Pittcon 2008: Back to New Orleans and Coffee and Beignets for Breakfast

Article

Spectroscopy

SpectroscopySpectroscopy-05-01-2008
Volume 23
Issue 5

John Coates presents a comprehensive review of the products and accessories introduced at Pittcon this year.

Before getting on with the job of reporting, I would like to make some brief editorial comments. One is to the various people who have provided me with information for this article. I would like to say thank you for getting the materials to me. However, I am certain that my review is far from complete. I have done my best by soliciting materials through the Spectroscopy staff, and on my own by dedicating three days of scouring the show for new products and new product information.

How was Pittcon 2008? For me, it was a good show. There were some interesting new products, and there was a continuation of some trends observed last year. There was a welcome increase in Raman products and quite a broadening of products for Raman spectroscopy. Some years back, in fact quite a good few years back, I commented on the fact that Raman always seemed to come up short and it did not meet its original expectations. I was criticized for these comments, and I willingly accepted the criticism at that time. Unknown to some, although I have been better known for work in infrared spectroscopy, I actually have had an active passion for Raman, back to the days when the technique was first introduced with lasers. At the time, the technique was known as "laser Raman spectroscopy." I actually even wrote a chapter in a book about the use of Raman in the oil and petroleum industries (3). This work was started in 1971 as part of my postgraduate work. My passion for Raman stems from the simplicity of the technique in terms of sample handling. It is an ideal technique to be included as a component in the famed Tricorder (for Star Trek buffs). You shine a laser on the subject and you get information back that leads to a material's identification —what could be better? That has to be the panacea for an analytical chemist.

Table I: Products introduced at Pittcon 2008

As we all know, life has not been that easy for Raman spectroscopy. However, some of the key obstacles are starting to be removed and we are becoming more accepting. My rule of thumb for years has been that good enough is OK. Thankfully, people are waking up to this fact for Raman, and people are no longer striving for ultimate resolution of ultimate stability for low-cost laser systems. We now see commercial Raman systems with 10-cm–1 and 15-cm–1 spectral resolution. This is OK because for a lot of applications this is adequate, and good enough is OK! Also, if you accept that 15 cm–1 is OK, then you can lower your laser stability requirements, and suddenly, low-cost solid-state lasers become acceptable. Because of the continued trend in Raman, I will provide a bit more focus on the topic in this article.

Table I (continued): Products introduced at Pittcon 2008

Another area in which we are seeing a meaningful and welcome trend is in portable and handheld instrumentation. At the show this year we saw three new handheld Fourier transform (FT)-IR products (actually, strictly two because two have common ancestry) and a palm-sized Raman instrument. Although not strictly handheld, there were several examples of portable instruments — several FT-IR and Raman products, as well as UV–vis products. Field-portable and handheld are starting to become a mantra in the analytical instrument business, and regular benchtop instruments tend to be somewhat passé, although they should not be ignored! There are some excellent new benchtop instruments, and like the trend from desktop to laptop computers, the benchtop products are becoming great value for the money. And, we must not ignore the enabling technologies. There were a good number of new components and core technology products introduced, as well as accessories. It is worth remembering that these products, often displayed in 10- or 20-ft booths, can become the mainstay of the industry. These technologies ultimately make real applications work, and they enable brand new market/business opportunities for the analytical industry. I have quoted this before, but in the past, the analytical instrument industry was likened to a collection of cottage industries. For me, this statement is now more appropriate than ever.

New and Recent Instrument Product Offerings

Based upon my earlier comments, I will start with a brief and partial focus on Raman spectroscopy. There may be some cross-referencing because in some cases there are companies that offer products in other areas of spectroscopy. I will continue the review in more of a company-biased approach than applications- or technique-biased.

As noted, in terms of what is new and where the trends are, Raman was probably one of the strongest showings in "new spectroscopic products" at Pittcon 2008. While the traditional major players either continue to offer products or have new, updated Raman instrument offerings, it is the smaller, emerging companies that are offering some of the major advancements in the science. It is pleasing to see that people are starting to realize that Raman does not have to be an expensive technique, and that we can make the products smaller. Ocean Optics (Dunedin, Florida) started this ball moving back in the late 1990s based upon their low-cost modular fiber-optic spectrometers. These products were picked up at the time by Raman Systems (originally based in Massachusetts, and now based in Austin, Texas). Raman Systems featured its handheld Raman spectrometer systems that were originally developed for field-based military applications.

A relatively new company, Enwave Optronics (Irvine, California), has introduced a series of cost-effective Raman instruments that start in the under-$10K mark. Enwave introduced a series of relatively small (4 in. × 6.5 in. × 8.25 in. being the smallest), cost-effective units presented with a small laptop with the same footprint. The most compact and least expensive was the EZRAMAN-LE, which provides 10-cm–1 resolution (spectral range of 150–3300 cm–1). Over the years, we have learned in both infrared and Raman that many practical applications of the techniques simply do not need high-resolution spectral data. For those requiring (or maybe perceiving to require) better resolution, there is the EZRAMAN-M, which offers 5-cm–1 resolution (spectral range 100 cm–3300 cm–1). These instruments are described as being field-portable, and they weigh in at a mere 6 lb. A 5-h battery system is offered for field portability. My guess is that the weight does not include the battery.

Another company that has been involved in the world of smaller, cost-reduced Raman instruments for a few years now is B&W Tek (Newark, Delaware). This company offers basic spectrometers, detectors, and also fully integrated Raman systems. Three products displayed at Pittcon were the BTC161E/162E series of high-throughput, thermoelectric cooled charge-coupled-device (CCD) spectrometers, intended as OEM building blocks and ideal for Raman; the BTR113A MiniRam II, a fully integrated Raman system; and the i-trometer, a miniature back-thinned CCD spectrometer. The Raman system provides a 10-cm–1 resolution with a spectral range of 175–3150 cm–1. The standard laser wavelength is 785 nm, although 473 nm, 532 nm, and custom wavelengths are available. The system measures 10.1 in. × 8.3 in. × 4.5 in. and weighs 6.8 lb, making it a good candidate as a portable system (a battery pack is included). Sampling-wise it provides fiber-optic interfacing as well as a plug-in cuvette-style interface.

DeltaNu (Laramie, Wyoming), a company also specializing in small-scale Raman systems, introduced a "milestone" product called the ReporteR. This system is a Raman instrument that is packaged in two different colored housings. The red one is for law enforcement applications, and a yellow version is intended for more general materials characterization and identification, such as for plastics and polymers. The instrument is fully integrated into a 6 in. × 3 in. × 1.75 in. package weighing 11 oz, and is powered by a 4-h rechargeable battery. The law enforcement version provides different modes of measurement for the surface measurement of materials and for samples contained in vials (for liquids and solids). It operates in real-time to provide an identification of an unknown illicit substance based on an internally stored library.

Princeton Instruments (Trenton, New Jersey) is a company whose name has been long associated with Raman spectroscopy. Over the years, they have provided optics systems and high-performance cameras for end users who like to build their own instruments. This year at Pittcon, the company introduced the TriVista CRS – Confocal Raman System. The system is designed to be flexible, providing for the use of tunable lasers, while providing good laser line rejection (down to 5 cm–1 from the laser line) and extremely high stray light rejection. The system enables the user to observe and record both the Stokes and the anti-Stokes spectral data at the same time.

ChemImage Corporation (Pittsburgh, Pennsylvania) has built up a reputation for spectral chemical imaging systems using different spectral imaging technologies. The company has introduced the FALCON II wide-field Raman Chemical imaging system. The system produces two-dimensional and three-dimensional molecular images, taking advantage of the company's proprietary Multi-Conjugate Filter, liquid crystal–based technology, and providing high-throughput hyperspectral screening of materials. The FALCON II incorporates an optimized CCD-based dispersive Raman spectrometer with low noise electronics. The system can provide a spectral resolving power of better than 0.5 cm–1. The combination of the optics (diffraction limited at 250 nm) and the CI Expert software enables the system to provide spatial resolution of chemical species below 1 μm.

Real-Time Analyzers (Middletown, Connecticut) is a small Connecticut-based Raman company formed a few years back by Stu Farquharson, who originated from Dow Chemical. Because of his background, the company has the name "real-time" as it pertains to the chemical process industry, and that is certainly one of the areas of focus for the company's products. However, from the start of Real-Time Analyzers, the company has become a significant supplier of substrates for surface-enhanced Raman spectroscopy (SERS). This technique significantly enhances the sensitivity of Raman for certain analytes and is well suited to the measurements of trace amounts of these compounds in an aqueous environment. The main reason for mentioning the company here is that it introduced a portable Raman analyzer that is well suited for field-based Raman measurements. Unlike most current small Raman systems, this portable instrument can operate with a 1064-nm Nd:YAG laser. The measurement principle is a little different than most Raman systems, and this provides the opportunity to produce nearly fluorescence-free Raman spectra, which is important for the next application. At Pittcon, the company demonstrated the use of the analyzer for identifying anthrax and related materials. The lack of fluorescence can help this application and others involving biologically related materials.

PerkinElmer (Shelton, Connecticut) has been strong in FT-IR and infrared spectroscopy since the company's original formation back in the mid-1950s. It has helped support Raman spectroscopy development over that period, but it could be considered an in and out company relative to Raman. In fairness, PerkinElmer was probably the first company to produce a Raman instrument, the LR-1, back in the late 1960s and early 1970s. It was also one of the first companies to produce an FT-Raman system (Nicolet was one of the others). PerkinElmer is now back in the Raman instrument business with its 400 model products — the RamanStation 400 and the RamanFlex 400 — and a Raman microscope, the RamanMicro 200. These are dispersive-based instruments based on an Echelle grating optical system. The RamanStation is a flexible benchtop instrument that offers a wide range of sampling options, including an automated xyz sampling platform for high-throughput well plate reading. The RamanFlex is a fiber-optic-based rack-style system for reaction monitoring and process-related applications.

In addition to its new Raman spectroscopy products, PerkinElmer introduced high-throughput sample introduction systems for its ELAN inductively coupled plasma mass spectrometry (ICP-MS) system and its Optima ICP instruments. The target applications for the systems are metals in drinking water (EPA methods 200.7 and 2008.) and other environmental applications. PerkinElmer also introduced the latest generation Optima series (7000 family products), ICP elemental analysis instrumentation for environmental, geochemical, product testing, and biofuels applications. In the area of elemental analysis, PerkinElmer has specialized in wear metals analysis for lubricating oils. It has produced the JANUS Oil Prep Workstation for increased automation in capital equipment maintenance.

Thermo Fisher Scientific (Waltham, Massachusetts) introduced new FT-IR and Raman products from what used to be its Nicolet stable. A theme of these products was simplification and ease of use. The iS10 FT-IR system is focused on QA/QC and investigative analytical work with simplified data analysis, sample handling, and instrument validation. The company describes the use of revolutionary deconvolution protocols to help simplify and automate the spectral interpretation process, including the identification of individual components of a mixture. On the sample handling side, for convenience, the iS10 enables a user to configure the instrument with two sampling techniques installed at a time. The iN10, an integrated FT-IR microscope, also was introduced. The product is equipped with a high-efficiency room-temperature detector, eliminating the need for and inconvenience of liquid nitrogen cooling. Sample location and measurement are automated by means of machine vision technology, and the OMNIC Picta software can extract comprehensive chemical and physical information, reducing the time required between taking the sample and presenting the answer.

Raman spectroscopy is described, in many contexts, as the complementary technique to infrared spectroscopy, and in support of that theme, Thermo Fisher Scientific has introduced complementary Raman products — the DXR Smart Raman spectrometer and the DXR Raman microscope. Unlike the infrared product, the DXR Raman is a dispersive instrument featuring a "triplet" spectrograph with a 2048-pixel CCD detector. It provides a full-range spectrum (50–3500 cm–1) with a 4-cm–1 spectral resolution, and a fingerprint-range spectrum (50–1800 cm–1) with a 2-cm–1 resolution. The Smart Raman spectrometer is intended to simplify Raman spectroscopy where the spectrometer recognizes accessories and components (lasers and gratings) and configures and optimizes the system automatically. The full benefits of Raman can be realized where the system accepts samples in a wide range of containers — from glass bottles, to blister packs, to well plates (for example). The DXR Raman microscope combines the benefits of the Smart system components with a novel microscope with spatial resolution down to 1 μm.

Horiba Jobin Yvon (Edison, New Jersey) has stayed true to form and continues to provide Raman products. Two key offerings from the company at this time are a new cost-effective Raman microscope, called the XploRA, and a continuation of the OEM component product line with a compact module that is small enough to fit in the palm of the hand. The XploRA is a compact and ruggedly designed Raman microscope that is intended for a wide range of applications, including clinical, pharmaceutical, forensic, biological, and mineralogical. It has a true confocal design featuring up to three lasers (blue to NIR) and four gratings, and it provides rapid Raman mapping and imaging. The system is designed as a microscope with the confocal Raman system added. The OEM component product line, which is intended for use in handheld Raman applications, operates with wavelength-stabilized mini-lasers (785 nm, 532 nm, or custom) and features a front-illuminated back-thinned CCD, with optional thermoelectric cooling for good Raman performance.

Although Horiba Jobin Yvon is well known to molecular spectroscopists for its Raman products, it is equally well known for high-performance spectrometer-based systems. The company introduced its FluoroMax-4 spectrofluorometer, which is capable of measuring picosecond fluorescence lifetimes. The instrument uses an ozone-free xenon arc lamp as its standard source, providing spectral coverage from the UV to the NIR (approximately 1000 nm). For lifetime measurements, there are plug-and-play LEDs and laser sources for maximum performance with the time-correlated single photon counting (TCSPC) applications. It is important to note that the company also offers a TCSPC microscopy system. The system, known as the DynaMyc, can produce maps from fluorescence lifetime and steady-state measurements. The company also presented the M Series II high-resolution research spectrometer, the 1000M Series II. This is a 1-m focal length spectrometer, with extremely low stray light, and it is ideally matched to Raman, low-temperature photoluminescence and ultrahigh resolution emission line measurements. Finally, ICP atomic emission systems were featured, from the ACTIVA family, including the ACTIVA-S, an affordable ICP emission system with a spectral range of 160–800 nm.

JASCO (Easton, Maryland) featured its new FT-IR microscope systems, the IRT-5000 and the IRT-7000, which readily interface to the existing FT-IR 4000 and 6000 spectrometer benches. A key innovative function featured on both of these products is "Smart Mapping," developed for microanalysis and IR imaging. The standard configuration of the 5000 includes a mid-band MCT, with the provision for a second detector. The 7000 provides for two detectors, the second being a 16-channel linear array (this array can be included as an option for the 5000). With the array option, both systems can be used for IR imaging. The smart mapping function enables mapping in a limited area without the need for an automated sample stage. This function also allows simultaneous viewing with an integrated CCD camera. Automated xyz sample mapping is available as an option. Both systems provide standard transmission, reflection, ATR, and grazing angle objectives for standard sample analysis.

Shimadzu Scientific Instruments (Columbia, Maryland) featured a new high-sensitivity FT-IR system known as the IRAffinity-1. The instrument has high-throughput optics with dynamic alignment. It is capable of providing a signal-to-noise ratio (S/N) of 30,000:1 and a maximum resolution of 0.5 cm–1. It features a ceramic source and a temperature-stabilized DLATGS detector. On the UV–vis side, the company introduced the UV-1800, with 1-nm spectral resolution and reduced straylight (approximately 50% improved), and improved S/N performance (over earlier models). Finally, Shimadzu also updated its line of AXIMA MALDI time-of-flight spectrometers. The AXIMA Performance provides high-energy interrogation for proteomics, biological, and organic samples. These include a range of high-mass species, such as intact proteins, as well as peptides, oligonucleotides, metabolites, and carbohydrates.

Hitachi High Technologies (Schaumburg, Illinois) introduced the U-3900 and U-3900H UV–vis spectrophotometers, which are designed for use in fields such as water quality, the environment, biotechnology, pharmaceuticals, and materials analysis. The spectrophotometers are constructed with a double-beam optical system and have separate lamps for the visible and UV wavelength ranges.

At last year's Pittcon, Bruker Optics (Billerica, Massachusetts) introduced the Alpha, the low-cost FT-IR system with the smallest footprint of any laboratory-based FT-IR instrument. A unique feature of the Alpha is its QuickSnap interchangeable accessory–sampling modules. This year, the company introduced three new sampling modules: a heated diamond attenuated total reflectance (ATR) for liquid analysis, a diffuse reflectance for powders and gemstone analysis, and a specular reflectance for surface analysis. Bruker Optics also introduced the MultiRAM, a standalone FT-Raman spectrometer. The MultiRAM is a fully automated FT-Raman instrument covering a range of applications from demanding research in academia, industry, and government laboratories to routine nondestructive analysis of both organic and inorganic materials. The dual-channel instrument is equipped with a 1064-nm Nd:YAG laser and accommodates a broad range of pre-aligned sampling accessories, including video stages, high–low temperature cells, fiber-optic probes, and a well plate accessory for high-throughput sampling.

The Daltonics NBC division of Bruker introduced the M-IR, a new rugged, fully self-contained mobile (Suitcase style) FT-IR analysis system. The system is fully integrated with a single-reflection ATR for easy sampling and cleaning, and it has the provision for an alternative flow-through cell. It is designed to operate between -5 °C and 40 °C. The system includes an embedded PC with a touch-screen user interface, and options for Ethernet, wireless, and USB external connectivity. It is powered via either a 4-h internal (rechargeable) battery or a 12-V power source, such as a vehicle "lighter-style" power connector. It is a fully functional FT-IR, providing normal functionality with the Bruker OPUS/Mentor software. The Daltonics division also introduced the HAWK FR (first responder) a rugged, tripod-mounted FT-IR intended for the homeland security market for low-cost chemical agent monitoring. The HAWK is derived from the RAPID, a mil-spec version designed for U.S. military applications.

A2 Technologies (Danbury, Connecticut) and Smiths Detection (Danbury, Connecticut) both introduced handheld FT-IR systems for material identification via an ATR touch probe. The systems share a common external design, with the version from Smiths Detection, the HazMatID Ranger, being yellow and the A2 Technologies version, the Exoscan, being red. The FT-IR is fully self-contained in a lightweight (approximately 7 lb) pistol-grip style battery-powered (3-h continuous) unit, designed for single-handed operation. It is a fully functional FT-IR system operating between 4000 cm–1 and 650 cm–1 at 4-cm–1 resolution. The sample interface is reflectance based and features an interchangeable ATR–external reflectance head. A PDA-based control panel is used for the user interface with a wireless communications link to an external PC. The two models are differentiated by application. The Exoscan is used for materials characterization, and the Ranger is used for HazMat identification for military and first responder applications. Applications of the Exoscan include surface coatings and composite surface chemistry in the aerospace industry.

In addition to this new handheld product, Smiths Detection also featured the IlluminatIR, its FT-IR accessory for optical microscopy; the IdentifyIR, a miniaturized FT-IR system designed for organic synthesis applications; and the Ionscan-LS ion mobility spectrometer. Ion mobility spectrometry (IMS) traditionally is not known in the laboratory, and we are more familiar with it in a security environment; it is widely used at the nation's airports for screening luggage for explosives. It is an analogous technique to mass spectrometry, in which materials are ionized and are separated and characterized, as a function of the ion's mobility, in an electric field. It works at atmospheric pressures (not a vacuum, as in mass spectrometry); it can be highly selective for certain classes of compounds; and it offers picogram to nanogram sensitivities (even femtogram under certain circumstances). It is currently being considered for pharmaceutical applications, with cleaning validation being an important example of an application.

Aspectrics (Pleasanton, California) introduced the concept of encoded photometric (EP)-IR, an infrared measurement technique that falls between dispersive and FT-IR spectrometry, at Pittcon 2005. Since that introduction, the company has advanced its products to provide multicomponent process analyzers featured at this year's Pittcon; the models 5000 and 5500 (mid-IR) and the 2750 (NIR) products. These products are offered integrated with liquid or gas–vapor sampling accessories. Application-specific versions are also offered, precalibrated, such as the BioDiesel Quality Analyzer (BQA 1000).

Ahura Scientific (Wilmington, Massachusetts) has established itself in a unique market niche for highly rugged, handheld spectrometers originally intended for HazMat and toxic chemical identification. Up to now it is best known for its FirstDefender, intended for hazardous chemical identification, and the TruScan Raman system for material characterization and verification.

The latest product from Ahura, the TruDefender FT, is a fully integrated FT-IR instrument with ATR-based sample handling and software for both data acquisition and sample identification. It is designed primarily as a HazMat tool for in situ characterization of toxic and hazardous chemicals. The instrument is ruggedly designed, yet it weighs less than 3 lb, including the rechargeable lithium ion battery. No details were provided at the time of the show in terms of spectral performance characteristics, but it was reported that useable spectra could be obtained for identification purposes in a few seconds. This is very much an applications-driven product for public safety, and an onboard hazard database provides medical response data for those exposed to specific corrosive or toxic materials identified by the instrument.

For many years, we have lived with the infrared spectrum ending at the far infrared. For many, that was around 200 cm–1, with both scanning dispersive instruments and FT-IR spectrometers equipped with cesium iodide optics. FT-IR instruments equipped with nontraditional beamsplitters, including silicon optics and Mylar pelicules, have been used to probe lower in the spectrum, and instruments that can be equipped for this range are still offered by companies such as Bruker, Thermo Fisher Scientific, and Bomem. Today, we have another class of instrument that probes the lower reaches of the vibrational (and rotation) spectrum, which is the terahertz spectrometers that cover the range from close to 0 cm–1 to 100 cm–1 (as low as 0.02 THz to 3 THz). Two companies visited at Pittcon with product offerings in this range were TeraView (Cambridge, United Kingdom) and Picometrix (Ann Arbor, Michigan). TeraView introduced the Spectra 3000, a spectrometer designed to accept standard ATR and transmission spectrometer accessories. The instrument also offers transmission imaging and standoff explosion detection accessories. The T-Ray 4000 is a time-domain terahertz (TD-THz) system, introduced by Picometrix, which operates in both transmission and reflection modes, with fiber-optic coupled sensor heads for high-speed imaging. It is intended for gas, liquid, and solid spectroscopy, and is ideal for nondestructive materials testing and inspection.

Two unique products were offered by BioTools (Jupiter, Florida), the ChiralIR and the BioRaman; the latter being a fast collection Raman spectrometer. The ChiralIR features an integrated FT-IR spectrometer (based on a Bomem bench) configured for vibrational circular dichroism (VCD). VCD in this configuration is defined as the difference, in absorbance, between left and right circularly polarized IR radiation. It combines the structural specificity of FT-IR spectroscopy with the stereo sensitivity of circular dichroism. It can be used for the separation of enantiomeric pairs of chiral molecules. It is an important tool for structural studies of biomolecules and physiologically important molecules. This product complements the ChiralRaman system that was awarded the 2004 R&D 100 award. The BioRaman offers 90% collection efficiency, producing very high quality Raman spectra with short collection times. It is ideally suited for biological systems in water.

ChemSight is a relatively new product designed to measure and identify minute quantities of hazardous gases and vapors with wide area coverage. The system is designed for continuous open path measurements with a line of sight of up to 100 m. A wide range of toxic materials are handled, with sensitivities ranging from 2 ppm/m to 200 ppm/m with identification in 1–30 s. It is designed for external operation over a range of -40 °C to +60 °C. The Site Protector software provides threat evaluation, gas identification, concentration, and time stamp.

Two state-of-the-art instruments were presented by SPECTRO (Mahway, New Jersey); the new ARCOS (Advanced Roland Circle Optical System) ICP optical emission spectrometer, and the SPECTRO iQ II X-ray fluorescence analyzer. The optics of the ARCOS utilize 32 linear CCD array detectors for the simultaneous recording of wavelengths between 130 nm and 770 nm. This, combined with a 750-mm focal length, makes the system ideal for ultratrace analysis for environmental applications, for line-rich spectra in metals analysis, and for organic materials in petrochemistry. The iQ uses polarized X-ray excitation and is developed for multielement analysis of solids, powders, and liquid samples. Typically, it is used for industrial process applications.

Agilent Technologies (Santa Clara, California), like many of the other larger instrument companies, is orienting itself toward markets and applications. The Materials Science Solution Unit (MSSU) has been added to the company. Its mission is to primarily offer nano-measurement solutions and support to accelerate discovery, manufacture, and commercialization of high value materials. The applications covered are high-tech research, pharmaceuticals, specialty chemicals, food safety, biotechnology, and semiconductors. The technology platforms include UV–vis spectroscopy, scanning probe (atomic force) microscopy, particle analysis, and high precision interferometry and optics. In addition to MSSU, Agilent continues to develop a strong product offering in mass spectrometry, including new Accurate-Mass time of flight (TOF) and Accurate Mass Quadrupole Q-TOF products. The 6220 (Accurate Mass TOF) liquid chromatography (LC)–MS system offers better than 2-ppm mass accuracy combined with 20,000 mass resolution and high-speed (32 GBit/s) data acquisition.

Although not thought of traditionally as infrared, we are starting to see products on the market based on cavity ring down spectroscopy (CRDS) and related technologies. These laser-based systems utilize the inherent high-resolution capability of the laser to provide unique analyses for industrial and environmental applications. Although intrinsically high resolution, they have low drift and excellent sensitivity, and are essentially calibration free, making them ideal for process analytical applications. Two new products from Picarro are based on this technology — the G1101-i isotopic CO2 analyzer and the G1102-i isotopic H2O analyzer. The CO2 analyzer is well suited for detecting greenhouse gas emissions.

While on the topic of the environment, albeit briefly, mercury analysis and mercury emissions remain high-profile applications. Milestone, Inc. (Shelton, Connecticut) has introduced an atomic measurement system for mercury analysis. The instrument, the Milestone DMA-80, does not require sample preparation, it features a 40-position autosampler for unattended operation, and it completes an analysis in five minutes.

One of my own pet areas of interest is small and micro-sized spectrometers. I have covered some that have been targeted toward specific applications. In this final part of the instrument section, I would like to focus on some companies and products that are continuing to bring new and innovative instruments and instrumentation platforms. Often, these small spectrometers can be and are integrated into custom-designed instruments for target applications. Other times, these products serve as a convenient (size-wise) or inexpensive way to do spectroscopy.

Probably the first and best known company in the area of small spectrometers is Ocean Optics (OOI), and they have introduced new products at Pittcon. The first is the Maya2000 Pro, a high-sensitivity back-thinned 2D FFT-CCD spectrometer for low light level and for UV-sensitive applications. The spectrometer provides better than 90% quantum efficiency with a wide dynamic range, and excellent UV response. It is interfaced with fiber optics, via SMA connectors, with light sources and sampling accessories. Another notable product introduced by OOI was Jaz, a family of stackable, modular components that come together to form a customized spectrometer system. The modules share common electronics and communications (including Ethernet connectivity for Internet addressability – via IP addresses), and can be powered via a rechargeable battery. The system does not require a PC for operations and has its own user interface, reminiscent of a gaming system controller, with an integrated display and data storage (via SD card).

Another strong player in the small instrument market is Avantes (Broomfield, Colorado). The Avantes products cover a wide spectral range, and new products were offered covering UV and NIR spectral ranges. In the case of the NIR, the company introduced the AvaSpec-256-2.5 fiber-optic spectrometer. This is a low-cost, fiber-optic–based spectrometer designed to cover the spectral range of 1100–2500 nm. Also introduced by Avantes was the AvaSpec-2048x14, a high sensitivity spectrometer, designed for OEM applications and ease of integration. The spectrometer can be powered via USB, external power, or battery. It features a high-sensitivity back-thinned CCD for good UV and NIR (short-wave NIR) performance.

Back in 2005, I was looking for a small NIR spectrometer system for integration into a handheld analyzer project. I used Pittcon 2005 as a means to survey new instrumentation, and in particular, what was new in small spectrometers. That timeframe was ripe because many technology products were being introduced at that time based on optical technologies that were originally developed from the telecom industry. At that show, there were at least four new companies or product lines that resulted from these developments, and a company called Valley Instruments was an example that caught my eye. They had novel (in terms of packaging) NIR instruments based on InGaAs technology that were cost effective. I started to look for the company a couple of months later and they had disappeared. I am happy to say that they have now reemerged as BaySpec, Inc. (Fremont, California). The company has a range of new spectrometer products, including the SuperGamut NIR spectrometer. This product was developed for the telecom industry, and so its design benefits from the requirements of that industry, including hermetic sealing and the ability to operate in almost any environment over a broad temperature range (-10 °C to 60 °C). The spectrometer offers a spectral range of 800–2500 nm, and with low power consumption, it is designed for battery operation.

Components, Enabling Technologies, and Accessories

One of the fascinating aspects of Pittcon is the broad spectrum of accessories and enabling technologies. Accessories range from modern sample handling accessories, including microscopes and spectral imaging systems, to highly capable, applications-specific software. Enabling technologies include special light sources, specialized detectors, and micro spectral measuring components. The latter includes some of the latest generations of miniature spectrometers. While companies have been producing these for a while, newer systems are becoming available that offer broader spectral ranges, different modes of interfacing (optical fibers being the most common), and smaller, lower-cost packages.

I have tried to be as complete as possible in terms of what is included in this section. My background is optical spectroscopy, and so I have tended to gravitate toward my comfort zone. I have received a broad range of materials from different companies covering a diverse range of technologies and applications. I will do my best to represent them here.

Companies that make traditional optical–spectral accessories–components such as Harrick (Pleasantville, New York), Pike (Madison, WIsconsin), Specac (Cranston, Rhode Island), International Crystal Laboratories (Garfield, New Jersey), and Axiom Analytical (Tustin, California) are still making and distributing a wide range of accessories for the laboratory, the plant, and specialized applications. Axiom almost exclusively focuses on process analytical accessories. Axiom Analytical presented FNL-120Ne (UV-Vis) and the RFP-400Ne (Raman) NeSSI platform-compatible products. NeSSI ("New Sampling System Initiative") is an industry-defined modular system of sampling accessory components based on a uniquely defined substrate conforming to the ISAS SP76 standard. Both components are interfaced via fiber-optic coupling. The company also introduced the RFP-460, a multipass Raman sampling probe. The RFP-400 is a multipass fiber optics sampling probe capable of providing up to 10× enhancement of the Raman signal. The company, under its Symbion brand, also introduced version 2.0 of its Symbion-LX instrument software.

Today, accessories are designed for ease of use and problem solving. An original technique used in infrared spectroscopy that was more of an art than a science was the making of compressed halide (KBr) pellets. A new KBr press from Pike, called the CrushIR, is intended to help automate and simplify what was once a very hit-or-miss process. It provides excellent reproducibility of pellet preparation, aided by the digital pressure reading and adjustable maximum pressure setting. The GladiATR is a new high-energy throughput diamond ATR accessory, also from Pike. The diamond forms a monolithic structure that is scratch and fracture resistant, and the sampling surface accepts hard objects, such as coated wires, rigid polymer pellets, and geological samples, without damage. In addition to the accessory optical design, there is a built-in imaging system for optimized sample positioning, with the output available on a large liquid crystal display.

Harrick has a tradition of reflectance-based accessories, and has expanded its product line to include fiber-optic interfacing to diffuse and specular reflectance with the Omni-Diff (diffuse reflectance) and the Omni-Spec specular reflectance. Both accessories are coupled via 1.5-m fibers to the FiberMate 2 interface. Based on the appropriate selection of fiber, the accessories can handle any wavelength region from the UV to the mid-IR. Harrick has also introduced a grazing angle ATR (VariGATR) for high sensitivity measurements on monolayers on silicon and metal substrates. The accessory accommodates samples up to 200 mm in diameter and has a built-in pressure application for ensuring optimal sample contact.

A new company, Middleton Research (Middleton, Wisconsin), formed by two "veterans" of spectroscopy engineering, Scott Little and Gabor Kemeny, is providing standards (NIST traceable) for spectral measurements, and some new and novel accessories, such as the IsolatIR. The IsolatIR is a "spectroscopy" glovebox that provides an inert or conditioned environment for samples while they are being measured. A standard accessory is placed into the glovebox, and this in turn is interfaced to the sample compartment of most FT-IR instruments. Middleton also provides hyperspectral chemical imaging integration and applications, and is the US-based distributor for SPECIM, Spectral Imaging, Ltd. (Oulu, Finland).

Earlier, it was mentioned that Harrick now offers accessories that are interfaced via optical fibers. NIR and Raman systems have long been interfaced via fiber optics, and for some, mid-infrared has been out of reach for fibers. In reality, this has not been the case, and Remspec has long been a pioneer in mid-IR optical fiber interfaces and has focused on reaction monitoring systems for both FT-IR and Raman. This year at Pittcon, Remspec featured new software packages, VizIR and VizRaman, and ReactionSleuth for its reaction monitoring systems. VizIR and VizRaman are data collection packages used to run the company's ReactionView (FT-IR) and Verax (Raman) systems, respectively. Another company, High Tech Photonics, offers a range of IR fiber-optic probes for transmission–reflection measurements, and a choice of mid-IR transmitting optical fibers. Two types of fiber are chalcogenide (As-S glass), designated CIR-fibers, and silver halide (AgCl:AgBr solid solution crystals), which are designated PIR-fibers. The fibers are differentiated in terms of their degrees of light attenuation and their spectral ranges.

Raman usually is not viewed as a technique suitable for trace analysis. For a long time, simply measuring the spectrum of a single sample or substrate proved to be a challenge. One technique mentioned earlier for enhancing the sensitivity of Raman spectroscopy is a sampling technique called SERS. A UK company called D3 Technologies presented a range of SERS solutions based on its proprietary substrate, Klarite. The material is supplied as a disposable solid phase substrate in the form of a chip or mounted on a microscope slide. It is claimed that for certain compounds, the Raman signal can be boosted up to 1 million times. Application examples include dilute solutions (dosage levels) of pharmaceutical products, proteins, and biological materials. When combined with suitable sampling, it can be used for explosives detection and homeland security applications.

A new optical technology for biochemical detection and for other liquid-based measurements, known as SpectroSens, was introduced by Stratophase, a spin-off company from the University of Southampton, England. SpectroSens is an optical chip that can measure variations in refractive index to better than 1 ppm. It can directly measure chemical substances via multiple refractive index measurements. One example is the measurement of biological materials dissolved in water by interaction with antibodies attached to the sensor surface.

A novel light engine technology primarily designed for life science and bioanalytical instrument applications was introduced by Lumencor. The source is designed as a single unit, offering high-power, narrow bandwidth light–radiation over the UV–vis–IR spectral region. The system offered provides the following wavelength ranges: 380–400 nm (violet), 430–450 nm (blue), 470–490 nm (cyan), 530–560 nm (green), and 630–650 nm (red), with power ranging from 50 to 150 mW (depending on wavelength selected). The first products offered are intended for fluorescence microscopy.

A polarization toolbox has been introduced by Olis, Inc. (Bogart, Georgia) as a stand-alone module or as an accessory to its other products. Olis currently offers a fluorimeter, a circular dichroism instrument, and a spectrophotometer. The accessory includes two polarizers, a modulator (photoelastic modulator), and a photon-counting module. The stand-alone module has the same components, but also includes a sample chamber and computer control software–hardware. The stand-alone version also requires the selection of a suitable source, typically an LED, a xenon arc lamp, or a laser.

For the past two years, the analysis of biofuels, and especially biodiesel, has been a focus for a number of companies, and analyses ranging from FT-IR, to gas chromatography (GC), ICP emission, and titrimetry have been featured with products offered by a wide range of companies. With analysis methods comes the requirement for measurement standards, and VHG Labs has introduced a range of standards, primarily for metals and sulfur analyses based on ±00 (100% fatty acid methyl ester based biodiesel).

Finale

There were many diverse new products and technologies to cover this year at Pittcon. I am certain that I did not cover everything, and my apologies about the products I might have missed. The show was personally very gratifying because of the new boost in Raman products and the increase in the use of smaller and lower-cost instrumentation. I hope that Raman is now back to stay. Some people might say that never went away, and that is true. But now we can really say that Raman is a mainstream technique and is offered in a broad spectrum (no pun intended) for instrumentation designs and formats. I am anticipating that the trend of smaller instrumentation will continue, and I hope to see that trend continue at Pittcon 2009.

John Coates is principal consultant for Coates Consulting in Newtown, Connecticut.

References

(1) J.P. Coates, Spectroscopy 3(4), 14–19 (1988).

(2) J.P. Coates, Spectroscopy 3(5), 14 (1988).

(3) J.P. Coates, "Laser Raman Spectroscopy in the Oil Industry," chapter in Recent Analytical Developments in the Petroleum Industry, D.R. Hodges, Ed. (Applied Science Publishers, Essex, England, 1974), pp. 13-44.

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