Patent Application
20150074015
The present invention relates to reference materials for use in calibrating analytical instruments.
Analytical instruments, such as inductively coupled plasma spectrometers (“ICP”), ICP-mass spectrometers (“ICP-MS”), gas chromatographs (“GC”), liquid chromatographs (“LC”), mass spectrometers (“MS”), and the like require routine calibration. Calibration is typically performed using a “standard,” such as commercially purchased reference sample (“RM”), or certified reference sample (“CRM”).
The CRM is a sample of one or more compounds, materials, etc., of known weight and chemical analysis. The specifics of the CRM, including its packaging, sample size, and phase (gas, liquid, solid), is a function of the analytical device being calibrated as well as the intended analytical application. CRMs include, for example, organic standards for GC, GC-MS, LC, and LC-MS. CRMs additionally include inorganic standards for calibrating atomic absorption spectrometer (“AA”), ICP, ICP-MS, ion chromatograph (“IC”), ion selective electrode (“ISE”), and X-ray fluorescence-fusion (“XRF-fusion”), among others. A certificate that includes a certified analysis for the each CRM is available from the supplier thereof. CRMs and certificates of analysis are available from SPEXCertiPrep of Metuchen, N J and others.
An analytical instrument is calibrated using a CRM in the following manner. A suitable CRM and corresponding certificate of analysis is obtained from a supplier. An operator keys the analysis information from the certificate into the computer that controls the analytical instrument. The CRM sample is introduced into the instrument requiring the calibration and is analyzed. Calibration software compares the response generated by the not-yet-calibrated instrument against the certified analysis from the certificate, as input by the operator.
To the extent the instrument response and the certified analyses deviate from one another, the instrument is adjusted via an appropriate calibration algorithm, in known fashion. The instrument is thus “calibrated,” at least for compounds found in the CRM.
This calibration process is subject to a variety of sources of human error, a few of which pertain directly to the CRM and its corresponding certificate of analysis. First, simple transcription errors can be made by the individual responsible for inputting the certified analysis. Second, an individual responsible for inputting the certified analysis might use the “nominal” concentration of the sample, rather than the actual concentration. For example, the nominal concentration of a sample might be 100 mg/L, but the actual concentration of the sample, as reported on the certificate of analysis, might be 99.8 mg/L. Depending upon the particular type of analytical method/instrument requiring calibration, this can introduce small systemic errors into a “calibrated” instrument.
Embodiments of the invention provide a way to improve the calibration process for an analytical instrument by reducing sources of human error. In accordance with the illustrative embodiment of the invention, packaging for a certified reference material (or a reference material) comprises a storage medium for storing a first information product in machine-readable form. The term “certified reference material” or “CRM” will hereinafter be used to refer to both certified reference materials and reference materials. The first information product is either:
The first information product, being machine readable, can be, without limitation, in the form of digitized information conveyed acoustically, chemically, electrically, magnetically, mechanically, or optically. It can be in the form of a physical image, wherein in some embodiments, the first information product (i.e., the information content of the first information product) is in a form that is not understandable to an unaided human viewer on inspection of the image. For example, if the first information product is in the form of a bar code (without accompanying alphanumeric characters) or a QR code, a human viewer will not be able to tell what alphanumeric characters are represented by simply viewing these codes; a bar code or QR code reader will be required for that. In some other embodiments, the information conveyed by the first information product is in a form that is understandable to a human viewer on inspection. For example, the first information product can be in the form of written language, such as a pictogram, an ideogram, a string (i.e., an ordered set of symbols, alphanumeric or otherwise). In some embodiments, even if the first information product is understandable to an unaided human viewer, it will be machine readable, such as by optical character recognition (“OCR”), or, if formed of magnetic ink characters, by magnetic ink character recognition (“MICR”). The phrases “[first] information product” and “information content of the [first] information product” are used synonymously herein.
The CRM package can be in the form of a bottle, ampule, vial, dromedary bag or any other vessel/container typically used by suppliers to store and transport reference materials or certified reference materials.
The storage medium can be, without limitation, a physical image (e.g., a bar code, a QR code, written language, etc.), an electronic chip/circuit (e.g., RFID tag, NFC tag, smart card, etc.), an optical storage medium (e.g., hologram, cd, dvd, etc.), or a magnetic storage medium. The storage medium can appear: (i) directly on a surface of the packaging, (ii) on a label/substrate on the surface of the packaging, (iii) be embedded in the packaging.
In some additional embodiments, the first information product is encoded in the CRM itself. In these embodiments, the first information product is obtained or “extracted” by analyzing the CRM via the (un-calibrated) analytical device or some secondary analytical device. For example, in a CRM comprising a protein array or chip, a number of additional unique proteins are added (sufficient to provide about 16-24 bits of information) to the standard proteins. A symbol (e.g., alphanumeric character, etc.) is assigned to each additional protein such that the additional proteins collectively define a string that codes the lot number for the protein array. Thus, to obtain the certified data analysis, the CRM must be analyzed.
In some further embodiments, the first information product is contained in a data storage device that is coupled to the CRM packaging (e.g., such as via a cord, etc.), wherein such devices include, without limitation, an NFC or RFID tag, a USB flash drive, or an SD card.
In still further embodiments, the first information product appears on a sales receipt/invoice/order confirmation for the CRM. In such embodiments, the first information product will typically be in the form of a bar code, a QR code, or written language.
The first information product is initially processed via specialized application software, referred to herein as the “eCert Data Application,” that is installed on (i) the computer that runs the analytical instrument or (ii) an “auxiliary” device, such as a tablet (e.g., iPod Touch®, iPhone® iPad®, Android-based device, or similar device). As discussed further below, the eCert Data Application is capable of performing one or more of the following tasks, in addition to any others:
In embodiments in which the eCert Data Application is installed on a computer that runs the analytical instrument, the first information product accompanying the CRM packaging is made available to the eCert Data Application, such as via scanners, readers, input devices, etc., that transmit the first information product to the computer. If the first information product is a pointer (e.g., a lot identifier or the like) to the certified analysis data, then the eCert Data Application causes the computer to connect to the CRM supplier's data processing system (e.g., server(s) and processor-accessible memory) via the Internet, etc., and download the certified analysis. If the first information product is the certified analysis itself, then the retrieval operation from the supplier's data processing system is skipped. Once imported, the eCert Data Application populates appropriate fields with the certified analysis data and performs other processing to prepare a second information product for transmission to the instrument software for calibration of the analytical instrument.
In some cases, the computer that controls the analytical device will not have Internet connectivity. In such embodiments, an auxiliary device that has Internet connectivity, such as smart phone, Wi-Fi-equipped device (such as an iPod Touch®) or tablet, etc., can be used. When used in conjunction with an auxiliary device, the eCert Data Application is typically implemented in two different instantiations. In particular, a modified version of the eCert Data Application that includes some but not all of the functionality of the full Application is installed on the auxiliary device and the full eCert Data Application is installed on the computer that controls the analytical device. For example, in some embodiments, the modified version of the eCert Data Application installed on the auxiliary device is capable of obtaining the certified analysis data but is not capable of performing some of the further processing that is normally implemented via the full eCert Data Application (discussed later in this Specification).
The first information product pertaining to the CRM is made available to auxiliary device by, for example, using (i) the auxiliary device's camera, (ii) peripheral devices that can be physically attached to the auxiliary device, such as bar code scanners, etc., or (iii) devices that “attach” via a computer telecommunications protocol, such as Bluetooth, Wi-Fi, Zigbee, etc., to read, for example, NFC tags or RFID tags. If the first information product is a pointer to the certified analysis, the modified eCert Data Application causes the auxiliary device to wirelessly connect to the CRM supplier's data processing system via the Internet, etc., and obtain the certified analysis data. If the first information product is the certified analysis itself, then the retrieval operation from the manufacturer's data processing system is skipped. In either scenario, the auxiliary device obtains the certified analysis data and then transmits it to the computer that controls the analytical instrument.
In some embodiments, the invention provides a system for disseminating a first information product pertaining to a certified reference material, wherein the system includes the certified reference material and a package that contains the certified reference material, wherein the package comprises a storage medium for storing a first information product in a machine-readable format, wherein the first information product comprises at least one of: (a) a pointer for accessing certified analysis data, in a machine-readable format, pertaining to the certified reference material; or (b) the certified analysis data.
In some additional embodiments, the invention provides a system for disseminating a first information product pertaining to a certified reference material, wherein the system includes the elements disclosed in the preceding paragraph as well as a data processing system, wherein the certified analysis data is stored in a memory accessible to the data processing system and is accessed via the pointer.
In further embodiments, the invention provides a method comprising the tasks of adding a quantity of a certified reference material to a package, incorporating, on the package, a storage medium for storing an information product in a machine-readable format; and encoding the first information product in the storage medium, wherein the first information product comprises at least one of: (a) a pointer for accessing certified analysis data, in a machine-readable format, pertaining to the certified reference material; or (b) the certified analysis data.
In another embodiment, the invention provides a method that includes the tasks disclosed in the preceding paragraph as well as the tasks of receiving, at a data processing system, a request from a requestor to transmit certified analysis data corresponding to the certified reference material; and transmitting the certified analysis data to the requestor.
In yet a further embodiment, the invention provides a computer-readable non-transitory medium containing program instructions for obtaining, organizing, and transmitting certified analysis data for calibrating an analytical instrument, wherein execution of the program instructions by one or more processors of a computer system causes the one or more processor to carry out the tasks of:
Additional embodiments of the invention are disclosed in the Detailed Description section of this Specification.
Definitions. The terms appearing below and any inflected forms thereof, are provided with the follow explicit definitions for use in this description and the appended claims.
System 100A includes computer 102, analytical instrument 112, and CRM packaging 114 containing CRM 116, interrelated as shown.
Computer 102 is a general purpose computer, and includes processor 104 and processor-accessible storage 106. Processor 104 is capable of, among other tasks, running the operating system of computer 102, executing specialized application software (discussed further below), and populating, updating, using, and managing data in processor-accessible storage 106.
Instrument software 106 is typically provided by the manufacturer of analytical instrument 112. The instrument software provides standardized or custom platforms for controlling analytical equipment 112. The functionality of instrument software 106 includes, without limitation, instrument control 124, instrument calibration 126, data acquisition 128, and data analysis 130. The nature and operation of the instrument software is well known to those skilled in the art.
The e-Cert Data Application 110, which is unique to embodiments of the present invention, is discussed extensively below and throughout this Specification.
With continued reference to
Analytical instrument 112 can be any of a wide variety of instruments suitable for the analysis and characterization of inorganic and organic compounds, as known in the art. For example, and without limitation, analytical instrument 112 can include a gas chromatograph, a gas chromatograph-mass spectrometer, a liquid chromatograph, liquid chromatograph-mass spectrometer, atomic absorption spectrometer, inductively coupled plasma spectrometer, inductively coupled plasma-mass spectrometer, ion chromatograph, and X-ray fluorescence.
CRM 116 is used to calibrate analytical instrument 112. Knowing that uncharacterized samples that are to be analyzed by instrument 112 will likely contain a set of specific analytes, but not knowing which analytes or the amounts thereofs in the samples, an instrument operator will obtain from a supplier an appropriate CRM for the calibration process. An “appropriate” CRM is one that includes many of the analytes that are expected to be present in the as-yet uncharacterized samples. More than one CRM may be required to calibrate the instrument in preparation for analyzing a given sample.
In accordance with the illustrative embodiment, CRM packaging 114 comprises storage medium 118 comprising a first information product 120. As discussed further below, first information product 120 is either a “pointer” to a machine readable version of the certified analysis data corresponding to the selected CRM, or it is a machine readable version of the certified analysis itself. In the illustrative embodiment, the pointer is a CRM lot number.
In some embodiments in which information product 120 is a pointer, the certified analysis data corresponding to the selected CRM is stored in memory locations that are accessible by the CRM supplier's data processing system. In some alternative embodiments, first information product 120 is encoded in the CRM itself. In yet some further embodiments, first information product 120 is stored in a device that is coupled (a memory stick, etc.) to CRM packaging 114 or is otherwise associated (an invoice, sales receipt, etc.) with the CRM.
The certified analysis data is “automatically” entered into eCert Data Application 110 that is installed on computer 102 in accordance with the illustrative embodiment. This enables an operator to avoid having to manually enter (e.g., via typing, etc.) the values that appear in a conventional certificate of analysis that is available for each CRM. Although, in some embodiments, an operator manually enters the “pointer” (e.g., lot number of the CRM, etc.) into the device that will access the certified analysis data (for “automatic” entry into the eCert Data Application). In some alternative embodiments, the eCert Data Application (or a modified version thereof) is installed on an auxiliary device, such as when computer 102 lacks connectivity to CRM supplier's data processing system.
Either before or after the certified analysis data is accessed by eCert Data Application 110, information pertaining to a selected “instrument method” by which the analytical instrument performs its analysis is also accessed by the eCert Data Application. The selected instrument method, with is normally one of a number of instruments methods available for selection, is part of the Instrument Software 108. Among other information, the instrument method will provide a list of analytes, and the wavelengths, masses, delay times, etc., at which the instrument will check for such analytes when it analyzes a sample.
In task 103, eCert Data Application “matches-up” the amounts of analytes from the certified data analysis with the list of analytes provided in the selected instrument method, thereby generating a second information product. The second information product, which includes the certified analysis data, is transmitted to instrument software 108 and populates same, per tasks 105 and 107.
In accordance with task 109, CRM 116 is analyzed by analytical instrument 112. There will be a deviation between the response of the uncalibrated instrument (i.e., the calculated concentration of each analyte in CRM 116) and the certified values for the concentration of those analytes in CRM 116. Instrument software 108 uses this information, in conjunction with calibration data, in ways known to those skilled in the art (instrument calibration functionality 126) to calibrate analytical instrument 112, per task 111. The analytical instrument can then be used to analyze uncharacterized samples.
A key aspect of embodiments presented herein pertains to task 101—obtaining a machine-readable version of certified analysis data via the first information product.
With continued referenced to
Additional description of the manner in which a machine-readable version of the certified analysis data is obtained provided later in this Specification (see, e.g.,
In CRM package 314A depicted in
In
In the embodiments depicted in
Of course, when shipped, the CRM packages depicted in
A format-appropriate peripheral device is used to “extract” first information product from the CRM packages. For example, a bar code reader, a QR code reader, and optical character reader are used, respectively, to obtain the first information product from respective bar code 346, QR code 348, and string 350. Likewise, an RFID reader is used to capture the first information product from RFID tag 452, an NFC reader is used to obtain the first information product from NFC tag 454, and a smart-card reader is used to obtain the first information product from smart card 456. Unless otherwise integrated into computer 102 or auxiliary device 238, these peripheral devices communicate over a wired or wireless data link to the computer or auxiliary device to provide the first information product thereto.
Although
Per task 502, the eCert Data Application is opened by a user. The eCert Data Application (or a modified version thereof) resides on computer 102 or auxiliary device 238 (
Referring now to
Per optional task 702 of method 700, a user enters credentials, such as a user name, password, and any other identifying, authenticating, of personal information required for access to the supplier's data processing system. The user's credentials are transmitted to the supplier's data processing system at task 704. The data processing system determines whether the user is authorized per query 706. If the user is not authorized, the user is so notified at task 708. If the user is authorized, at query 710, inquire whether updates to the eCert Data Application are available. If not, processing advances to task 504 of
Referring again to
Per task 904, the eCert Data Application causes computer 102 or auxiliary device 238 to transmit the pointer and user credentials to the CRM supplier's data processing system. The data processing system determines, at query 906, whether the user is authorized to access the data processing system. If not, then access is prevented and the user is notified at task 908. If user credentials were previously supplied during the user's current interaction with the data processing system (see, e.g., tasks 702 through 708 of method 700 at
The CRM supplier might not want to provide a user with access to certified analysis data for a CRM that the user has not ordered. To that end, method 802A includes query 910, wherein the data processing system determines from supplier records whether the user has in fact ordered the CRM that is the subject of the user's inquiry. If not, download of the certified analysis data is prevented and the user is so notified per task 912.
If the user has ordered the corresponding CRM, the data processing system determines at query 914 whether the CRM has expired. Each CRM will have an expiration date, which is necessitated due to potential degradation of the included analytes or permeation thereof through the packaging.
If the CRM has expired, the data processing system determines whether it is has been recertified, per query 920. If the CRM has not been recertified, the user is notified at task 922 and, optionally, download of the certified analysis data is prevented. If the CRM has been recertified then, at task 924, the user is notified and a new identifier for that CRM lot, as appropriate, is provided to the user. Recertification is based on follow-up testing that shows that the original certified analysis for the CRM is still valid.
If, at task 914, the data processing system determines that the CRM has not expired, query 916 determines whether the CRM is to expire within a timeframe that is considered by the supplier to be “impending” or “soon” (e.g., within 1 month, etc.). If expiration is determined to be impending, then the user is notified and provided with an option to re-order the CRM per task 918.
Following a negative determination at query 916, or following tasks 918 or 924, the certified analysis data is downloaded to the computer/auxiliary device according to task 926.
Returning to
Method 802B is analogous to task 902 of method 802A. That is, the method involves extracting the certified analysis data from:
The third method disclosed for obtaining the certified analysis data is to retrieve a C.A. (certified analysis) file. This method is applicable in situations in which a user has previously obtained the certified analysis data (either via method 802A or 802B) and, during the course of processing (as discussed later in conjunction with
Thus, method 802A (see,
With reference to task 1002 of
The user is queried by the eCert Data Application at 1004 as to whether certified analysis data corresponding to an additional CRM is to be required. Such additional information will be necessary, for example, when the instrument “method” that is selected (see task 1008) requires certified data for analytes that are not present in the first CRM. If such additional information is required, then processing returns to task 504 of the method depicted in
If the user responds in the negative to query 1004, then at task 1006, the user select a dilution factor, if appropriate, and the eCert Data Application adjusts the certified analysis data to account for the specified dilution. Such dilution might be necessary, for example, if the concentration of the analytes in the CRM is too high for the analytical device being used or the expected range of the unknown sample that will be analyzed.
At task 1008, the user selects an instrument method, which is then imported at task 1010 from the instrument software into the eCert Data Application. The instrument method, which is familiar to those skilled in the art, will provide a listing of analytes and, for example, one or more wavelengths, masses, delay times, etc., at which the instrument will check for such analytes.
Per task 1012, the certified analysis data is matched up with the analytes listed in the instrument method (see
With reference now to
After saving the data in the C.A. File, or choosing not to save it, the CRM is analyzed by analytical instrument 112 at task 109 of method 100C. Those skilled in the art will know how to use any of a variety of analytical instruments to analyze the CRM.
The response of analytical instrument 112 is reported to the instrument software. This information, and well as the certified analysis data, is used at task 111 to calibrate analytical instrument 112 via instrument calibration functionality 126 of instrument software 108. The selection of appropriate calibration curves, and the application of the certified analysis data and instrument response thereto, is within the capabilities of those skilled in the art.
Task 1202 recites adding a quantity of a certified reference material to a package. This task is performed by the CRM supplier, typically after the certified analysis has been performed. Per task 1204, a storage medium for storing the first information product that is to accompany the CRM is incorporated in the package that is to contain the CRM. The first information product is stored/encoded in the storage medium, per task 1206.
It is important to note that, depending on the nature of the storage medium, the encoding of the first information product can occur simultaneously with the creation of the storage medium and, in some case, with its incorporation in/on the package. For example, the lines comprising a bar code encode the first information product. So, the storage medium is formed and the first information product is encoded simultaneously. In embodiments in which the bar code appears directly on a surface of the CRM package, the incorporation of the storage medium (bar code) on the package occurs simultaneously with the creation of the storage medium and with the encoding of the first information product. Thus, depending on the nature of the storage medium and the manner in which it is incorporated in the CRM package, tasks 1204 and 1206 can occur simultaneously.
Method 1200A is thus directed to CRM packaging and, more generally, to a method for disseminating information pertaining to a certified reference material. Method 1200B extends method 1200A, reciting tasks 1208 and 1210. Per task 1208, receiving, at the CRM supplier's data processing system, a request to transmit certified analysis data corresponding to the CRM to a requestor thereof. At task 1210, the requested information is transmitted to the requestor.
In the methods described thus far, a first information product is extracted from a storage medium that, in most embodiments, is coupled to the CRM packaging. The first information product is a pointer to the certified analysis data or the certified analysis data itself. If the first information product is a pointer, the pointer is then used to obtain the certified analysis data, such as by triggering a download or email from the CRM supplier's data processing system. In some additional embodiments, a purchaser of a CRM contacts (e.g., via phone, e-mail, etc.) the CRM supplier after ordering a CRM and requests that the certified analysis data be forwarded to the purchaser, such as via e-mail. In some further embodiments, a purchaser can visit the website of the CRM supplier to request and download the certified analysis data. Additionally, in some embodiments, the purchaser can obtain the certified analysis data from a “cloud”-based file repository, such as DropBox™, Microsoft SkyDrive, etc. Also, in some embodiments, when a user places an order for a CRM, certified analysis data is automatically transmitted to the purchaser via a cloud-based file repository. In all such embodiments, the file comprising the certified analysis data is in machine-readable format (e.g., such as an Excel file, .csv, a custom XML file, etc.) for importation into the e-Cert Data Application.
The CRM page also depicts the various analytes in the CRM, the nominal concentration of each analyte, the certified value (i.e., the certified analysis data), and the concentration after dilution. The latter value is calculated by applying the user-entered dilution factor (“10” in this example) to the certified values.
It is to be understood that the disclosure teaches just one example of the illustrative embodiment and that many variations of the invention can easily be devised by those skilled in the art after reading this disclosure and that the scope of the present invention is to be determined by the following claims.
