Standard Reference Material (SRM) 2944 is a cuvette-shaped, Bi-ion-doped glass, recommended for optimal use for relative spectral correction of emission from 590nm to 805nm and day-to-day performance verification of steady-state fluorescence spectrometers. Properties of this standard that influence its effective use or contribute to the uncertainty in its certified emission spectrum were explored here. These properties include its photostability, absorbance, dissolution rate in water, anisotropy and temperature coefficient of fluorescence intensity. The expanded uncertainties (k=2) in the certified spectrum are about 4% around the nominal peak maximum at 704nm and increase to about 6% at the wings, using an excitation wavelength of 515nm.

Measurements of the chemical compositions of materials and the levels of certain substances in them are vital when assessing and improving public health, safety and the environment, are necessary to ensure trade equity, and are required when monitoring and improving industrial products and services. Chemical measurements play a crucial role in most areas of the economy, including healthcare, food and nutrition, agriculture, environmental technologies, chemicals and materials, instrumentation, electronics, forensics, energy, and transportation.This chapter presents a broad overview of the analytical techniques that can be used to perform the higher order chemical characterization of materials. Techniques covered include mass spectrometry, molecular spectrometry, atomic spectrometry, nuclear analytical methods, chromatographic methods and classical chemical methods.For each technique, information is provided on the principle(s) of operation, the scope of the technique, the nature of the sample that can be used, qualitative analysis, traceable quantitative analysis, and key references. Examples of representative data are provided for each technique, where possible.

Standard Reference Material (SRM) 2942 is a cuvette-shaped, Ce-ion-doped glass, recommended for use for relative spectral correction of emission from 320 to 430nm and day-to-day performance verification of steady-state fluorescence spectrometers. Properties of this standard that influence its effective use or contribute to the uncertainty in its certified emission spectrum were explored here. These properties include its photostability, absorbance, dissolution rate in water, anisotropy and temperature coefficient of fluorescence intensity. The expanded uncertainties in the certified spectrum are about 9% around the peak maximum at 330nm, using an excitation wavelength of 310nm. The SRM also exhibits a strong resistance to photodegradation, with no measurable decrease in fluorescence intensity even after 25h of irradiation with UV light>280nm from a Xe lamp.

Standard Reference Material (SRM) 2943 is a cuvette-shaped, Cu-ion-doped glass, recommended for use for relative spectral correction of emission and day-to-day performance verification of steady-state fluorescence spectrometers. Properties of this standard that influence its effective use or contribute to the uncertainty in its certified emission spectrum were explored here. These properties include its photostability, absorbance, dissolution rate in water, anisotropy and temperature coefficient of fluorescence intensity. The expanded uncertainties in the certified spectrum are about 5% around the peak maximum at 446nm, using an excitation wavelength of 330nm. SRM 2943 can replace SRM 936a quinine sulfate dihydrate, which is no longer sold by NIST, for many applications, as it covers the same spectral range. SRM 2943 is significantly more photostable than organic dyes, but unlike the other fluorescent glass SRMs in this series, it does photodegrade gradually under lamp-based excitation.

Maintaining the integrity of analytical data over time is a challenge. Years ago, data were recorded on paper that was pasted directly into a laboratory notebook. The digital age has made maintaining the integrity of data harder. Nowadays, digitized analytical data are often separated from information about how the sample was collected and prepared for analysis and how the data were acquired. The data are stored on digital media, while the related information about the data may be written in a paper notebook or stored separately in other digital files. Sometimes the connection between this "scientific meta-data" and the analytical data is lost, rendering the spectrum or chromatogram useless. We have been working with ASTM Subcommittee E13.15 on Analytical Data to create the Analytical Information Markup Language or AnIML-a new way to interchange and store spectroscopy and chromatography data based on XML (Extensible Markup Language). XML is a language for describing what data are by enclosing them in computer-useable tags. Recording the units associated with the analytical data and metadata is an essential issue for any data representation scheme that must be addressed by all domain-specific markup languages. As scientific markup languages proliferate, it is very desirable to have a single scheme for handling units to facilitate moving information between different data domains. At NIST, we have been developing a general markup language just for units that we call UnitsML. This presentation will describe how UnitsML is used and how it is being incorporated into AnIML.

Standard Reference Material (SRM) 2940 is a cuvette-shaped, Mn-ion-doped glass, recommended for use for relative spectral correction of emission and day-to-day performance validation of steady-state fluorescence spectrometers. Properties of this standard that influence its effective use or contribute to the uncertainty in its certified emission spectrum were explored here. These properties include its photostability, absorbance, dissolution rate in water, anisotropy, temperature coefficient of fluorescence intensity, and fluorescence lifetimes. Long and short lifetime components of the fluorescence displayed different emission spectra, making the certified spectrum useful with fluorescence instruments employing continuous excitation only. The expanded uncertainties in the certified spectrum are about 5% around the peak maximum at 620nm, using an excitation wavelength of 412nm. The SRM also exhibits a strong resistance to photodegradation, with no measurable decrease in fluorescence intensity even after 17h of irradiation with the visible light from a Xe lamp.

New analytical methods using fluorescence detection are becoming increasingly quantitative and require easy-to-use material standards for fluorometer qualification and method validation. NIST is responding to this need by developing and producing such standards. Reported here is the first step in this process, which is to qualify a research-grade fluorescence spectrometer for measuring true fluorescence spectra of reference material candidates. "True" spectra are defined here as those with fluorescence intensity, either relative or absolute as required, and wavelength both being reported with high accuracy and known precision, after wavelength has been calibrated and corrections for excitation intensity and detection system response have been applied. The uncertainties determined in relative and absolute intensity-corrected fluorescence spectra using both calibrated source (CS)- and calibrated detector (CD)-based methods were compared. The CS-based method gave uncertainties, typically about +/-5% for relative spectral correction, that were about half that of the CD-based method for determining both relative and absolute spectral correction factors. Absolute spectral correction factors can be determined using either method without knowing the optical geometry of the instrument. The absolute spectral correction factors were found to have much larger uncertainties than the corresponding relative correction factors with uncertainties for the CS-based method of +/-10% to +/-15% being typical and +/-20% or more not being uncommon, particularly for excitation and emission wavelengths below 400 nm. Uncertainties arising from detection system nonlinearity and instrument polarization ratios were also explored.

Standard Reference Material® (SRM®) 2941 is a cuvette-shaped, uranyl-ion-doped glass, recommended for use for relative spectral correction of emission and day-to-day performance validation of fluorescence spectrometers. Properties of this standard that influence its effective use or contribute to the uncertainty in its certified emission spectrum have been explored here. These properties include its photostability, absorbance, dissolution rate in water, anisotropy, temperature coefficient of fluorescence intensity, and fluorescence lifetimes. The expanded uncertainties in the certified spectrum are about 4% around the peak maximum at 526nm, using an excitation wavelength of 427nm. The SRM also exhibits a strong resistance to photodegradation, with no measurable decrease in fluorescence intensity even after 8h of laser irradiation.

The scope of this project covers the storing of result data produced by generic laboratory devices during processing of analytical experiments, the data describing the examination methods, and the audit trail using the Analytical Information Markup Language (AnIML) standard. This project also considers the integration of generic devices in automated laboratory environments. AnIML is an upcoming ASTM standard format for recording analytical data and workflows with accompanying experimental metadata. Adapting this standard to existing instruments currently requires manual intervention. The goal of this project is to automate as many steps as possible in generating an AnIML document with all its essential information supplied directly by the analytical instrument. Software with such functionality could be integrated into analytical instruments or reside in firmware boxes hooked to the instruments. This would allow a smooth transition to the new standard even in complex existing environments. A set of prerequisites have to be fulfilled before the feasibility of this approach can be shown. The prototype application we describe here integrates the generic description of an instrument using the Laboratory Equipment Control Interface Specification, Object Management Group (LECIS OMG) Device Capability Dataset. Information about the device's commands and the device's data stream with its semantics can be found there. The experiment's metadata are provided by the test order. In both cases, XML schemas contain the information syntax. Using this information, we developed a generic interface that maps the result stream semantically and then transforms it into an AnIML document without manual intervention. At this time, we have completed and tested a prototype implementation and are working to support the full functionality of both the LECIS OMG and the ASTM AnIML standards. (JALA 2006;11:247–53)

SpectroML, a markup language for ultraviolet-visible spectroscopy data, has been developed as a “Web-aware” mechanism for instrument-to-instrument, instrument-to-application, and application-to-application data interchange and archiving. This article documents the application of SpectroML to the interchange and archiving of measurement data from three spectrophotometers that are used in the NIST optical filter standards program. It describes how result data from the NIST national reference spectrophotometer and two commercial spectrophotometers are converted into SpectroML format and how SpectroML-formatted data and metadata are imported into the optical filter standards database.

The Analytical Information Markup Language (AnIML) is a standardization effort of ASTM (formerly American Society for Testing and Materials) Subcommittee E13.15 on Analytical Data. AnIML provides an XML-based format for analytical data. It is designed specifically for spectroscopy and chromatography data, but is suitable for use with many different analytical measurement techniques. AnIML consists of a generic core structure that permits the storage of arbitrary analytical data. These include multi-dimensional data, name-value pairs, and hierarchies. The concept of technique definitions permits the formal specification of constraints for usage of the core. This way, a definition can prescribe how the data for specific measurement techniques should be captured in the data file. To address changing requirements, AnIML supports an extension concept that allows vendors or end users to specify additional data that should be stored for a technique. These extensions can also be formally documented so that they do not break compatibility with existing software. This article presents an overview of AnIML and demonstrates how AnIML can be used to record data from everyday experimental workflows in a laboratoryenvironment. Issues related to the usage of AnIML in regulated environments are also discussed, including the use of digital signatures and audit trail functionality to ensure data integrity.

We have recently begun to explore the use of UV laser ablation micromachining to construct microfluidic devices in polymers. This technique can create microchannels rapidly and modify the resulting polymer surface in a single step. By ablating under different atmospheres, it is possible to alter both the surface chemistries and physical surface morphologies of the microchannels. We have employed electroosmotic flow measurements, chemical mapping, and optical microscopy to characterize the microfluidic devices. In addition, we have studied the parameters affecting the ablation, such as the laser wavelength, laser fluence, laser firing repetition rate, and the material being ablated.