and non-organic, aqueous and non-aqueous materials. Elemental trace and ultra-trace analysis detection ranges from parts per million (ppm), to parts per billion (ppb) and parts per trillion (ppt) levels, using proven techniques.

Application AND Technique Description
Elemental analysis is a qualitative and quantitative process for identifying the elemental composition of materials (e.g., chemical compounds, minerals, metals, fluids). Certain elemental techniques can even identify the isotopes of a given element.

We offer several elemental analysis techniques:



Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is a technique that can identify elements from sodium to uranium in solids, liquids, and aerosol filters. ICP-MS is a type of mass spectrometry that uses an Inductively coupled plasma to ionize the sample. It atomizes the sample and creates atomic and small polyatomic ions, which are then detected. It is known and used for its ability to detect metals and several non-metals in liquid samples at very low concentrations. It can detect different isotopes of the same element, which makes it a versatile tool in Isotopic labeling. Compared to atomic absorption spectroscopy, ICP-MS has greater speed, precision, and sensitivity.

In the pharmaceutical industry, ICP-MS is used for detecting inorganic impurities in pharmaceuticals and their ingredients. Chapter <232> Elemental Impurities - Limits; defines the maximum limits of fifteen elements in pharmaceutical products and Chapter <233> Elemental Impurities - Procedures; defines how the testing for these elements should be performed. These chapters have caused an increase in the need for ICP-MS testing. Previously, other analytic methods had been sufficient.


Target limits (J) for the fourteen elements specified in USP <232>.

Element Oral daily dose PDE* (ug/day) Target limit J(ug/g)
Cadmium 5 0.5
Lead 5 0.5
Inorganic arsenic 15 1.5
Inorganic mercury 30 3
Iridium 100 10
Osmium 100 10
Palladium 100 10
Platinum 100 10
Rhodium 100 10
Ruthenium 100 10
Chromium 1100 1100
Molybdenum 3000 300
Nickel 200 50
Vanadium 100 20
Copper 3000 300
*PDE = permitted daily exposure based on a 50 kg person
  • ICP/MS is ideal for trace element analysis for a wide range of sample types and industries
  • ICP/MS is a destructive technique
  • Also widely used in the geochemistry industry for radiometric dating, in which it is used to analyze the relative abundance of different isotopes; in particular uranium and lead.


Energy Dispersive X-ray - (EDX) is a rapid technique for identifying the elements from beryllium to uranium in solid materials. EDX uses an electron beam to stimulate the emission of characteristic x-rays of the elements from the sample surface. The elemental results are presented in an x-ray spectrum. EDX can be used to analyze localized areas or generate chemical maps. Both qualitative and quantitative analyses can be performed. (Triclinic Labs typically uses EDX for the identification of contaminants.)

EDX is very good for elemental analysis or chemical characterization of a sample with high levels of ionic elements (carbon, oxygen, copper, silver, aluminum, etc.) - including relative elemental composition information.

Downsides include:
  • Potentially destructive test because items may need to be cut for sample preparation, sputter coated, or otherwise modified before being placed in the chamber
  • Thin film materials, such as chloride and sulfate, can be volatilized under sublimation and carried away in the vacuum and subsequently not detected.

Figure 1. Foreign particle SEM image with spot (#4) and regional (#1,2,3) elemental analysis and resulting elemental composition shown in table. Region 3 demonstrates copper substrate and the inclusion body (regions 1, 2) contains aluminum, oxygen, copper, lanthanum, and carbon. A second smaller particle (4) contains carbon, silicon, and copper.

Figure 2. Synthetic sample showing EDX false color imaging. Magenta crystals are calcium carbonate, green crystals are calcium sulfate (gypsum), and the lilac crystal is graphite.


X-ray fluorescence (XRF) is a non-destructive analytical technique used to determine the elemental composition of materials, primarily inorganics and simple organic molecules. XRF analyzers determine the chemistry of a sample by measuring the fluorescent (or secondary) X-ray emitted from a sample when it is excited by a primary X-ray source. Each element in a sample produces a set of characteristic fluorescent X-rays (“a fingerprint”) unique for that specific element, which is why XRF spectroscopy is an excellent technology for qualitative and quantitative analysis of material composition.

XRF is used in the following industries.

  • Pharmaceuticals and Cosmetics - non-destructive elemental analyses of impurities in active pharmaceutical ingredients and excipients in line with the recommendations in ICH Q3D, USP<232>, USP<233> and USP<735>. Applications that have traditionally been performed by ICP MS are now possible without the need for time-consuming and costly sample preparation.
  • Oil and gas - positive material identification (PMI) of piping material - critical where flow accelerated corrosion or sulfidic corrosion, is a concern
  • Metal fabricating - non-destructive elemental analysis to ensure incorrect or out-of-specification metals or alloys don’t enter the manufacturing process
  • Automotive & Aerospace - inspection and quality control of metallic and coated parts
  • Precious metal recycling - accurately determine the grade of precious metals and prevent metals from entering the recycling process
  • Mining & exploration - quickly identify the most economically usable resources

Instruments Used Model: Notes:


Thermo


iCAP RQ ICP-MS


This innovative single quadrupole (SQ) ICP-MS is the ideal trace elemental analyzer for a wide range of sample types.

Method Development, Validation, Release Testing.
Thermo Phemom XL SEM/EDX Fully integrated elemental and BSE detector
Panalytical Epsilon 4 ED-XRF Spectrometer for the elemental analysis ranges from carbon (C) to americium (Am), and the concentration ranges from sub-ppm to 100 wt%.