Experts in elemental and isotopic analysis of organic and inorganic materials

Elemental analysis is a process where a sample is analyzed for its elemental (and sometimes isotopic) composition. Elemental analysis can be qualitative (determining what elements are present), and it can be quantitative (determining how much of each element is present).

There are numerous techniques for analyzing elemental composition.

Please see below for an overview

We offer both cGMP and non GMP testing services. Please see below for more detail about the services we offer.

GMP SERVICES AVAILABLE

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* (µg/day)	Target limit J (µg/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

Proton Induced X-Ray Emission (PIXE) is a non-destructive technique that can identify elements from sodium to uranium in solids, liquids, and aerosol filters. It uses a proton beam to excite an electron shell change to force the emission of detectable X-rays. PIXE can be used to analyze multi-element samples because each element's X-rays are characteristic of the element and do not overlap with each other.

High Sensitivity (detection limit ~1 ppm for thin foils and ~10 ppm for thick samples)
Measurement at Atmospheric Pressure Possible (by allowing the beam to exit from the beam line through a thin window, large samples may be analyzed in air).
Multi-element Capability (major elemental analysis is performed for any element from sodium to uranium in a single spectrum )
Non-destructive (minimal beam induced effects on the specimen)
Surface sensitive method (typical analysis depth is on the order of 1 µm)

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%.

Request More info or a Free Consultation (click)or Call 765.588.6200