XPS Testing

XPS Testing

X-ray Photoelectron Spectroscopy (XPS) works by shining X-rays onto a sample surface and measuring the electrons released from the outermost layers. Because the energy of these electrons depends on the elements present and how they are chemically bonded, XPS can reveal surface composition, oxidation states, bonding environments, and trace contamination that may not be visible by bulk analysis. For drug development scientists, formulation teams, analytical project managers, and CRO partners, XPS provides information that bulk methods often cannot reveal: whether an API is enriched at a particle surface, whether an excipient coating is complete, whether a metal oxide exists in a specific oxidation state, or whether processing residues are driving unexpected performance changes. BOC Sciences offers comprehensive XPS Testing services for APIs, excipients, solid dispersions, polymeric carriers, coatings, nanomaterials, and process-contact surfaces. Our scientists design sample-specific XPS experiments, interpret high-resolution spectra, and integrate the results with complementary analytical testing to help clients convert complex surface chemistry data into actionable formulation, process, and material decisions.

BOC Sciences XPS Testing Services

Surface Elemental Composition Analysis

We perform survey-scan XPS analysis to determine the near-surface elemental profile of pharmaceutical solids, coatings, particles, and functional materials, supporting both standalone investigations and broader analysis and purification programs.

  • Atomic Percentage Reporting: Quantify surface-level elements such as C, O, N, S, P, F, Cl, Si, Na, Mg, Ca, and transition metals.
  • Surface Enrichment Assessment: Compare API, excipient, salt, surfactant, or coating-related markers at the outer surface.
  • Unknown Surface Screening: Detect unexpected residues, inorganic particulates, or adsorbed contamination layers.
  • Material Comparison: Evaluate surface composition differences across batches, suppliers, processes, or storage conditions.

Chemical State & Bonding Environment Analysis

Our high-resolution XPS methods provide chemical-state information that supports structure characterization of surfaces where oxidation, salt formation, surface functionalization, or bonding changes may affect product behavior.

  • High-Resolution Narrow Scans: Acquire C 1s, O 1s, N 1s, S 2p, P 2p, F 1s, Cl 2p, Si 2p, and metal core-level spectra.
  • Oxidation State Assignment: Differentiate metallic, oxide, hydroxide, sulfide, phosphate, carbonate, and organometallic environments.
  • Functional Group Evaluation: Resolve surface contributions from C-C, C-O, C=O, O-C=O, C-F, amine, amide, sulfate, and phosphate species.
  • Spectral Deconvolution: Apply scientifically justified peak fitting, charge referencing, and comparative interpretation.

Surface Contamination & Residue Investigation

BOC Sciences helps identify surface-originated issues that may arise from processing aids, container contact, cleaning residues, adsorbed organics, metal traces, or environmental exposure, complementing heavy metal analysis and targeted residue studies.

  • Foreign Material Identification: Determine whether visible or invisible surface residues are organic, inorganic, metallic, or silicone-based.
  • Process Troubleshooting: Link surface chemistry changes to milling, spray drying, lyophilization, filtration, coating, or packaging-contact steps.
  • Comparative Failure Analysis: Compare representative and non-representative samples to pinpoint surface-level differences.
  • Root-Cause Support: Combine XPS evidence with microscopy, chromatography, elemental, or spectroscopic data when needed.

Depth Profiling, Mapping & Interface Studies

For coatings, layered materials, modified particles, and oxide films, we provide depth-resolved and spatially resolved XPS strategies that can be integrated with elemental and material analysis technologies.

  • Ion-Etch Depth Profiling: Track composition changes from the surface into subsurface regions using controlled sputtering steps.
  • Angle-Resolved XPS: Compare signal intensity at different take-off angles to investigate ultrathin surface layers.
  • Small-Area Analysis: Examine stains, particles, coating defects, or localized regions of interest.
  • Interface Characterization: Evaluate polymer coatings, inorganic layers, surface oxides, and functionalized carrier interfaces.
Resolve Surface Chemistry Questions with Expert XPS Testing

BOC Sciences delivers scientifically interpreted XPS data for APIs, excipients, coatings, particles, and functional materials, helping teams identify surface composition, chemical states, contamination sources, and interface behavior.

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Advanced Technologies in XPS Testing

Monochromatic XPS Acquisition

Monochromatic XPS Acquisition

We use monochromatic X-ray excitation and carefully selected acquisition parameters to generate high-quality survey and narrow-scan spectra for pharmaceutical solids, polymers, inorganic materials, and hybrid drug delivery systems.

High Resolution Spectral Fitting

High-Resolution Spectral Fitting

Our scientists apply peak fitting, background selection, charge correction, and chemical-state interpretation to distinguish overlapping components and translate binding energy shifts into meaningful surface chemistry assignments.

Charge Compensation

Charge Compensation for Insulators

Many APIs, excipients, coatings, and polymeric materials are electrically insulating. We optimize charge neutralization and referencing strategies to reduce peak shifting and improve confidence in chemical-state analysis.

Depth Profiling

Controlled Depth Profiling

By combining XPS acquisition with carefully controlled ion etching, including Ar+-based approaches when suitable, we examine coating thickness trends, oxide layers, surface treatments, and buried interfaces.

Correlative Surface Analysis

Correlative Surface Analysis

XPS findings can be integrated with spectroscopy testing, X-ray fluorescence testing, ICP, Raman, XRD, and thermal techniques to build a stronger material evidence package.

Sample Specific Method Design

Sample-Specific Method Design

We design XPS studies around the actual project question, whether the goal is identifying a residue, verifying a functionalized surface, comparing API particles, or evaluating an ultrathin coating.

BOC Sciences' XPS Testing: Supported Sample Scope

BOC Sciences provides XPS Testing for vacuum-compatible pharmaceutical, chemical, polymeric, inorganic, and hybrid materials. Our team helps clients determine whether the submitted sample is suitable for XPS, how it should be mounted, and whether complementary techniques are recommended for a more complete interpretation.

Pharmaceutical Solids

  • APIs, salts, co-crystals, and intermediates
  • Excipients, blends, granules, and solid dispersions
  • Spray-dried, milled, micronized, or coated particles
  • Tablet fragments, film coatings, and surface-modified powders

Drug Delivery Materials

  • Polymeric carriers and functionalized nanoparticles
  • Lipid-based or surfactant-modified particle surfaces
  • Hydrogel, membrane, and coating materials after suitable drying
  • Fluorinated, PEGylated, amine-modified, or oxidized surfaces

Interfaces & Process Materials

  • Metal, glass, ceramic, silicon, and polymer substrates
  • SiO2, TiO2, Al2O3, and other oxide layers
  • Processing residues, stains, particulates, and deposits
  • Packaging-contact, filtration, tubing, and surface-treatment materials

Custom XPS Study Design for Complex Surface Questions

Submit your sample description, formulation context, suspected issue, or target surface chemistry. Our analytical scientists will design a focused XPS strategy tailored to your material and project objective.

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Our XPS Testing Project Workflow

Assessment

1Project & Sample Assessment

We review the sample type, expected composition, surface question, handling sensitivity, vacuum compatibility, and available background data to determine whether XPS alone or a combined analytical plan is most suitable.

Method Design

2Method Design & Sample Preparation

Our team defines the analysis area, mounting approach, survey and high-resolution regions, charge compensation strategy, and optional depth-profiling or mapping conditions while minimizing handling-related surface contamination.

Data Acquisition

3Data Acquisition & Spectral Interpretation

We acquire survey and narrow-scan spectra, calculate surface atomic composition, assign chemical states, compare representative samples, and perform peak fitting when chemically meaningful and technically justified.

Reporting

4Integrated Reporting & Recommendations

The final report presents spectra, atomic percentages, peak assignments, depth or mapping results when applicable, interpretation notes, and practical recommendations for formulation, process, material, or further analytical decisions.

Solutions for Critical XPS Testing Challenges

01

Surface Contamination Masking Key Signals

Pharmaceutical and polymeric samples can adsorb hydrocarbons, silicone residues, metal traces, or handling-related contaminants that dominate the first few nanometers of the surface. BOC Sciences uses careful sample handling, comparative controls, high-resolution peak interpretation, and optional complementary element analysis to separate meaningful material chemistry from incidental surface contamination.

02

Charging Effects in Organic and Insulating Samples

APIs, excipients, polymers, oxides, and coated particles frequently charge during XPS acquisition, causing binding energy shifts and ambiguous assignments. Our approach combines charge neutralization, reference peak selection, replicate checks, and chemically consistent fitting models to improve confidence when interpreting C 1s, O 1s, N 1s, S 2p, P 2p, and halogen-containing spectra.

03

Distinguishing Surface Enrichment from Bulk Composition

Bulk assays may miss API or excipient segregation at particle surfaces, while XPS may reveal only the outermost chemistry. BOC Sciences integrates XPS with API analysis, XRD testing, thermal analysis, and particle-level characterization to help clients understand whether surface enrichment reflects formulation design, process drift, or material incompatibility.

04

Ambiguous Metal, Oxide, and Inorganic Residue Signals

Metal-containing particles, oxide films, catalyst traces, inorganic excipients, and salts can produce overlapping peaks or multiple oxidation states. We combine high-resolution XPS fitting with reference-informed interpretation and optional ICP testing, XRF, or microscopy-based approaches to distinguish true chemical-state changes from mixed-surface artifacts.

Partner with Experts in Surface Chemical Characterization

Collaborate with BOC Sciences to investigate surface composition, oxidation states, coating uniformity, contamination sources, and material interfaces through expert XPS Testing supported by multidisciplinary analytical insight.

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Why Choose Our XPS Testing?

Surface-Focused Drug Development Insight

We help clients answer surface-specific questions that directly influence formulation behavior, particle performance, coating function, material compatibility, and process troubleshooting.

Interpretation Beyond Raw Spectra

Our reports emphasize chemically meaningful assignments, comparative interpretation, peak-fitting rationale, and project-relevant conclusions rather than isolated spectral outputs.

Multitechnique Analytical Integration

XPS can be combined with Raman testing, thermal analysis, XRD, XRF, chromatography, and microscopy to resolve complex material questions from multiple perspectives.

Flexible Support for Complex Samples

From API powders and polymer coatings to inorganic particles and treated surfaces, our team adapts XPS acquisition and interpretation strategies to the physical nature of each sample.

BOC Sciences' XPS Testing for Diverse Applications

API & Excipient Surface Studies

  • API surface enrichment in blends or particles
  • Excipient adsorption and surface segregation
  • Salt, co-crystal, or functional group changes
  • Surface chemistry comparison across process conditions

Coatings & Drug Delivery Materials

  • Polymer coating composition and uniformity
  • Surface-functionalized nanoparticles and carriers
  • Fluorinated, PEGylated, amine, or phosphate surfaces
  • Oxide, silane, lipid, or surfactant-modified interfaces

Troubleshooting & Material Investigation

  • Unknown residues, stains, and surface particulates
  • Metal oxide and inorganic residue assignments
  • Processing, storage, or contact-surface effects
  • Complementary support for purity determination and material comparison

XPS Testing Case Studies

Client Needs: A formulation team observed variable dissolution behavior in a spray-dried amorphous dispersion containing a weakly basic API and a cellulosic polymer. Bulk assays showed comparable composition, but the team suspected surface-level API enrichment after process scale-up.

Challenges: The sample was electrically insulating, highly organic, and prone to adventitious carbon contamination. The analytical question required differentiating API-specific nitrogen and aromatic carbon signals from polymer-related oxygen-rich surface chemistry.

Solution: BOC Sciences mounted representative powder fractions under low-contamination handling, acquired survey spectra and high-resolution C 1s, O 1s, and N 1s scans across twelve particle areas, and applied charge compensation with consistent C 1s referencing. We compared API-rich spectral markers against polymer-rich controls and correlated findings with DSC testing and XRD results.

Outcome: XPS confirmed higher API-related nitrogen and aromatic carbon contributions at the particle surface in the scale-up batch, supporting process adjustment of drying conditions and feed concentration.

Client Needs: A chemistry group needed to determine whether a pale surface discoloration on an API intermediate was associated with an inorganic oxide, a trace metal-containing residue, or an organic process impurity.

Challenges: The visible discoloration was localized and the total residue level was low. Conventional bulk testing did not reflect the surface chemistry responsible for the appearance change.

Solution: We selected stained and unstained regions for small-area XPS acquisition, collected high-resolution Fe 2p, O 1s, C 1s, and Cl 2p spectra, and used comparative peak fitting to separate oxide, hydroxide, and organic chloride contributions. The XPS evidence was integrated with X-ray powder diffraction and targeted metal screening.

Outcome: The surface discoloration was linked to a thin iron oxide/hydroxide-rich residue rather than a bulk impurity, allowing the client to focus investigation on contact surfaces and final isolation handling.

Client Needs: A drug delivery research team required confirmation that amine-functionalized polymeric nanoparticles retained surface nitrogen functionality after ligand coupling and purification.

Challenges: The functional layer was expected to be ultrathin, and the dried nanoparticles contained overlapping carbon, oxygen, and nitrogen environments from the polymer matrix, linker, and residual processing materials.

Solution: BOC Sciences prepared dried nanoparticle deposits on clean conductive substrates, acquired replicate survey scans and high-resolution N 1s/C 1s spectra, and compared unmodified, activated, and ligand-coupled samples. We used nitrogen chemical-state fitting, surface atomic percentage trends, and control-subtracted interpretation to confirm coupling-associated signal changes while screening for residual salts and processing additives.

Outcome: The XPS dataset confirmed increased surface nitrogen contribution and a shifted N 1s component consistent with ligand coupling, helping the client refine washing conditions and surface functionalization parameters.

Frequently Asked Questions

Frequently Asked Questions

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