Methods and apparatus for spectroscopic identification and/or calibrated quantification of surface concentration of materials

Inventors

Reid, Michael R.

Assignees

Photon Systems Inc

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Publication Number

US-10732037-B1

Patent

Publication Date

2020-08-04

Expiration Date


Abstract

Apparatus and methods for creating deposits of uniformly spaced or uniformly overlapping droplets of selected chemicals where each droplet has an a priori known amount of the selected chemical or chemicals is taught (including biological and microbial materials). In some embodiments the deposits may be used as samples of different but known concentrations that may be used to calibrate spectroscopic inspection instruments to enable such instruments to not only provide identification in situ of unknown materials but also to provide calibrated and traceable surface concentrations of such materials. In some embodiments, such calibrated instruments may be used in enhanced processes for validating the cleanliness of manufacturing surfaces such as surfaces of equipment used in the preparation of pharmaceuticals, food, or semiconductor devices. Such instruments may be used to ensure adequate purity, or non-contamination, of surfaces of products themselves or packaging materials or of locations where such products will be used. Such calibrated instruments may also be useful in detecting cleanliness of non-manufacturing surfaces where contamination may be of concern, whether they be public or private spaces such as laboratories, restaurants, airports, satellites or other spacecraft. In some embodiments, such instruments may range from deep UV instruments to far infrared instruments or beyond.

Core Innovation

A method calibrating a spectroscopic surface analysis instrument is described as providing both identification of trace materials of interest and quantitative indications of concentrations of one or more materials of interest. The instrument includes a housing, a source capable of producing and directing excitation radiation onto a surface to be examined, at least one optical element for receiving emission radiation from a location on the surface, a detector for receiving at least a portion of the emission radiation, and control electronics for operating the instrument.

The calibration approach includes creating and storing quantitative calibration data and operating the instrument in a calibration mode. In the calibration mode, the instrument provides excitation radiation onto a plurality of sample surfaces in a serial manner, where each sample has a known material with at least one known concentration. The method collects data from emission radiation returned from each sample while the proximal end of the instrument is located within a known spatial separation distance from each sample.

The collected data is processed to provide calibration data for a desired range of concentrations for a specific material. Upon use of the instrument to examine a surface to be tested, which may have an unknown material thereon, the obtained emission radiation is compared to the calibration data to ascertain information about the type and quantity of material of interest that is present for quantitative indications.

The described system further supports calibrated, traceable quantitative surface/areal concentrations using calibration samples that are read by the spectroscopic instrument to generate calibration data over desired concentration ranges, including workflows that support concentration-to-signal comparisons and calibration data representations such as linear or quadratic fits.

Claims Coverage

The partial content includes four independent claims. Across these claims, the inventive focus is on calibrating a spectroscopic surface analysis instrument to determine material identity and/or quantitative concentration information using calibration-mode serial measurements on known-concentration sample surfaces at a known spatial separation distance, along with associated determination logic and calibration-data creation/storage. A further independent claim adds an environmental/facility context for chemical handling equipment and chemical handling machines.

Instrument calibration combining trace material identification with quantitative concentration indications

A method that calibrates a spectroscopic surface analysis instrument to provide both identification of trace materials of interest and quantitative indications of concentrations of one or more materials of interest, using instrument components and electronic determination circuitry that recognizes whether emission radiation corresponds to selected materials and yields concentration, above predefined level, or below predefined level determinations.

Calibration mode serial measurements to create and store quantitative calibration data for concentration ranges

A method that calibrates a spectroscopic surface analysis instrument by operating in a calibration mode to provide excitation radiation on a plurality of sample surfaces in a serial manner, collecting emission radiation data while the proximal end is located within a known spatial separation distance from each sample, and processing the data to provide calibration data for a desired range of concentrations; then comparing emission radiation from an unknown surface to the stored calibration data to ascertain quantity information.

Calibration data creation and stored quantitative calibration data for concentration determination

An electronic circuit provides for creating and storing quantitative calibration data, with additional electronic circuitry for determining a concentration level associated with emission radiation from a selected material as an actual concentration or as above a predefined level or below a predefined level.

Chemical handling facility and chemical handling machine context

A method wherein the chemical handling equipment comprises equipment in a chemical handling facility selected from pharmaceutical, food, explosives, nanoparticle, semiconductor, or research laboratory and wherein the chemical handling facility comprises a facility selected from manufacturing, packaging, or transportation, and wherein the chemical handling equipment is a chemical handling machine selected from ingredient processing, ingredient mixing, packaging, transportation, a vehicle, or a dispensing machine.

Overall, the independent claims require calibration-mode serial measurements on sample surfaces with known material concentrations at a known spatial separation distance, the creation and storage of quantitative calibration data, and electronic determination logic that maps emission radiation to material identity and/or concentration determinations, including above/below predefined levels. One independent claim additionally specifies a broad chemical handling facility and chemical handling machine context.

Stated Advantages

Provides identification of trace materials of interest.

Provides quantitative indications of concentrations of one or more materials of interest, including concentration determinations or above/below predefined level determinations.

Enables comparison of emission radiation from an unknown surface to stored calibration data to ascertain type and quantity of material of interest.

Provides calibration data for a desired range of concentrations of a specific material.

Documented Applications

Cleaning verification/validation and rapid re-clean decision loops are described as applications supported by the calibrated, traceable quantitative surface/areal concentration indications.

Calibrating and using spectroscopic surface analysis instruments for trace material identification and calibrated quantitative areal concentration indication on surfaces are described as the document’s main use case.

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