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Analytical Chemistry

Better Than Ever At Pittcon 2006

Attendance may be slipping, but enthusiasm for new and innovative analytical instrumentation has not waned

by Stu Borman
April 3, 2006 | A version of this story appeared in Volume 84, Issue 14

Pittcon, the Pittsburgh Conference on Analytical Chemistry & Applied Spectroscopy, was first held in Pittsburgh in 1950. This year, Pittcon held its 57th meeting in Orlando, Fla., where it delivered on its annual promise to provide a wide range of edifying presentations on analytical chemistry and to introduce a plethora of the latest analytical instruments for research and industry. The 2006 meeting saw the use of innovative technologies to develop instruments that, at least in some cases, are smaller and cheaper, offer higher performance, and are overall just better than ever before.

Not to be completely outshone by the novelty of some of the instruments at this year's Pittcon exposition, conference organizers introduced several "firsts" of their own. For the first time this year, Pittcon's technical program began on Sunday afternoon "to reduce overlap with concurrent sessions and with the expo later in the week," said Pittcon 2006 President Kevin J. McKaveney at an opening day press conference. This was the first year the conference provided free wireless Internet access in the convention hall on show days to make it easier for exhibitors and conferees to stay in touch with their work and families. And for the first time this year, Pittcon also permitted exhibitors to serve alcoholic beverages in their booths "to encourage more interaction," McKaveney said.

Starting the technical sessions on Sunday instead of Monday "worked out very well for us," McKaveney said. "Having a full Sunday program, we saw wonderful attendance for our Pittcon Heritage Award presentation, for plenary speaker Roger Y. Tsien, and our poster mixer afterward, which had the best attendance we've had in years, if not ever."

The Pittcon Heritage Award, honoring instrumentation entrepreneurship, is cosponsored by the conference and the Chemical Heritage Foundation. This year's honoree was Masao Horiba, who in 1945 founded Horiba Radio Laboratory while he was still a graduate student at Kyoto Imperial University. Now Horiba Ltd., the company markets analytical and diagnostic equipment and had sales of more than $800 million in 2004. Plenary speaker Tsien, a Howard Hughes Medical Institute investigator and professor of pharmacology and of chemistry and biochemistry at the University of California, San Diego, spoke on the design of molecules capable of reporting or mediating signal transduction inside living cells.

Pittcon 2006 featured more than 2,300 technical presentations, including 60 invited symposia, 114 contributed sessions, 54 poster sessions, nine workshops, and eight new product forum sessions. "This year, we have a higher concentration in the area of life sciences and pharmaceutical sciences, and we're also covering specialized areas of interest like bioterrorism, nanotechnology, and environmental analysis," said McKaveney, who is an executive sales representative for Waters, in Milford, Mass., when he isn't orchestrating one of the world's largest scientific conferences.

In the educational area, the conference featured more than 100 different short courses and sponsored its annual Science Week program, which includes educational programs and workshops for local science teachers, lectures and demonstrations for students, and grants to support elementary through college science education.

The Volusia County School District, in Florida, received this year's Pittcon Science Education Award, a $24,000 grant for equipment for teaching environmental studies. The annual award is made for the best science education proposal by an institution in the Pittcon host-city area. Pittcon, in conjunction with the Peabody Orlando Hotel, also presented a $25,000 grant to the Orlando Science Center to help fund the purchase of a portable digital video globe to extend its educational outreach program.

Registration for last year's Pittcon was about 20,900, and "we were hoping for a 10% increase in attendance this year," McKaveney said. Instead, there was a falloff, with tentative registration figures showing a total of about 19,900, a 5% drop in conferees and exhibitors.

"There was only a 2% drop in conferees from last year," McKaveney told C&EN. "I find that very positive. We had an approximately 8% drop in exhibitor registrations, and I believe that is due to exhibitors sending fewer representatives to cut costs and improve their return on investment."

Attendance at all conferences has been adversely affected by the events of Sept. 11, 2001; increased competition from other shows; and restricted travel budgets, McKaveney said. In addition, there has been "a drop in international attendees because of greater difficulty in obtaining visas." For example, the number of registrants from China was about 300 behind last year's.

"We hit our peak attendance in 1996, with about 35,000 attendees and exhibitors," he said. "Certainly, we feel we have a lot to offer here, and we want to work to build the attendance back up. Whether we get to those high levels of 35,000 again is hard to say, but I believe we can do better on attendance."

Each year at Pittcon, Centcom, the American Chemical Society's advertising management division, sponsors a breakfast for analytical instrument industry leaders, and this year was no exception. At the 2006 breakfast, Paul R. Knight, a partner at Thomas Weisel Partners, a New York City-based investment bank, told attendees that the life sciences sector was the major growth area for instrument sales from 2000 through 2003, but today sales are instead growing fastest in the industrial sector: the chemical, energy, environmental, and food industries. The largest market driver of all has been growth in sales to India and China (see page 61). "Asia was 11% of instrument market demand in 2000, and by 2007 it will represent 20-25% of total demand," Knight said.

A second speaker at the breakfast, Mike McMullen, vice president and general manager of chemical analysis solutions at Agilent Technologies, said that instrument industry customers need better analytical solutions to their problems; that is, they need the ability to carry out faster analyses at lower costs and yet obtain higher quality information. "Our responsibility as instrument vendors is to understand our customers' workflows and to develop automation and innovation that help better solve their problems," he said.

Indeed, instrument companies demonstrated some new ways to solve customers' problems at this year's massive Pittcon exposition. Each year, C&EN asks academic researchers to evaluate and comment on Pittcon new product introductions in several disciplinary areas. Our adviser in atomic spectroscopy this year is chemistry professor Gary M. Hieftje, head of the Laboratory of Spectrochemistry at Indiana University, Bloomington. Hieftje believes most Pittcon atomic spectroscopy offerings this year "were evolutionary rather than revolutionary" but points to several notable developments.

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Credit: Photo By Stu Borman
Credit: Photo By Stu Borman

One such development is Thermo Electron's new iCAP 6000 series of inductively coupled plasma (ICP) emission spectrometers. These are benchtop instruments with "an unusually small footprint, claimed to be the smallest in the industry," Hieftje said. Dan Shine, Thermo's vice president for elemental analysis, said the iCAP instruments have an innovative design that delivers "enhanced productivity and reduced cost of ownership for their users."

Also introduced this year was an extension to Thermo's S-Series and M-Series atomic absorption spectrometers-the addition of an intelligent spectrometer qualification (iSQ) unit that automatically tests and confirms instrument performance prior to an analytical run. "The iSQ module appears to be nicely designed and should be of benefit to high-volume laboratories that need to minimize operator time for instrument calibration and optimization," Hieftje said.

Shimadzu Scientific Instruments' new ICPE-9000 ICP emission spectrometer is equipped with a 1-inch charge-coupled device (CCD) detector, an Echelle spectrometer, and a minitorch that reduces argon gas consumption by half compared with conventional torches, the company says. "I like the minitorch," Hieftje said. "But then I would, since my group introduced it many years ago. It offers performance equal to that of a larger torch but at lower radio frequency power levels and reduced argon flow rates."

Varian introduced 810-MS and 820-MS ICP-mass spectrometry (ICP-MS) instruments that feature a new collision reaction interface (CRI). "The CRI is indeed new and quite attractive," Hieftje said. Unlike the separate collision or reaction cells located just prior to the MS analyzer in conventional ICP-MS instruments, "the CRI adds collision or reaction gases directly to the extracted plasma stream in the sampler and skimmer cones leading to the mass spectrometer," he said. Collisions that occur in those zones accomplish the same thing as in conventional cells-reducing and removing interfering species that would otherwise be extracted into the MS unit's ion optics. But the CRI design enables labs "to easily achieve lower detection limits and more accurate quantitation for difficult elements in complex samples," Varian says.

New Wave Research introduced the LIBS-Elite, one of the first commercial instruments for lab use of laser-induced breakdown spectroscopy (LIBS). The LIBS-Elite includes laser ablation technology to facilitate elemental analysis of a variety of materials. In addition, it utilizes an open sample cell at atmospheric pressure, "which simplifies sample handling," Hieftje said.

And Cetac Technologies introduced the Aridus II nebulizer system, "useful for both ICP atomic emission spectrometry and ICP-MS," he said. "The system is claimed to offer better sensitivities and lower oxide levels in ICP-MS. If present, oxides often overlap spectrally with the masses at which analyte species lie."

In the chromatography area, "it didn't seem to be a big year for new separations introductions at Pittcon" either, said chemistry professor James W. Jorgenson of the University of North Carolina, Chapel Hill, a specialist in capillary electrophoresis and capillary liquid chromatography. Several introductions were "largely incremental improvements of already introduced technologies. This year showed solid progress in the quality and variety of separations tools being offered, but with no new developments that took your breath away."

Jorgenson notes that more manufacturers were selling high-performance liquid chromatography (HPLC) columns with sub-2-µm particle packing material for high-efficiency separations this year. In addition, Waters introduced the Acquity SQD, a mass spectrometer-interfaced version of its high-efficiency UPLC (ultra-performance liquid chromatography) system. And in January, Agilent released its new 1200 Series LC system, which uses improved column and system design to achieve performance advantages: faster analysis time and up to 60% higher resolution than conventional HPLC.

Although no major announcements appeared for lab-on-a-chip instruments this year, evolutionary advances continue to be made in those fields as well, "especially in the overall direction of miniaturization," said Z. Hugh Fan, a specialist in microfluidics and an associate professor of mechanical and aerospace engineering at the University of Florida, Gainesville. Recent miniaturization successes include Agilent's HPLC chip, a microfluidic device that boosts sensitivity and reduces sample size requirements in nanoflow LC-MS of small-molecule and proteomics samples; and Ionchip, a chip-based quadrupole mass spectrometer from Microsaic Systems fabricated using microelectromechanical systems (MEMS) technology.

Things were a bit more lively in the area of molecular spectroscopy this year. Innovations included Aspectrics' Encoded Photometric IR (EP-IR) technology and the launch by Polychromix of Phazir, a portable, handheld near-IR device that's the latest addition to the company's near-IR digital transform spectrometer (DTS) family.

"These two companies have brought out different but very interesting new technologies for encoding IR spectra, which allows simultaneous observation of the entire IR spectral region with a single detector, a task that normally requires either an interferometer or an array detector," said professor of chemistry and of geosciences M. Bonner Denton of the University of Arizona, Tucson. "That means you can sell these instruments for a whole lot less money than those with conventional IR array detectors or interferometers," Denton said. His research interests include analytical spectroscopy, optical imaging, and lab automation, and whose group is currently developing a pocket-sized Raman spectrometer for a future Mars Rover mission.

In Aspectrics' EP-IR system, both a grating and a rotating encoder wheel are used to encode an IR signal from a sample, and Fourier transform is then used to convert that into wavelength versus intensity data. This technology makes it possible to carry out IR-based analysis less expensively.

The use of MEMS spatial light-modulation devices to disperse IR radiation in Polychromix's new handheld Phazir and in the firm's other DTS instruments makes possible "a compact and versatile chemical analysis system at an unprecedented low cost," the company claims. Polychromix currently markets DTS systems for general purpose spectroscopy applications, but it anticipates potential process control uses, ranging from flue gas monitoring to trans-fat measurements in food analysis.

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"If one talks about handheld systems, you also want to mention Ahura, which showed a handheld Raman spectrometer that looks to be very powerful," Denton said. "This handheld unit demonstrates high performance levels equivalent to a standard major research instrument." Ahura's handheld instrument, called FirstDefender, is designed to identify unknown liquids and solids under field conditions. According to the company, the system "is built to the rigorous requirements of the military and optimized to the needs of civilian first responders. It is entirely self-contained, rugged, lightweight, and easy to use."

The Swiss Army knife of imaging technology also came out this year. NT-MDT's new NTegra Spectra is a benchtop system that combines atomic force microscopy with conventional optical, fluorescence, laser-scanning confocal, and near-field scanning microscopies. It also includes an automated Raman and fluorescence spectrometer that complements the imaging information. Applications include corrosion and polymer investigations, drug delivery studies, carbon nanotube research, and imaging of single molecules.

"It's a really nice system-very impressive," Denton said. "It has tremendous flexibility and combines multiple capabilities in a single well-integrated package. It's all modular. You can swap components back and forth, so you can buy what you need and add onto it later. The company had it running and doing really nice things on the show floor."

Another technology that impressed him at the show was the NIR Analyzer XL, a near-IR spectrometer from Axsun Technologies. "Typical resolutions of affordable near-IR spectrometers are in the tens of wavenumbers, whereas Axsun's system has 0.1-wavenumber resolution," Denton said. "The company is taking techniques that would conventionally be used to make integrated circuits and using them to make optical components instead. I think this approach is going to revolutionize how optical spectrometers are built in the future."

Things were cooking in the MS area this year as well. One Pittcon 2006 highlight was Thermo Electron's LTQ Orbitrap mass spectrometer, "the first totally new mass analyzer to be introduced to the market in more than 20 years," according to the company.

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Credit: Photo by Zheng Ouyang
Credit: Photo by Zheng Ouyang

The Orbitrap design was patented in 1999 (U.S. patent 5,886,346) and was first described in detail in a scientific journal six years ago (Anal. Chem. 2000, 72, 1156). The Orbitrap "has ions spinning around a carefully shaped central electrode while shuttling back and forth over its long axis in harmonic motion at frequencies dependent only on their mass-to-charge ratios," explained professor of analytical chemistry R. Graham Cooks and associate research scientist Zheng Ouyang of Purdue University, who commented together by e-mail on MS new products. Cooks's group specializes in MS fundamental phenomena, instrumentation, and analytical applications, and Ouyang has been responsible for the construction of a number of new types of mass spectrometers.

Thermo's LTQ Orbitrap is a hybrid instrument in that it combines the Orbitrap analyzer with a linear ion-trap analyzer, the Finnigan LTQ. According to the company, this design enables faster and more sensitive detection of compounds in complex mixtures than with conventional mass spectrometers. The instrument's "outstanding mass accuracy, mass resolution, and [high sensitivity] make it a clear alternative to existing hybrid time-of-flight systems," Thermo says. Media representatives vote on what they believe to be the most significant new products at Pittcon each year, and the LTQ Orbitrap won the first-place Pittcon Editors' Gold Award this year.

Cooks and Ouyang pointed out that the LTQ Orbitrap's performance is comparable to that of a Fourier transform ion cyclotron resonance mass spectrometer and would be attractive to FT-ICR users because it's cheaper to maintain. "It would also be attractive to quadrupole time-of-flight users due to the relatively small additional cost to obtain higher resolution and better mass accuracy together with more stages of tandem MS," they noted.

Cooks and Ouyang also liked two new tools for ion dissociation in ion trap instruments-Thermo's Pulsed-Q Dissociation (PQD) and Agilent and Bruker's implementations of electron transfer dissociation (ETD) fragmentation.

PQD is a new fragmentation technique for protein analysis that eliminates the low-mass cut-off for ion traps. "Using Thermo's PQD method, fragments with mass/charge ratios below one-third those of precursor ions can be observed in ion trap mass spectra," whereas they cannot be efficiently observed with conventional ion trap instruments, Cooks and Ouyang said. "This capability resolves a perceived difficulty and in some cases a real disadvantage with ion traps." With PQD, "the intensity of fragments is increased, too, since more energetic excitation conditions are accessed, leading to better recognition of peptides."

ETD fragmentation is also designed for protein analysis. "The ETD experiment was first reported a year ago and has been introduced in commercial ion trap instruments by Agilent and Bruker," Cooks and Ouyang noted. "ETD provides a unique mode of fragmentation that generates highly characteristic fragments and eases the analysis of peptides and proteins bearing functionally important modifications, such as phosphorylation and glycosylation.

"The overall weight of mass spectrometers is one of their disadvantages, severely limiting in situ applications of this premier analytical method," Cooks and Ouyang said. "The past decade has seen increasing emphasis on small analytical instruments, including mass spectrometers."

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Credit: Photo by Stu Borman
Credit: Photo by Stu Borman

At least three portable MS systems emerged at this year's Pittcon. One of them was Microsaic Systems' Ionchip-based quadrupole mass analyzer, which Fan also mentioned as a miniaturization advance. Microsaic uses MEMS technology to construct its Ionchip, an integrated component that combines an ion source, mass analyzer, and detector. Ionchip technology is based on research conducted in the past decade or so by professor Richard Syms, head of an optical and semiconductor devices research group at Imperial College London.

Microsaic's Ionchip-based mass spectrometers can fingerprint compounds in solid, liquid, or gas samples. "Ionchip technology makes it possible for customers to buy a personal analyzer and use it just like any personal computer peripheral," said Alan Finlay, Microsaic's chief executive officer.

At Pittcon, the company launched two Ionchip-based instruments targeted at lab and security applications: the Ionchip ChemCube personal sample analyzer and the Ionchip ChemPack, a waterproof, rugged, battery-powered system designed for field use. The systems have electron impact ionization sources, near-unit mass resolution, and low parts-per-billion detection limits in favorable cases, Cooks and Ouyang noted.

Griffin Analytical Technologies presented the handheld GCAT 600 mass spectrometer, based on a cylindrical ion trap (CIT). The CIT incorporates much smaller vacuum systems and power electronics than those required in conventional MS systems. "The self-contained instrument has a direct air sampling interface and tandem MS capability and is intended for networked point-detection applications, such as perimeter security and depot monitoring," Cooks and Ouyang said.

And Purdue University's Discovery Park, a commercial incubator center, demonstrated the Mini 10, a handheld mass spectrometer with tandem MS capabilities that was developed and constructed in Cooks's group by a team led by Ouyang. The Mini 10 is about the size of a shoebox and weighs only about 10 kg. Its development was funded in part by the Department of Homeland Security, and it is accurate and fast enough to be used for airport security and homeland security as well as environmental and forensic applications.

Other significant Pittcon MS developments this year included the introduction of Thermo's DFS double-focusing sector mass spectrometer, "the first double-sector instrument that can be shipped in one piece and set up within one day," Cooks and Ouyang said, and Varian's new CRI interface for ICP-MS, which also was mentioned by Hieftje.

There were two other top Editors' Awards this year, in addition to the Gold Award to the LTQ Orbitrap. The Editors' Silver Award went to Chem+Mix, a system for automated solution preparation by Chata Biosystems. Chem+Mix facilitates the preparation of buffers or mixed organic solvents in volumes from 200 mL to 2 L. The system is compatible with virtually any analytical instrument that requires preblended reagent mixtures. The Editors' Bronze Award went to MassWorks from Cerno Bioscience, a data acquisition software package for MS. It uses a calibration algorithm to improve mass accuracy, enhance noise filtering, and improve quantitation.

At the opening-day Pittcon press conference, Beth L. Kirol, PPG Industries technical manager and Pittcon 2007 president-elect, noted that Pittcon organizers had earlier announced their decision to move Pittcon 2007 from New Orleans to Chicago. "The move was a very difficult decision," she said. "It was made after months of very careful consideration of all the factors involved and exhaustive debate. ... The conference remains committed to returning to New Orleans in 2008."

McKaveney added that Pittcon 2006 shaped up to be "a wonderful show, and I think that will carry over into Chicago next year. We're looking forward to being there."

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