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Analytical Chemistry

New And Notable At Pittcon

Scientific Instrumentation And More

by Stephen K. Ritter
March 24, 2008 | APPEARED IN VOLUME 86, ISSUE 12

Pittcon Editors' Award Winners

(1) Bruker AXS presented the Smart X2S (crystal-to-structure) compact X-ray crystallography system, which took home the Pittcon Editors' Gold Award. Originally launched in September, the Smart X2S is the first benchtop instrument for atomic-resolution crystal structure determination of small molecules. Its fully automated "walk-away" design was created for chemists who don't have specialized training in crystallography. Traditional X-ray systems for structure determinations are large instruments that require significant infrastructure. In the absence of a diffractometer or experience, chemists forgo structural confirmation at key stages of their research or send samples to an off-site crystallographer or to a service lab. The low-cost Smart X2S requires only a plug-in to a wall outlet yet should permit chemists to routinely obtain publication-quality structures in their own labs in a few hours. The instrument should appeal to academic teaching labs, research labs, and companies without a crystallographer on staff.

(2) Nlisis Chromatography debuted the Meltfit One, a novel device that reliably couples gas chromatography capillary columns together for specialized applications. It is this year's Pittcon Editors' Silver Award winner. Scientists typically use glass or metal fittings to connect a precolumn to a GC column or to connect two columns together for GC/GC and other methods. But establishing a seamless, stable connection that won't leak under high pressure is difficult to pull off with small-diameter columns and requires experience and patience. Nlisis (pronounced as "analysis") worked with GC users to design the Meltfit so that anyone can quickly make perfect connections every time without leaks or dead volume between the columns. The automated device consists of a portable case with a stage that has a recess for placing a small glass tube. The columns to be joined are inserted into the ends of the tube, the stage is heated to soften the tube, and air or inert gas pressure is applied so that the tube fits snugly around the column ends when it cools.

Bruker AXS showcased the S2 Picofox benchtop total-reflection X-ray fluorescence (TXRF) spectrometer for trace-element analysis, which received the Pittcon Editors' Bronze Award. The TXRF technique was previously limited to large systems used for semiconductor and coatings testing. The transportable S2 Picofox, designed for lab or field use, opens up TXRF to complement or replace atomic absorption spectroscopy and inductively coupled plasma mass spectrometry in clinical, nutritional, mining, and environmental applications. The instrument offers "zero-wait sample prep," allowing direct analysis of nanogram or larger amounts of almost any type of liquid, suspension, solid, filter, or particulate matter sample. It incorporates Bruker's XFlash silicon drift detector to measure elements ranging from aluminum to uranium at concentrations from 0.1 ppb to percent levels.

Molecular Spectroscopy

Picarro exhibited the G1102-i isotopic water vapor analyzer, a cavity ring-down spectrometer designed to use hydrogen and oxygen isotopes in water as fingerprints for industrial process monitoring and environmental field studies. Cavity ring-down spectroscopy (CRDS) is a high-resolution absorption technique based on detection of the slow decrease in intensity, or ring-down rate, of laser light bouncing between two mirrors in a gas sample cavity. Picarro has an existing line of CRDS analyzers for isotopic monitoring of carbon dioxide, ammonia, hydrogen sulfide, formaldehyde, and other compounds. The easy-to-use G1102-i opens up a potentially broad new market for CRDS, according to the company. For example, the instrument can pinpoint sources of moisture contamination in semiconductor processing and determine the point of origin of foods and pharmaceuticals. It can also replace costly lab-based infrared/mass spectrometry systems for energy exploration and atmospheric studies.

(3) PerkinElmer introduced the Lambda XLS (shown), a UV-Vis spectrometer for quality control and assurance, as well as for teaching laboratories. The company also introduced the Lambda Bio, a UV-Vis spectrometer for bioscience laboratories. Both instruments, which have compact designs and cover a spectral range of 190-1,100 nm, were designed as low-cost, routine platforms. They are amenable to customized methods, but the XLS and Bio come preconfigured with standard methods addressing a wide range of applications. The Bio, for example, is preconfigured for DNA, RNA, and oligonucleotide concentration and purity analysis, as well as for protein assays and cell density measurements. PerkinElmer also displayed its recently launched Lambda 1050 UV-Vis/near-IR system, which uses three detectors to cover a wide scanning range of 175-3,300 nm and is geared toward materials science applications.

Shimadzu exhibited the UV-1800, the company's latest UV-Vis spectrometer. The UV-1800 features 1-nm resolution over a spectral range of 190-1,100 nm and has the smallest footprint (45 × 49 cm) of any compact, stand-alone UV-Vis spectrometer, according to the company. Improvements include Shimadzu's low-stray-light diffraction grating, which restricts stray light to half that of the earlier UV-1700 model, and a brighter optical system that reduces the noise level (at 700 nm) to 25% that of the UV-1700 level. Equipped with several measurement modes-photometric, spectrum, kinetic, and biomethod-the UV-1800 is suited for a variety of projects, including DNA and protein analysis. The instrument can function on its own, or it can be controlled by a separate computer.

(4) Thermo Fisher Scientific launched a set of Raman and infrared spectroscopy platforms under a program called "Spectroscopy Simplified." These instruments are aimed at helping users in forensic and multipurpose quality-control labs move quickly from "sample to answer." The DXR SmartRaman spectrometer, which the company is promoting as the first Raman analyzer designed specifically for quality control, can be set up for single-button operation. It gives labs the ability to reproducibly characterize products directly through glass or plastic packaging to save time and avoid product contamination. Thermo also launched the DXR Raman microscope (shown), which is intended to help nonspecialist users achieve fast sampling and analysis of particles down to 1-μm spatial resolution. It's designed for analyzing trace forensic evidence, materials in defect or failure analysis, and more. On the IR side, Thermo introduced the Nicolet iS10 FTIR and an FTIR microscope, the Nicolet iN10. A key feature of the IR instruments is software that simplifies data interpretation.

(5) Ocean Optics displayed the Jaz modular UV-Vis spectroscopy suite, a family of small, stackable components that share common electronics and communications systems. The modules can operate together or separately, and they can be configured as needed for lab, field, or remote-sensing applications. Jaz features a light-source module available with deuterium or tungsten bulbs. The spectrometer module incorporates switchable gratings and slits that, together with a linear charge-coupled device detector, provide a spectral range of 200-1,100 nm. An easy-to-read OLED display module, which looks like a video game controller (shown), includes a microprocessor to drive the system. Contact with an external computer is still possible via a module containing an Ethernet connection and data-storage card. The entire system can be powered through this module or by a module containing a rechargeable battery.

PerkinElmer presented the Optima 7000 series of inductively coupled plasma-optical emission spectroscopy (ICP-OES) instruments, which update previous Optima models. The Optima 7000 family is designed for inorganic analysis in the environmental, geochemical, product testing, and biofuels markets. The instruments include a universal data acquisition mode that records spectral data over time, enabling users to go back and retrieve unused data without having to rerun a sample. Other features include the ability to generate time-specific quality-control charts and error flag generation when a sample result falls above or below a user-specified value. The Optima 7000 series is part of PerkinElmer's EcoAnalytix initiative, which focuses on challenges in food safety, water analysis, and biofuels development. For example, the EcoAnalytix Trace Metals Biodiesel Analyzer platform, based on the Optima 7000, is designed to test for group 1 and group 2 metals and phosphorus in biodiesel quality control.

Horiba Jobin Yvon showed the MF2 MultiFrequency Fluorometer, a speedy fluorescence spectrometer for studying solutions, powders, and thin films to provide information about the molecular behavior of cells, nanodevices, and other materials. Typical frequency-domain instruments that measure fluorescence dynamics excite the sample with a stepwise sequence of light frequencies and then monitor the fluorescence lifetime response to each frequency. The MF2 excites the sample with up to eight frequencies of light in the UV to near-IR range simultaneously, expanding the available frequency range. This approach allows the fluorescence data to be collected all at once so that experiments that used to take minutes can now be done in seconds. The ability to make these quick measurements should open up fluorescence spectroscopy to kinetics studies, including stopped-flow and fast-reaction experiments to resolve closely spaced dynamic events from one another, according to the company.

Chromatography & Separations

Waters displayed several new instrument configurations based on its Acquity Ultra-Performance Liquid Chromatography (UPLC) technology, which was first introduced at Pittcon in 2004. The Patrol UPLC Process Analyzer, the first process analytical technology (PAT) system to use UPLC, can draw a sample from a product line, fermentor, or reaction tank and complete an automated analysis in about three minutes. Before UPLC, LC wasn't fast enough for on-line analysis, relegating LC monitoring to off-line quality-control labs. The Patrol system is expected to improve pharmaceutical manufacturing efficiency in particular. Waters also introduced a UPLC/MS/MS system for food safety testing. This system combines Acquity UPLC technology with the Quattro Premier XE mass spectrometer as a tool for analyzing veterinary drug residues, pesticides, and other contaminants in foods. In addition, Waters displayed the MassTrak Amino Acid Analysis Solution, a system that combines Acquity UPLC with Waters' AccQTag derivatization chemistry for amino acid analysis of urine and blood samples.

Thar Instruments launched the Method Station II analytical-scale supercritical fluid chromatography (SFC) system. Like other Thar SFC instruments, Method Station II uses pressurized carbon dioxide solvent and methanol or other cosolvent as the mobile phase. The SFC technique typically has faster separation times and higher resolution than normal-phase HPLC and is useful for drug discovery and pharmaceutical process chemistry research. The key feature of the Method Station II is an Analytical-2-Prep column oven that is larger than its predecessor. The oven's unique drawer design is the first to allow multiple HPLC or SFC columns of different diameters to be loaded at the same time. This attribute permits users to test different parameters for drug separations without repeatedly stopping and starting the instrument to switch columns. The Method Station II is configured with a UV-Vis detector and operates at rates up to 10 mL per minute.

(6) Dionex unveiled the ASE 150 and ASE 350 (shown) accelerated solvent extraction (ASE) systems, the first new lab-scale ASE devices introduced in more than 10 years. ASE uses common organic solvents and a combination of elevated temperature and pressure to extract organic compounds from solid and semisolid materials. It's a useful method for lipid determinations in food samples, environmental pesticide measurements, and polymer and pharmaceutical process monitoring. The automated ASE 150 and ASE 350 are faster and save solvent relative to Soxhlet, sonication, supercritical fluid, and microwave extraction procedures, according to the company. The instruments include "pH-hardened" components that permit extraction of acid- and base-treated samples without damaging the plumbing. The ASE 350 model, designed for high-throughput labs, can handle up to 24 samples at once.

Agilent promoted several enhancements to its flagship 7890A gas chromatograph, introduced at Pittcon last year, and its 5975C GC/MS, which can work with the 7890A GC as the front end. The company introduced a GC/GC configuration that uses a differential flow modulator to focus and transfer effluent from the first GC column to the second GC column with better precision and without the need for cryogenic cooling (standard for GC/GC in the past). The new system should reduce cost and make GC/GC a routine analytical method, according to the company. Agilent also announced the acquisition of the Blos bead nitrogen-phosphorus detector technology. This detector is expected to increase productivity for environmental and forensic applications and should be available for Agilent instruments later this year. Agilent further introduced the Triple-Axis Detector for the 5975C. The detector has a unique geometry and electron multiplier design that lowers the detection limit of the 5975C by a factor of two and doubles the detector's expected lifetime.


Pittcon Potpourri

(7) CEM introduced the Sprint Rapid Protein Analyzer, an instrument designed to provide faster and more accurate total protein determination of food and animal feed. Traditional protein tests, such as Kjeldahl ammonia measurement or Dumas combustion, require harsh conditions and take hours to measure the total nitrogen content of a sample and correlate the value to protein content. But these methods can be unreliable if a sample contains or is adulterated with nonprotein nitrogen compounds, as demonstrated in last year's pet-food scare. The compact Sprint system prevents nonprotein interference by using CEM's iTAG protein-tagging technology, which the company says is the first effort to simplify and fully automate protein tagging for food-testing applications. The analyzer is CEM's first foray into non-microwave-based products. It uses a disposable kit so that the operator need only weigh a sample, put it in the instrument, push a button, and wait two minutes for the test result.

(8) JEOL enhanced its portfolio of imaging instruments with several new offerings at Pittcon. Leading the way was the NeoScope JCM-5000, a benchtop scanning electron microscope (SEM) codeveloped with Nikon Instruments. The compact, low-cost NeoScope is a versatile SEM that requires no sample preparation and is as easy to use as a digital camera, the companies say. Those attributes, along with high magnification (to 20,000??) without losing depth of field, are expected to make the NeoScope appealing to the bioscience and industrial inspection communities that often rely on optical microscopes. JEOL also displayed the JIB-4500 MultiBeam, a first-of-a-kind instrument that permits simultaneous SEM imaging with focused ion beam (FIB) deposition or ablation of materials; SEM uses an electron beam, whereas FIB uses a gallium ion beam. The MultiBeam is expected to be useful for structural biology and electronics studies.,

Shimadzu showed the MCE-202 MultiNA automated capillary electrophoresis system for high-speed analysis of DNA and RNA. The MCE instrument is faster, less costly per test, and more sensitive than alternative electrophoresis technologies, company representatives say. The user-friendly MultiNA employs reusable microchips and automates sample pretreatment, separation, detection, and data analysis all in a single device. When used under recommended conditions, the chips can process 3,600 or more analyses before being replaced. An LED-excited fluorescence detector increases sensitivity to more than 10 times that of ethidium bromide stain used in classical electrophoresis. And by processing with up to four microchips in parallel, the MCE-202 can deliver results in just 75 seconds when using the shortest analysis mode. MultiNA users can perform either automatic or manual data analysis and confirm completed results even while the unit is processing other samples.

Hitachi exhibited the LaChromUltra, a low-cost liquid chromatograph with the flexibility to run conventional HPLC or ultra-high-speed LC on a single system. LaChromUltra's specially designed "finger-tight" column connections withstand pressures up to 60 MPa yet make it easy to switch between conventional HPLC columns and ultra LC columns without tools. Ultra LC columns contain smaller particle size packing material (2 μm), permitting the LaChromUltra to provide faster analyses without increasing column temperature or significantly increasing column pressure. For example, LaChromUltra achieves a 90% reduction in analysis time relative to Hitachi's LaChrom Elite HPLC system while maintaining the desired high-resolution separations. LaChromUltra is available with UV, UV-Vis, diode array, or fluorescence detectors and has an autosampler for high-throughput sampling.

Mass Spectrometry

(9) Varian unveiled the 920-MS triple-quadrupole Fourier transform mass spectrometer (TQ-FTMS), a platform that provides the ultrahigh resolution and mass accuracy chemists need for advanced proteomics, metabolomics, and petrochemical and environmental analyses. The 920-MS couples the technology of Varian's 320-MS triple-quadrupole mass spectrometer with its FTICR (ion cyclotron resonance) detectors to give users more experimental choices and capabilities in a single instrument. The 920-MS breaks additional new ground by including both LC and GC interfaces to introduce samples for ionization; in the past, FTMS has primarily used LC sample introduction. The available magnet field strengths include 7, 9.4, 12, and 15 tesla-the latter being the highest field magnet commercially available for FTMS.

Thermo Fisher Scientific exhibited several new combinations of instruments and ionization sources in its mass spectrometry stable. In one example, the company introduced a MALDI (matrix-assisted laser desorption ionization) molecule fragmentation source for its LTQ XL linear ion-trap spectrometer. This combination provides researchers a new route to information-rich spectra for analysis of digested proteins, peptides, and posttranslational protein modifications. In another example, Thermo introduced MALDI and electron-transfer dissociation (ETD) ionization capabilities for its LTQ Orbitrap radial ion-trap spectrometer. The MALDI LTQ Orbitrap provides ever-higher resolution for proteomics and metabolomics studies. And the LTQ Orbitrap XL ETD, which provides MS/MS data, is now the most advanced overall proteomics platform available, according to the company. Thermo's ImageQuest software is available for each of the new configurations for mass spectrometric imaging, allowing users to detect and determine the distribution of compounds in biological samples or polymers without extensive sample preparation.

Bruker Daltonics introduced a new generation of its Qq-TOF (time-of-flight) mass spectrometer, called the micrOTOF-Q II. This instrument is designed for fast, high-resolution LC/MS/MS experiments in proteomics, metabolomics, and biomarker profiling applications. One of the new features is an updated SmartFormula 3D formula-determination method, which deciphers all the possible molecular formulas for a sample peak and reduces the possibilities down to just a single candidate. The program now combines the exact mass and isotopic profile of small-molecule sample peaks from both MS and MS/MS spectra, improving formula determination for compounds up to 1,000 daltons. Bruker also announced the related Complete Molecular Confidence solution, an automated method that verifies molecular formulas and structures for small molecules by combining formula information from SmartFormula 3D with predicted structures from 1-D and 2-D NMR data generated in Bruker's Avance III NMR system.

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