American Lab 0502

American Laboratory ®May 2012

Practical Resources for Laboratory Scientists

Micro Raman at Pittcon® 2012

Focus on Separation Science at Pittcon® 2012: Advances in Gas Chromatography

Pittcon® 2012: Laboratory Instrumentation and Equipment Product Showcase

New Developments in Supercritical Fluid Chromatography (SFC) at Pittcon® 2012: 20/20 Vision?

Pittcon® 2012 Roundup of Spectroscopy and Mass Spectrometry

Advances in Liquid Phase Separation at Pittcon® 2012

Benchtop Basics: Tips for Buying pH Meters and Balances

Mass Spectrometers for Use in Clinical Diagnostics

Volume 44, Number 5

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AMERICAN LABORATORY • 2 • MAY 2012

American Laboratory®

Volume 44, Number 5www.americanlaboratory.com


by J. Hunt………...........................................................…………................................pg 20The wide variety of lab equipment and instrumentation featured at Pittcon is showcased in this review.

Conference Review


by R.L. Stevenson……...............................................………….................................pg 12This comprehensive review of separation science products introduced at Pittcon 2012 includes a number of GC systems and columns.

Conference Review


by R.L. Stevenson………............................................…………................................pg 28Novel developments in stationary phases for SFC and SFC instrumentation are featured in this review of Pittcon 2012 products.

Conference Review

Conference Review

Contents Product Intelligence


by J. Perkel………........................................................…………................................pg 30

This review presents new product launches in spectroscopy and mass spectrometry.

Conference Review

What Is This?This month’s cover image was provided by Dr. Fred E. Hossler, Pro-fessor Emeritus, Dept. of Anatomy & Cell Biology, Quillen College of Medicine, East Tennessee State University, Johnson City, TN., U.S.A. The sample, provided by a local dermatology clinic, was captured using a Zeiss DSM 940 scanning electron microscope. Using routine SEM, the original magnification of this sample was 200×. The image has been artificially colored using Photoshop. What do you think it is? To comment, go to http://goo.gl/AEjrd. See the answer to the April cover on page 56.

Product Highlights…………...................……................................................……..pg 52

New Products


by R.L. Stevenson………............................................…………...............................pg 38

Instruments for liquid phase separation and an array of LC columns round out this review.

Benchtop Basics: Tips for Buying pH Meters and Balances

by C. Smith….….........………………………..................................................…………...…pg 51

Mass Spectrometers for Use in Clinical Diagnostics

by T. Keith Brock……………………………................................................………..….....pg 53

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an American Laboratory/Labcompare publicationAmerican Laboratory (ISSN 0044-7749) Volume 44, Number 5

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Editor’s Page Micro Raman at Pittcon® 2012by B. Foster..…..………………..............................................................................………pg 6

Industry News and Events…….........................................………......................pg 55

Advertising Index………………...............................................................….....…...pg 56

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Micro Raman was big news at Pittcon® 2012 . While the hardware has stabilized, there were intriguing new develop-

ments in the science and its applications .

Bridging the microscopy/ spectroscopy chasmHistorically, atomic force microscopy (AFM) has been the gateway for Raman microscopy, but the emphasis at Pittcon was on the optical . Major manufacturers—from micro Raman in-dustry leaders Renishaw (www .renishaw .com) and Horiba (www .horiba .com) to Bruker Optics (www .brukeroptics .com), Jasco (www . jascoinc .com), Kaiser Optical Systems (www .kosi .com), and Thermo Fisher Scientific (www . thermofisher .com)—all featured fully inte-grated systems, typically centered on Olym-pus BX research-level microscopes (www . olympusamerica .com) . (WITec [www .witec .de] and CRAIC Technologies [www .micro-spectra .com], which follow similar formats, elected not to exhibit at Pittcon this year .)

While similar in design, each company features something slightly different, mak-

ing comparison shopping with your own sample especially important . For example, Jasco offers proprietary vertical scanning (SPRintS), which keeps the beam perpen-dicular to the sample throughout the scan to remove any pin-cushioning aberration, and a special Dual Spatial Filter (DSF); this removes not only fluorescence, which can often mask the Raman signal, but back-ground Raman as well . Figure 1a shows a nanodiamond in the center of a groove in a polymer matrix . Figure 1b shows the typi-cal Raman spectrum, with both fluores-cence, which obscures the baseline, and a high background signal from the polymer matrix . The DSF (1c) effectively removes both, revealing a clean, distinct peak for the nanodiamond .

Renishaw joined the 3-D revolution with the new StreamLine HR™ . The new soft-ware makes 3-D images using Raman band intensity or more complex parameters such as principal components derived from che-mometric analysis . The user can rapidly re-view the data by rotating and zooming in on the volume in real time, with control over colors and transparency .


Micro Raman at Pittcon® 2012by Barbara Foster

In Figure 2, for example, a ruby’s chro-mium R2 photoluminescence band was used to reveal internal stress . First, the surface was indented . Next, using move-able plane slices within the volume, spec-tra were displayed from three different perspectives—in this case, two planes per-pendicular to the surface across the cen-ter of the indent, and a third in a plane below the indent . Data like these help materials scientists understand deforma-tion and fracture mechanisms .

Micro Raman for the nonresearch userMicro Raman is not just for the research lab, however . B&W Tek (www .bwtek .com) introduced the new BAC151A Video Mi-croscope Sampling System (Figure 3) . The new system is compatible with all B&W Tek Raman probes, featuring XY control with coarse and fine adjustments as well as Z-axis to focus the laser on the desired plane to maximize the Raman signal . An optional dual laser configuration offers input for two different lasers through a single port . The integrated camera facilitates precise Raman sampling through BWSpec™, permitting both laser beam tracking and image capture .Enwave (www .enwaveopt .com) takes a simi-lar approach with the μSense line, which uses fiber optics and video to connect Ra-man to laboratory-based stands .

Figure 1 - Nanodiamond in polymer matrix: a) 1 μm diamond (center speck) in polymer matrix (yellow circle), b) Raman spectrum without DSF, and c) Raman spectrum with DSF revealing clean spectrum of diamond without interference of fluorescence background or Raman signal from the matrix.

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BaySpec (www .bayspec .com) retains full capabilities in its upper end offering, Nomadic, but introduced the clever new MovingLab, which integrates a rotatable PC into the microscope head, making it espe-cially useful for forensics labs and field work .

The DeltaNu ExamineR™, developed by its Intevac Vision Systems group (www . intevac .com), uses a free-space design to cre-ate a unique modular system that mounts atop virtually any microscope . The system comes in two wavelength variations—532 nm and 785 nm—and offers two software options: NuSpec™ for instrument control, data acquisition, and library development; and NuImage™ for Raman mapping . An additional attachment performs Raman analyses on liquids .

Micro Raman for studentsBioTools (www .btools .com) announced the new BioRAMAN™ at Pittcon (Figure 4) . This shoe-box-sized micro Raman system features interchangeable objectives (40× and 60×) for micro work and UV cuvettes for solution work, an ideal combination for college labs or small start-ups interested in using micro Raman to investigate the bio-molecular structure of proteins and similar materials . Dr . Rina Dukor also explained that their unique new design has improved their signal-to-noise ratio twofold .

Polarized light emerging as an important Raman and IR adjunctHoriba’s technical guru, David Tuschel, stressed the importance of keeping the microscope fully functional while asking, “What else is possible?” and found that using polarized light opened opportuni-ties for new crystallographic investigations that complement X-ray diffraction studies . In his recent molecular spectroscopy ar-ticle,1 David explains that Raman scattering depends not only on molecular mass and bond strength, but also crystal symmetry and orientation . As a result, it is highly sus-ceptible to the direction and polarization of both the incident and resulting scattered illumination . Using the conventional polar-izer on a microscope to control the incident illumination and the analyzer to control the polarization direction of the scattered light enables collection of highly informative mi-cro Raman spectra . As he points out in the abstract, these “polarization/orientation (P/O) micro-Raman [spectra] can be used to identify vibrational modes, determine crystal structure, distinguish allotropes and polymorphs, differentiate single from poly-crystalline materials, and determine orien-tation of the crystal and degree of disorder, all on a micrometer scale .” He goes on to describe application to ionic solids, cova-lent solids, and molecular crystals and for

EDITOR’S PAGE continued

the characterization of minerals, integrated electronics, photonic devices, microelectro-mechanical systems (MEMs), photovoltaics, field effect transistors (FETs), and the newly emerging organic semiconductors includ-ing light-emitting diodes (OLEDs) .

Anasys (www .anasysinstruments .com), well known for its “AFM+” (AFM+thermal analysis, AFM+IR), has now added Pol to study molecular orientation . A nanosec-ond pulse of polarized IR radiation causes the AFM probe to resonate . Measuring the amplitude of the IR absorbance directly under the probe as a function of polariza-tion angle delivers direct measurement of molecular orientation . Using the AFM as a platform allows the user to measure and visualize molecular orientation with nano scale spatial resolution .

Figure 2 - 3-D imaging of stress within a ruby using Renishaw’s new StreamLineHR.

Figure 3 - B&W TEK’s BAC151A Video Micro-scope Sampling System uses a standard C-mount head and fiber optic Raman feed to attach to any microscope stand.

Figure 4 - The new shoe-box-sized BioRAMAN from BioTools offers the flexibility of both a microscope and a cuvette system, and features sample holders for a) liquids, b) microscopy samples, and c) solids.

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Traditionally, micro Raman has been most extensively used in the materials sciences . However, BioTools has taken the combination of the Pol-Raman to a different level, especially targeted at the life sciences . The ChiralRAMAN2X™ measures Raman Optical Activity (ROA), defined as the difference in Ra-man intensity for the right (R) minus left (L) circularly polarized light in-cident on or scattered by chiral mole-cules . The ChiralRAMAN2X integrates a Raman spectrometer with an inverted microscope and is especially helpful in characterizing biomolecular structures and behavior of proteins, nucleic acids, carbohydrates, and viruses under realis-tic, aqueous conditions .

Micro Raman moves into health care and high throughputRenishaw debuted the RA800 series, a new automated platform for health care, developed with partner Renishaw Diag-nostics (www .renishawdiagnostics .com) in Glasgow, Scotland . One variant is al-

ready in use with Renishaw Diagnostics Ltd. (RDL), where it forms part of RDL’s RenDx™ RUO Multiplex Assay System, developed as a tool for research into infec-tious diseases . The accompanying SP-1000 robotic sample processor contains several different modules including a washing station with unique integrated magnetic heater/shaker . The SP-1000 is thermally controlled and can process 46 samples and controls in under 2 .5 hr . All RenDx assays use novel patented technology based on surface enhanced resonance Raman spec-troscopy (SERS) .

SERS has been a topic of some discussion over the past several years . Until recently, these active substrates have been difficult to manufacture . However, in addition to Renishaw’s offerings, the Pittcon floor saw a dramatic expansion in SERS activi-ties, notably from companies like Thermo Fisher Scientific, offering both silver and gold substrates, and Real-Time Analyz-ers (www .rta .biz), which targets the high-throughput arena with its SERS 96-well plates, capillaries, and vials .

EDITOR’S PAGE continued

SummaryFrom research stand to student “shoe box,” the microscopy/spectroscopy chasm is defi-nitely shrinking as micro Raman becomes part of the analytical mainstream in both the materials and life sciences . Optical mi-cro Raman has become a mainstay and is now an important correlative technique to AFM-Raman, giving “eyes to chemistry” from the nano scale to the micro scale .

Reference1 . Tuschel, D . Molecular spectroscopy work-

bench: Raman crystallography in theory and in practice . Spectroscopy Mar 2012, 27(3); www .spectroscopyonline .com .

Barbara Foster is President and Chief Strategic Con-sultant, The Microscopy & Imaging Place, Inc. (“The MIP”), McKinney, TX, U.S.A., and Consulting Editor, American Laboratory/ Labcompare; tel.: 972-924-5310; e-mail: [email protected]; www.MicroscopyMarket.com. Ms. Fos-ter extends her thanks to all of the product managers, technical, and senior staff who so generously provided their time for interviews at Pittcon.

Introducing the GCMS-QP2010 Ultra — Shimadzu’s

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For gas chromatography (GC), the big news at Pittcon® 2012 was the absence of Agilent (www .agilent .com) and PerkinElmer

(www .perkinelmer .com) . This was a con-sequence of an overall downsizing caused by the “six-year effect” where the cycles of ACHEMA and Analytica coincide . Many firms are reluctant to increase promo-tional spending, so compromises must be made . The reduction of spending at Pittcon was evident across the board, but was particularly strong in GC . Twenty years ago, Pittcon was viewed by spec-troscopists as the world’s largest meeting in separation science . Slowly at first, the focus shifted: At Pittcon 2012, spectros-copy clearly dominated the exhibition .

New gas chromatographsSCION™ GC/MS systemsBruker (www .bdal .com) has a long his-tory of innovation in mass spectrometry, so when the company acquired the Varian GC and quadrupole mass spectrometers, I expected interesting advances . It didn’t take long . The new SCION™ SQ™ (single quadrupole) and TQ™ (triple quadrupole) GC/MS systems—which won the Pittcon Editors’ Silver Award—utilize unique ion optics to improve signal-to-noise . For ex-ample, the TQ uses an elliptical ion path to cancel out noise . Plus, active focusing of the helium molecules reduces dispersion, which improves peak heights .


Conference Review

The mass spectrometers are designed to enable the nonspecialist to use the power of MS detection without the hassle of com-plicated method setup and data analysis . For example, the SCION TQ GC/MS/MS facilitates multiple reaction monitor-ing (MRM) . The operator enters the name of the analyte, and the MRMs autofill from a library of 2500 analytes . Support-ing application notes for food, beverage, environmental, forensics, sports medi-cine, and petrochemicals are available . When coupled to either the Bruker 436 or 451 GC, the entire package has a very small footprint . The 451 GC has flame ionization detection (FID), electrochemi-cal detection (ECD), thermal conductiv-ity detection (TCD), thermionic specific detecton (TSD), and pulsed flame photo-metric detection (PFPD) options . Other options include purge and trap, program-mable temperature vaporizer (PTV), and solid probe inlets .

Bruker also upgraded the software to the CompassCDS™ 3 .0 Scalable Software So-lution . As the name implies, the software scales from a single instrument and PC to multiple chromatographs in a client server mode . Specific applications such as natural gas, transformer oil PIONA, and simulated distillation are supported via application-specific plug-in modules . The Compass-CDS is 21 CFR Part 11-compliant, with audit trails and encrypted all-in-one data files .

GCMS-QP2010 SE GC/MSEntry-level quadrupole mass spectrometers continue to decline in price, reflecting improved design and higher unit volume, which justifies more tooling . To seize this advantage, Shimadzu Scientific Instru-ments (www .ssi .shimadzu .com) introduced the GCMS-QP2010 SE . The design focuses on economy and simple operation of ba-sic features . Ion optics are optimized with a high-performance quadrupole mass fil-ter . Fully automated MS tuning provides consistent results . The instrument can use most common columns, provided the carrier gas flow is no greater than 4 mL/min . The SE also includes an ecology mode that reduces function and electrical power by about 50% when the run sequence has been completed .

Company founders Genzo Shimadzu, Sr . (1839–1894) and Genzo Shimadzu, Jr . (1869–1951) were honored as recipients of the 2012 Pittcon Heritage Award for their contributions to metrology . The senior Shimadzu founded the firm in 1875 to pro-vide service to imported instruments and also manufacture distillation devices and Atwood machines (accelerometers) . The younger Shimadzu expanded the firm into balances and spectrographs, including X-ray .

TRACE 1300 Series GCIn many labs, each GC is dedicated to a single application, often operating 24/7 . They are optimized at purchase for the

by Robert L. Stevenson


Key developments in separation science shown at Pittcon® 2012, held March 11–15 in Orlando, FL, are highlighted in this article . This comprehensive, three-part review features gas chromatography (GC) columns and consumables, innovations in supercritical fluid chromatography (SFC), and advances in liquid phase separation .

Trademarks are owned by Avantor Performance Materials, Inc. or its affi liates unless otherwise noted.© 2012 Avantor Performance Materials, Inc.

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GAS CHROMATOGRAPHy continued

the natural stream bed smell, and was told that it was “geosmin” (4S, 4aS,8aR)-4,8a-dimethyl-1,2,3,4,5,6,7,8-octahydronaphthalen-4a-ol . The human nose has a detection threshold of about 5 ppt .

800 Series thermal energy analyzerIn the mid-1970s, Thermo Instruments was a startup manufacturing a nitrosamine detector for GC and LC that was as sensitive as it was expensive and large . This was a niche market mostly dealing with cig-arette smoke . Thermo moved on to other things, and ultimately sold off the detector product line . Over time, Ellutia acquired the tech-nology (www .ellutia .com) . This year, the company introduced the 800 Series TEA (thermal energy analyzer), which includes an embed-ded GC and detector . The 800 operates in two modes, each of which is specific for nitrogen analytes . In the nitrogen mode, GC effluent passes through a catalytic pyrolyzer operating at 700 to 850 °C, which oxidizes the analytes to NO and on to nitrosamines . Ozone gas is added, which forms excited NO2

* . This rapidly decays to the ground state by emitting light, which is detected with the photomultiplier .

For assaying nitro and nitroso analytes, the column effluent is pyro-lyzed under reducing conditions . The resulting NO is reacted with ozone to produce NO2

*, which decays rapidly by emitting light at 600 nm . Detection sensitivity compared to carbon is 107 . The detec-tion limit is <2 pg/sec .

CALIDUS™ micro GCLast year at Pittcon, Falcon Analytical (www .falconfast .net) intro-duced the CALIDUS™ Model 101-HT micro gas chromatograph, which provided very fast separations in a portable instrument . This year the news was 1) Falcon was purchased by SGS Group Management (www .sgs .com) and 2) the CALIDUS provides a complete simulated distillation of petroleum, meeting the re-quirements of ASTM Method D2887 in 9 min or less . Chrom Perfect® process control software from Justice Laboratory Software (www .justiceinnovations .com) now controls and takes data from the CALIDUS .

GC sample preparationSuccess in assays by GC often requires selecting appropriate sample preparation . Thus, several firms introduced new technology to fill application niches .

LC-GC 9000According to Brechbühler (www .brechbuhler .ch), coupling LC to GC offers simple sample prep with high enrichment, high resolu-tion, and improved detection sensitivity . The sample is fractionated by LC . Fractions of interest are transferred by a hard plumbed valve to a high-volume GC injector for GC separation, including any conventional GC detector such as MS or MSn . Switching the LC column effluent to GC can be based on time or triggered by detec-tor response . Noneluting materials for the LC stage are backflushed to waste . The entire instrument is called the LC-GC 9000 . Since

application . Also, a small footprint improves productivity since one can squeeze more chromatographs onto the bench . With these macros in mind, Thermo Fisher Scientific (www .thermofisher .com) introduced the TRACE 1300 Series GC . The instrument can be configured with a range of injectors and detectors as dictated by the application . The company seems to favor the ion traps or quad-rupole . The volume of some detectors has been reduced to improve detection sensitivity . Injector backflushing is available . The human interface is via a computer for the 1300 . The TRACE 1310 uses an icon-based touchscreen .

TRIDION™-9 GC/TMSOver the last five+ years, Torion (www .torion .com) introduced a series of portable GC/MS instruments . Each generation shows significant improvements over prior models . The TRIDION™-9 is the latest and most portable . It still uses a toroidal ion trap mass an-alyzer (TMS), but the weight has been reduced to 30 lb, including the helium cartridge for the carrier gas . Typical run times are less than 3 min . Target applications include chemical-biological warfare (CBW) agents, environmental, and food safety .

CANARY-3™ and LIGA-GCDefiant Technologies (www .defiant-tech .com) introduced two novel GC systems with micromachined columns and detector for environ-mental monitoring . The CANARY-3™ starts with a choice of three thermal desorption preconcentrator inlets tuned to different volatil-ity ranges . For high volatiles, a torturous path preconcentrator has a very high surface-to-volume, finned structure that supports sorptive coatings . The coatings are sol-gels, which provide high capacity, selec-tive retention, and low mass . Upon heating, the low thermal mass releases the analytes in a plug to the GC . The column is a work of micromachined art . It is a three-layer sandwich called the LIGA-GC . The center is a nickel coupon with an array of holes . The “bread” is a LIGA machined serpentine that connects the holes in series to give a 1-m column the size of a dime . For 10 m of length, the column is layered to form a cube, smaller than a sugar cube .

Detection is with a delay-line surface acoustic wave microbalance resonator, which is about the size of a dime . The resonator is coated with a thin sorptive polymer . The sorption/desorption process produces a signature that is unique to each analyte . Two cells are used: One is for reference, and the other monitors the column effluent . A microprocessor converts the difference to a signal that is proportional to the detected mass . Detection limits are low picogram levels .

At the other end of the booth was the FROG-4000™, a handheld micro GC system for monitoring volatile organics, including BTEX (benzene, toluene, etc .), alcohols, ketones, etc ., with an analysis time of less than 5 min with a temperature-programmed run . The interior de-sign is similar in design to the CANARY, but is equipped with a pho-toionization detector (PID) and extended front legs to sit on a pond perimeter or stream bank . I asked what chemicals were responsible for


Sampling uses a valve and loop flow path for reliability and precision . The sample path is entirely chemically inert and thermostated . This guarantees complete transfer of the sample and eliminates car-ryover . Applications include blood alco-hol, residual solvents in pharmaceuticals and food packaging, BTEX in water, and residual monomers in polymers . The Master also supports purge-and-trap sam-pling, which improves the detection limit by 100 times compared to prior models . The Master is compatible with all known GCs . Optional tray cooling is designed for biosamples .

Versa headspace vial samplerStatic headspace sampling is popular be-cause it is fast, easy, and works well for vola-tile organics (VOCs) in a range of matrices . Teledyne Tekmar (www .teledynetekmar .com) relies on years of experience to of-fer a range of headspace samplers . The latest, the Versa, features a small foot-print, yet holds 20 × 22 mL vials . The sample pathway is constructed of inert materials and can be heated to 200 °C . The headspace sampler performs an au-tomated leak checking protocol for trou-ble detection and resolution .

Sampling dissolved gasesEclipse 4660 purge-and-trap sample concentrator/4551A water autosamplerGood business in the analytical instrument industry is often a case of being in the right place with the right product at the right time . Sampling dissolved gas, especially methane, is a case in point . Fracking of gas-producing strata has raised concerns about dissolved gases, particularly methane, in water supplies . O.I. Analytical (www .oico .com) presented a poster describing the use of the Eclipse 4660 purge-and-trap sample concentrator and 4551A water autosam-pler for fracking studies of methane in wa-ter . A significant number that will require remediation were found .

Brechbühler is a channel partner for Ther-mo Fisher Scientific, the preferred modules are the TRACE Ultra GC with large-volume on-column injection and Phoenix 40 binary pump for the LC . One application was the residual oil in recycled cardboard, which is used for food packaging .

GPC sample preparationPower-Prep™ GPCOf course, LC in the form of gel perme-ation chromatography (GPC) has been used for decades for off-line sample prep for GC . Gilson (www .gilson .com) contin-ues to promote a GPC feeding a fraction collector, which then serves as an autosam-pler for GC . Fluid Management Systems (www .fmsenvironmental .com) introduced the Power-Prep™ GPC system . Each dis-posable column is packed with cross-linked polystyrene/divinylbenzene bead-packed PTFE tubes . Pesticide residues, polychlori-nated biphenyls (PCBs), and dioxins ap-pear to be the major focus of the Power-Prep . Sorbents for solid-phase extraction (SPE) are silica gel, alumina, Florisil™ (U.S. Silica Company, www .ussilica .com), and C18 . Cleanup with GPC reduces sol-vent, expensive glassware, and operator time compared to manual methods .

Static headspace samplingMaster static headspace samplerHeadspace sampling of air above a liquid sample has evolved over the last 35 years . It is still attractive, since headspace analysis is not labor-intensive, provides excellent de-tection limits, and avoids risks of contami-nation with other samples and the opera-tor . The Master static headspace sampler from DANI (www .danispa .it) provides a carousel sample tray for 120 vials . Each vial is identified by bar code . Vial size ranges from 10 to 22 mL . Before analysis, the oven controls the sample temperature of 18 vials, with constant, user-controlled incubation time . A shaker accelerates and improves efficiency, improving detection sensitivity and reducing variability . The automatic leak check ensures sample integrity .

Thursday, April 19, 2012 11:27:41 AMColor profile: Disabled

LGX50 sample preparation module for GCSampling liquids for dissolved gases is a real engineering chal-lenge since gas–liquid interfaces must be avoided . Attempting to move a liquid too quickly produces cavitation, compromis-ing the sample . With these constraints in mind, EST Analytical (www .estanalytical .com) introduced the LGX50 sample prepara-tion module for GC via the U .S . EPA’s RSK175 (3810) proto-col . The LGX50 contains two racks for 50 40-mL septum-sealed vials . One rack holds the samples; the other holds blank vials with a stir bar . Before adding sample, the vial is purged with He to remove CO

2 and air . A controlled aliquot of the liquid

sample is transferred to the evacuated blank vial along with an internal standard . The sample liquid is protected from external contamination or analyte loss . The sample is heated and stirred for a proscribed time before transferring the headspace to the sample loop for assay by GC with appropriate detectors such as an FID for hydrocarbons .

Model 7400 for sampling dissolved gasesCDS Analytical (www .cdsanalytical .com) introduced the Model 7400, also for sampling dissolved gases in water . The 7400 fea-tures a 72-position autosampler with three trays for 24 vials . Internal standard addition is automated . All sample contacting pathways are PEEK, silica, or electroformed nickel for reduced carryover and contamination .

Model 4000 pyrolyzerPyrolysis of solids combined with GC often provides unique signa-tures that facilitate tracing the origin of the material . For example, a poster from CDS compared pyrograms of various plastics to confirm that they were indeed made with renewable materials . Some were as advertised, but others appeared to be copolymers of both bio and petroleum sources . The Model 4000 pyrolyzer from CDS quickly in-



stalls on any GC . It uses a resistively heated platinum coil that can be heated at any rate between 0 .01 °C/min and 20,000 °C/sec . GC in particular often uses canisters for sampling volatile analytes .

Gas sampling technology is often split between canisters and sor-bent tubes . Canisters are suitable for total sampling, including per-manent gases, while sorbent tubes are more suitable for analytes that are reactive with sorbents or condensable .

CIA Advantage™Markes International, Inc. (www .markes .com) introduced the CIA Advantage™ for automated analysis of VOCs in canisters . The CIA is designed for 27 canisters, which enables unattended 24/7 operation . Addition of internal standard is automated . No cryogen is required, saving thousands of dollars per year . Carryover is reduced to less than 0 .2 ng by heating the transfer lines to 200 °C . With GC/MS, the de-tection limits are less than 0 .1 ppb . Using the selected ion monitoring (SIM) mode on the MS reduces the detection limit to less than 10 ppt .

Model 2012 air samplerThe Model 2012 air sampler from CDS Analytical is optimized for the collection of volatile organics according to U .S . EPA Method TO-17 . The compact, portable air sampler has a capacity of four tubes . An embedded computer controls all functions, including se-quential sampling for up to 12 hr with a booster battery .

Two-Stage Brass Small-Profile Regulator/Analytical Series Point-of-Use ManifoldsIn chromatography, smaller is generally better . Airgas, Inc. (www .airgas .com) introduced two complementary products to supply high-purity gases for GC and other purposes . The new Two-Stage Brass Small-Profile Regulator is much smaller, which reduces the

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Stir bar for the Twister®

Stir Bar Sorptive Extraction (SBSE) with the GERSTEL Twister® (www .gerstel .com) is a simple, economical technique for extracting and concentrating analytes from solutions . Extraction efficiency depends on partition-ing between the sorbent on the stir bar and the sample matrix . This year, the company introduced the EG-S ethylene glycol-silicone coated magnetic stir bar, which provides po-lar (H-bonding) selectivity to complement the PDMS sorbent . PDMS preferentially sorbs nonpolar analytes . Use of both bars provides an overall analyte profile of volatile and semivolatile organic compounds . After sorbing the analytes, the Twister bar is load-ed in a thermal desorption injector to the GC . Since the EG-S bar also sorbs some wa-ter, the solvent vent mode is recommended . The EG-S phase has a Tmax

of 220 °C .

Sample dryingPowerVap ConcentratorDryng samples is probably the biggest time sink in most sample preps for chro-matography . If one is not careful, sam-ples can be overdried and thus destroyed . With these and other pain points in mind, Fluid Management Systems in-troduced the PowerVap Concentrator, a standalone direct-to-vial concentration system that processes up to six samples in parallel but with individual control of each . For example, the evaporation/dry-ing of material in each of the the six wells is monitored continuously with optical sensors . When the endpoint is reached, the flow of drying nitrogen is turned off, along with the heater . The sample is col-lected in a 500-μL or 1-mL autosampler vial, which is attached to the bottom of the larger sample tube .

MultiPurpose SamplerA similar sample-drying module was intro-duced by GERSTEL GmbH & Co. (www .gerstelus .com) for the MultiPurpose Sam-pler (MPS) . Samples are concentrated un-der user-defined temperature and vacuum . Solvent exchange for improved detector compatibility is a common task that can be selected by a mouse click in a sequence

footprint, opening up new design possibili-ties for the lab . The clean sweep flow path quickly flushes residual gas, which can be a concern after changing cylinders .

With good reason, many labs locate the gas supply outside the laboratory . Airgas pre-sented Analytical Series Point-of-Use Mani-folds, which are intended for high-purity gas use (99 .9999 percent pure) . These man-ifolds incorporate a packless diaphragm inlet valve, compact regulator (above), and outlet metering valve, providing gas control at the bench . Multiple manifolds can be mounted onto a single back plate so that all gases are in the same panel .

Injection syringesDiamond DesignAs detection limits in GC/MS get smaller, chromatographers are discovering design problems that had not been seen before . Take the common syringe—SGE (www .sge .com) found that the old design occasionally had problems with carryover traced to the adhesive that joins the needle hub to the glass barrel . Occasionally, the adhesive was not filled to the end, leaving an exposed annulus, or the adhesive could contact and thus contaminate the sample . To eliminate this, SGE introduced the Diamond De-sign, in which a PTFE seal isolates the bar-rel from the metal tip . This also increases syringe lifetime by 10 times .

Solid-phase extractionSPE-Xpress™U .S . EPA Method 1664 for oil and grease just got easier with the introduction of the SPE-XPress™ from Environmental Express (www .envexp .com) . Each unit is capable of processing three 1-L water samples in paral-lel with a throughput of about 1/hr/station . The SPE-XPress filters a 1-L sample and ex-tracts the oil and grease from the SPE disk with n-hexane . The hexane solution is col-lected in a tared aluminum pan, where it is evaporated to dryness and ready for weigh-ing . User-friendly software controls internal steps, such as verification of complete sam-ple processing and conditioning of the SPE disk, plus makes data available to a LIMS .



table . The MPS is used in GC, HPLC, and MS . GERSTEL also introduced a shaker module for the MPS, which provides either shaking or vortexing up to 3000 rpm . Up to eight vials can be pro-cessed at a time . Mixing movement is restricted to horizontal mo-tion, which prevents sample loss on the vial cap .

Hydrogen generators for GCGas chromatography columns generally run better when hy-drogen is the carrier gas . Plus, FIDs require hydrogen with

very low organic contamination . The choice is usually between hydrogen generators and high-pressure tanks . Hydrogen gen-erators have certainly improved . F-DGS SAS (www .f-dgs .com) exhibited a line of hydrogen generators for GC, including generators for multiple instruments . Hydrogen purity is better than 6 nines; maximum delivery pressure is 240 psi . Residual water is removed with a desiccant cartridge . Control is via a 128 × 64 touchscreen . Water is from a 2 .3-L internal reser-voir or can be plumbed directly from an external source of 10- megohm water or higher . No acid or base is required .

Columns for gas chromatographyRtx®-BAC columnsNew columns for assay of blood alcohol from Restek (www .restek .com/BACPlus) provide rapid (<2 min) isothermal, base-line separation of ethanol, methanol, ac-etone, tert-butanol, acetaldehyde, isopro-panol, and n-propanol . The two-column set (BAC-1 and BAC-2) give chromato-grams with changes in elution order, for confirmation of peak identification . Each column is individually tested with a BAC test mix .

Secondary columns for C×GCSecondary columns in GC×GC need to be fast (i .e ., short) and with broad selectivity . Restek introduced the Rtx 200 series (www .restek .com/catalog/view/32442/15124) as secondary col-umns with a trifluoropropyl surface chemistry that provides orthogonal selectivity to phenyl, cyano, and Carbo-wax stationary phases . The Rtx 200 col-umns are thermally stable, low bleed, and compatible with difficult analytes such as phenols . T

max is 340 °C .

RT®-Alumina Bond/MAPD columnsBecause of high selectivity, alumi-na is often preferred for separating light petroleum factions containing C2–C5, including olefins . Restek RT®-Alumina BOND/MAPD PLOT columns (www .restek .com/catalog/view/11267) provide rapid separation


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of hydrocarbons up to a Tmax

of 250 °C . Stable response factors make the MAPD column ideal for process applications where recalibration must be minimized . The columns are available in fused silica and metal (MXT®) .

MXT®-Q-BOND columnsMetal columns are more robust and hence suitable for portable instruments . Restek metal MXT®-Q-BOND and MXT-S-BOND PLOT phases (www .restek .com/chromatogram/view/GC_PC1184) were developed for the assay of oxygenated solvents . Columns are available in tight 3 .5- or 7 .0-in . coils .

Triart Hybrid columnsYMC America, Inc. (www .ymcamerica .com) extended its family of Triart Hybrid columns . Since their introduction, the high pH stabil-ity of the columns has attracted attention, but also raised the obvious question of scaleability . Some chromatographers are reluctant to de-velop analytical methods that do not scale to prep and potentially process . Thus, YMC in-troduced bulk phases on particle cuts of 10, 15, 20, and 50 μm . Now you can pack your own prep scale columns . The company also showcased its full range of particle sizes of the Triart C8 .

Nano stationary phase technologyOne poster in particular caught my eye . Dr . Allen Britten of Cape Breton Uni-versity in Nova Scotia presented a series of posters on nano stationary phases with better efficiency and resolution than I’d seen before . Below is a quote from his poster abstract (2090-3P):

This current investigation is re-lated to the evaluation of nano stationary phase (NSP) GC capil-lary columns for environmental sample analysis . The stationary phase has the same composition as that of conventional station-ary phases, but due to its nano size, the particles form a specific orientation with the capillary sur-face . Surface bonding and cross-

linking of the NSP provides su-perior thermal stability compared to that of high molecular weight polysiloxane stationary phases . Better selectivity of the NSP is due to a specific orientation, re-sulting in a stronger interaction of analytes . The selectivity and stability of NSPs are the two most important properties differentiat-ing them from conventional sta-tionary phases .

I’m sure that we will see much more on nano stationary phase technology in the near future .

Column hardwareSilTite™ µ-unionFor five decades, SGE has built a reputa-tion for producing small parts that solve real problems in separation science . The latest example is a very small and hence low-thermal-mass fitting (<0 .5 g) designed to couple GC columns in a temperature-programmed oven . Cool spots must be avoided . The SilTite™ μ-union uses SGE’s double cone ferrule to make the seal without wrenches for fused-silica capillar-ies . This should be particularly useful in GC×GC or creating mixed column sets, including guard columns .

SilTite ferrules for GC injectors and detectors are available in graphite, Vespel®

(DuPont, www2 .dupont .com), and SGE’s proprietary SilTite FingerTite . The latter provides a strong, maintenance-free, creep-free connection . It is particularly recom-mended for GC/MS .

A review of new instruments and col-umns for liquid phase separation ap-pears on page 38 . Supercritical fluid chromatography systems are reviewed on page 28 .

Robert L. Stevenson, Ph.D., is a Consultant and Edi-tor of Separation Science for American Laboratory/Labcompare; e-mail: [email protected].


Pittcon® 2012 was held March 11–15, 2012 at the Orange County Convention Center in Orlando, Florida . The fol-lowing product showcase provides a brief outline of new and current laboratory equipment and instrumentation

featured at the conference, from solutions for sample preparation, particle analysis, and other measurement-based systems, to general laboratory equipment .

Sample preparationAutomated sample preparation workstationThe new Omni LH96 automated workstation from Omni Inter-national (www .lh96 .com) takes sample preparation to a new level by combining homogenization, liquid handling, pipetting, and weighing in a single platform small enough to still fit inside a lami-nar fumehood . The LH96 automated workstation is customizable to an application’s sample prep, such as pharmaceutical, drug dis-covery, proteomics, sample processing, and nanotechnology .

Protein quantitation systemEMD Millipore (www .millipore .com) launched the new Direct Detect™ bio-molecular quantitation system for the measurement of protein quantity in a sample as low as 0 .2 mg/mL to 5 mg/mL within just a few seconds . The Direct Detect system utilizes infra-red measurement for the analysis of proteins rather than UV-VIS spectroscopy measurement from conventional assays, such as the Bradford and Lowry assays, which are somewhat limited .

Automated library construction systemThe new SPRIworks HT from Beckman Coulter (www . beckmancoulter .com) is an automated library construction sys-tem for high-throughput sample preparation . The SPRIworks HT solution for Illumina next-generation sequencers (NGS) processes up to 96 libraries a day with improved speed with or without size selection and greater reproducibility, as compared to only eight li-braries a day manually . The SPRIworks HT can also be automated on an automated liquid handler for additional methods, including polymerase chain reaction (PCR) .

UltracentrifugeBeckman Coulter also showcased the new Optima X Series Ul-tracentrifuges (Figure 1), which provide several key features useful for enhanced end-user experience, including quiet centrifugation


Conference Review by Jeanely Hunt


Figure 1 - Optima X Series Ultracentrifuge.

Figure 2 - Ultra Centrifugal Mill ZM 200. Watch video at http://goo.gl/cIiO1.

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cross-contamination, the RevElution can procure sample volumes up to 2 L with a sample range that includes bacteria, fungi, molds, and whole cells of various other samples for testing in food and bev-erage, environmental, or life science ap-plications . This easy-to-use sample prep instrument can be applied for cell culture, immunoassay, and PCR .

SonicatorThe new Q55 Sonicator from Qsonica (www .sonicator .com) is a compact ul-trasonic processor that utilizes minimal bench space and is relatively simple to operate . This sonicator operates at a 20-kHz frequency for cell disruption of standard samples and other sample prep small volumes .

Particle analysis and size measurementThe FlowCAM PV Series imaging par-ticle analysis system from Fluid Imaging Technologies (www .fluidimaging .com) was unveiled at Pittcon . The particle vision (PV) series provide economical image particle analysis in a small benchtop footprint . The systems are capable of running up to 32 si-multaneous measurements for a variety of applications, such as quality control of drug formulations, characterization of silica par-ticles and column packing, and wash-water analysis .

Micromeritics Instrument Corporation (www .micromeritics .com) showcased an extensive line of instruments for materi-als characterization, including surface area analyzers and porosimetry systems . Included in the line were several particle size analyzers . The Saturn DigiSizer® II high-definition digital particle size ana-lyzer was highlighted . This digital particle size analyzer uses light scattering to detect particles from 40 nm to 2 .5 mm .

The WAVE Series electroacoustic and con-ductivity pore analyzers from Quantachrome Instruments (www .quantachrome .com) were demonstrated at Pittcon . These pore charac-terization systems can measure pore size range of 10 nm–5 μm, +0 .1 mV min pore

at less than 51 dBA, remote monitoring from a computer or smart phone, secu-rity compliance and tracking, simulation protocols saving time and sample, and energy efficiency . Available in two models (XE and XPN), these ultracentrifuges can reach a maximum of 100,000 rpm and 802,000 × g .

Laboratory millThe Ultra Centrifugal Mill ZM 200 (Figure 2) with a new cyclone from RETSCH (www .retsch .com) is a laborato-ry rotor mill with a speed range of 6000–18,000 rpm for fine grinding of samples in various applications, including envi-ronmental, pharmaceuticals, materials, and food . Featuring a newly redesigned cyclone, the ZM 20 rotor mill improves its flexibility for sample preparation of 250-mL to 5-L volumes .

The 6970 EFM Freezer/Mill from SPEX SamplePrep (www .spexsampleprep .com) was showcased with new program functions . This laboratory freezer/mill can maintain samples at liquid nitrogen temperature without direct contact to liquid nitrogen . It is also capable of milling samples ranging from 0 .5 to 100 g for various applications, such as pharmaceuticals, materials testing, pathology, and environmental .

Laboratory evaporatorThe RapidVap Vertex evaporator from Labconco Corporation (www .labconco .com) processes samples using dry heat and the nitrogen blow-down method for applications in drug discovery, environmental, forensic testing, and clinical analysis . With a capacity of up to 50 samples in the same run, the Rapid-Vap dry evaporator is ETL, ETL-C, and CE compliant .

Laboratory concentratorLabconco Corporation also featured the RevElution Bio-Concentrator . This bio-concentrator system features a small footprint that can concentrate liquid microbial samples at 100 mL/min with 90% analyte recovery . With no risk of

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Dual beam microscopeFEI Company (www .fei .com) showcased the Versa 3D DualBeam™ microscope, which provides three-dimensional imag-ing and analysis for a variety of sample types . Capable of running both a high-vacuum and low-vacuum mode, electron beam and ion beam resolution will vary . This flexible configuration also al-lows characterization of materials with an additional environmen-tal scanning electron microscope (ESEM) mode option .

Hyperspectral imaging systemThe new HI 90 hyperspectral imaging system from Bruker Cor-poration (www .bruker .com) is an imaging system based on remote chemical sensing for the determination and quantification of haz-ardous gases . With scanning speeds 1000 times faster than tradi-tional systems, the HI 90 system has a range of applications in-cluding environmental testing, forensics, and homeland security . The imaging is a result of real-time video overlay and hyperspectral imaging with standard 850–1440 cm–1 spectral range .

Laboratory instrumentationAutomatic biochemistry analyzerNewly introduced at the conference, the YSI 2900 biochemistry analyzer from YSI Inc. (www .ysilifesciences .com) automates the biochemical analysis of a wide range of analytes, such as glucose, lactate, ethanol, choline, and sucrose with analysis time of 60 sec or less . Equipped with a proprietary enzyme electrode, this bio-chemistry analyzer can provide fast and analyte-specific results in a variety of samples for applications in bioprocessing, food and beverage, biofuels, and clinical laboratory testing .

Flow calorimeterTTP Labtech (www .ttplabtech .com) introduced the chipCAL, a microliter flow calorimeter for rapid screening and optimization of enzyme analysis and characterization . The chipCAL nearly auto-mates the analysis of enzyme activity within 2–10 min . With only as small as a 15-μL sample, this flow calorimeter cuts down on the

zeta potential, and 0 .5% porosity resolution of various sample types in chromatography, materials, or environmental applications .

Malvern Instruments Ltd. (www .malvern .com) showcased the new Mastersizer 3000 laser diffraction particle size analyzer with small benchtop footprint . Capable of analyzing both dry and wet samples, the Mastersizer 3000 particle size analyzer measures par-ticle size distribution from 0 .01 to 3500 μm .

The new CAMSIZER XT particle analyzer from RETSCH en-ables the measurement of particle sizes from 1 μm to 3 mm for finer samples (wet or dry), including shape, quantity, density, and transparency . Improved optical resolution allows the particle size analyzer to improve product quality for materials, food, and phar-maceutical applications .

Microscopy/imagingMicroscope Digital CameraThe new BLC line of Microscope Digital Cameras with an LCD tablet was introduced by Carltex Inc. (www .carltex .com) . These new microscope tablet cameras provide comparable quality images to CCD cameras; are easy to install; and provide 2 megapixels, 1600 × 1200 resolution . This high-definition laboratory digital tablet camera has key applications in laboratory research and aca-demic learning environments .

Scanning electron microscopeThe Phenom proX desktop scanning electron microscope (SEM) from Phenom-World BV (www .phenom-world .com) is a three- dimensional imaging system with magnification of 80–45,000× . The Phenom proX SEM can perform 30 sec or less sample load-ing . Equipped with an energy-dispersive spectroscopy (EDS) detec-tor as well, the Phenom proX is also an X-ray analysis system since the sample’s elemental composition can also be determined .

Figure 3 - CIA Advantage.

Figure 4 - SC 950 vacuum pump. Watch video at http://goo.gl/yAR4v.


for Karl Fischer and potentiometric titrations . These compact titra-tors come in many different versions for respective applications .

Laboratory equipmentLaboratory vacuum pump KNF Neuberger Inc. (www .knf .com) introduced the new SC 950 vacuum pump system (Figure 4) . This vacuum pump short-ens the processing time of solvents with a high pumping capac-ity of 50 L/min and deep end vacuum of 1 .5 Torr . The SC 950 laboratory vacuum pump system has a small footprint and is available with wireless remote . With four operating modes, the laboratory vacuum pump is flexible for a variety of labora-tory applications .

Laboratory diaphragm pumpVacuubrand (www .vacuubrand .com) featured the ME1 line of Compact Oil-Free Diaphragm Pumps . These diaphragm pumps al-low for efficient single or multiple filtrations in a compact design . With 75 Torr (100 mbar) ultimate vacuum and 14 1pm (0 .5 cfm) free air capacity, the ME1 diaphragm pumps provide quiet and low vibration operation for a variety of applications, such as chemistry, microbiology, and environmental testing .

Fume HoodThe new UniMax Floor Mounted Fume Hood was announced by HEMCO Corporation (www .hemcocorp .com) . This line of laboratory walk-in fume hoods is available in a variety of sizes and can easily accommodate systems such as distillation apparatus and reactors . The UniMax Fume Hood features a modular design that is chemical resistant, allowing for customization of designs for an individual laboratory’s requirements .

Glassware washerThe System4Lab glassware washer cleaning solution (Figure 5) was showcased by Miele (www .miele-pro .com) . This solution includes a laboratory glassware washer, lab service, glassware detergents,

amount of precious sample needed to provide low-cost biological assay analysis . With the potential for high-throughput screening, applications for the chipCAL flow calorimeter include the food, fermentation, and biopharma industries .

RefractometerThe new Pro-Juice refractometer from Bellingham + Stanley (www .bs-ltd .com), featured for its application in food and bev-erage testing, was designed to overcome repeatability issues ex-perienced when using conventional refractometers . The refrac-tometer prevents irregular measurements through the use of a peristaltic pump and provides thermal conditioning treatment for premeasurement of the sample to provide overall consistent and reliable results .

VOC analysis systemMarkes International (www .markes .com) showcased the CIA Advantage™, an automated volatile organic compound (VOC) analysis system designed for canister air and gas (Figure 3) . This cryogen-free VOC analyzer is fully U .S . EPA Method TO-14/15 compliant . With a detection limit of <0 .1 ppb, the CIA Advantage can analyze both high- and low-concentration samples, and can easily add to all major GC and GC/MS systems .

pH meterSenova Systems Inc. (www .senovasystems .com) announced at the show the new pHit pH Sensor, a calibration-free, solid-state pH meter . Replacing traditional glass electrodes, the pHit eliminates the need for calibration . It also eliminates the need for expen-sive buffers and overall maintenance . This new pH sensor has wet-dry reversible use to provide versatility for typical research or medical applications .

Pipette testing systemBrandTech Scientific Inc. (www .brandtech .com) showcased the new BRAND PLT™ Pipette Leak Testing Unit . This useful pipette leak tester validates the functionality of pipettes to ensure accurate performance in the lab without having to send pipettes out for calibration . The easy-to-use PLT can detect air displacement and leak rate at 1hPa ml/s .

Liquid handling robotic systemMetrohm USA (www .metrohmusa .com) presented the 898 XYZ Sample Changer, a liquid handling robotic system . The sample changer automates the analysis of many samples with up to 82-sample capacity .

TitratorThe Ti-Touch Titrator Series from Metrohm USA was also fea-tured . These new compact titrators for routine analysis are available


and an application support lab—all under a five-year limited warranty .

Laboratory counting scaleAdam Equipment (www .adamequipment .com) unveiled a new line of weighing scales, the Warrior wash-down scales . A robust design from stainless steel pro-vides stability for a variety of weigh-ing applications, in particular, those for pharmaceutical and cleanroom require-ments . In addition to standard weigh-ing, the Warrior scale line also can provide percentage, dynamic, animal, and check weigh-ing, and parts and check counting . These laboratory scales provide measurement in grams, kilograms, ounces, pounds, and Newtons, in various languages including English, Spanish, French, and German .

Water purification systemRephiLe Bioscience Ltd. (www .rephile .com) introduced both the new, large Direct-Pure EDI water systems and large Direct-Pure RO water systems . The EDI water system has a water production rate of 30–120 L/hr, whereas the reverse os-mosis water system can product 50–150 L/hr (depending on the model) . Designed for larger laboratories and applications in buffer/media preparation, feedwater for ultrapure water systems, and chemical analysis, these two high-flow water systems can process up to 2000 L of water per day .

Laboratory consumablesCertified reference standardsSPEX CertiPrep (www .spexcertiprep .com) introduced new certified reference standards for trace metals . Primarily for food testing, in particular the wine indus-

try, these wine standards are offered for both red and white wine for trace metal analysis . Available in 21 mL, these trace metal standards also provide additional sample information, such as alcohol con-tent, sulfite, and chloride levels .


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Laboratory softwareThe ACD/Spectrus Workbooks by Advanced Chemistry Development, Inc. (www .acdlabs .com) was launched at the show . This new laboratory software solu-tion is equipped with techniques specific for analytical characterization in spec-troscopy, spectrometry, and separation science . The ACD/Spectrus laboratory software can capture analytical data and chemical structure for data processing and interpretation for these various laboratory analytical techniques .

ConclusionPittcon, the premier exhibition for intro-ducing the latest laboratory instrumenta-tion and equipment, will be held next year at the Pennsylvania Convention Center in Philadelphia, the “City of Brotherly Love .” The dates are March 17–21, 2013 .

Compare and learn more about these new products and other laboratory equipment at www .labcompare .com .

Jeanely Hunt is Content Editor for American Laboratory/Labcompare; e-mail: [email protected].

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Thirty years ago, supercritical fluid chromatography (SFC) was described optimistically as the mode of the future, uni-

fying and replacing GC and HPLC for many applications . Although this has not happened yet, Waters (www .waters .com) clearly has the vision now . Waters has enjoyed 20/20 vision in the past, so let’s check back in 2020 .

ACqUITy UPC2™Waters added a Pittcon Editors’ Gold Award to its collection of plaques from prior years . The new ACQUITY UPC2™ (UltraPerformance Convergence Chroma-tography™) is showing greatly improved and truly useful detection sensitivity using SFC . Last year, I reported on six new SFCs on the floor at Pittcon®, including the ACQUITY® SFC from Waters . These clear-ly demonstrated that improved technology was reigniting market interest .

Despite introducing a new analytical SFC chromatograph in 2011, chromatogra-phers at Waters saw that ACQUITY SFC was only the first step in a long staircase . They decided to take the express eleva-tor to the top . UPC2 combines SFC with Waters UPLC® technology and expertise in fluidics, kinetics, and thermodynamics to deliver fast, reproducible separations . For example, supercritical CO

2 has very low vis-

cosity, which improves mass transfer kinetics, and hence column efficiency, even compared to hexane or water . The SFC region offers another degree of freedom to the operating space . Thus, one can vary pressure and tem-perature independently to optimize a separa-tion . With CO

2, pressure can change solubil-

ity of analytes significantly . Plus, CO2 is more

compatible with MS than most any other mo-bile phase, and is much less expensive .


Conference Review

During the Q&A following the formal introduction, Art Caputo, President of Waters, predicted that UPC2 will grow quickly and relegate HPLC and GC to niche techniques in eight years . He pointed out that ACQUITY technology was introduced eight years ago, and today the LC business is dominated by ultrahigh-performance liquid chromatography (UHPLC) . Point made!

Let’s look at the advantages first: Waters believes that UPC2 is ideal for tough-to- analyze compounds, including hydro-phobics and chirals, lipids, fuels, natural products, surfactants, and thermally labile analytes . As an example, Waters showed an 18-peak chromatogram of mixed analytes complete in less than 8 min . The peaks are very narrow . A side-by-side comparison of an impurity profile with reversed-phase liquid chromatography (RPLC) confirms that SFC can be much more efficient, and also has or-thogonal selectivity .

Now for the limitations: SFC of polar mole-cules needs to be worked out . SFC still works best for chloroform-soluble analytes . Perhaps someone will develop SFC-HILIC (hydro-philic interaction chromatography) technol-ogy for polars . Also, SFC has not shown util-ity for analytes larger than about 10,000 Da . Will it work for membrane proteins? This is a difficult application segment for HPLC and UHPLC . Then there is the cost of in-struments—SFC is a bit more expensive than UHPLC . This difference could be made up by improved productivity and lower mobile phase cost . But an SFC costs four times as much as a comparable GC . The cost of mo-bile phase in GC is low, especially if one uses hydrogen generators, so the economics are not favorable . Historically, the rate of conver-sion to a superior technology (e .g ., capillary columns replacing packed columns) in GC is only about 3% per year .

New preparative SFCChiral separations are the most often-cited advantage of SFC, both on the ana-lytical and preparative scale . JASCO (www . jascoinc .com) introduced the Prep-2088 preparative SFC, which features a circular dichroic (CD) detector, optimized mobile phase pumps, and backpressure regulator . The CO

2 pump has a cooled pump head .

Maximum flow is 120 mL/min with a Pmax

of 5000 psi . The modifier pump has a maxi-mum flow of 80 mL/min . The new back-pressure regulator keeps the system stable, irrespective of the flow . Constant pressure is essential to control solubility .

One example in the press conference that introduced the Prep-2088 showed a chiral separation of two enantiomers that provided resolution of about 0 .7, which means that the valley between the two-peak maxima is a mixture . Using the CD signal as a guide, the operator collected the leading edge of the first peak and the trailing edge of the last peak . The middle valley, which is a mixed fraction, was collected for reinjection . This is not a new concept in prep, but the conve-nience and performance of the 2088 appears to qualify as a major advance .

SFC columnsIn the past, chromatographers chose col-umns for SFC from the long list of HPLC columns . This worked, but it is now appar-ent that SFC can be improved with columns that have been designed, packed, and tested for SFC .

BEH 2-EP, CSH Fluoro- Phenyl, and HSS C18 SBIn support of the UPC2, Waters introduced three columns and promised one more . Each is specifically optimized for SFC .



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future, you should consider this as part of column scouting for method development .

Advances in liquid phase separations chromatography from Pittcon® 2012 are reviewed on page 38 . A review of gas chro-matography instruments and columns appears on page 12 .

Robert L. Stevenson, Ph.D., is a Consultant and Editor of Separation Science for

American Laboratory/Labcompare; e-mail: [email protected].

1) The BEH 2-EP (ethylpyridine) is bonded to a 1 .7-μm ethylene-bridged hybrid particle . This is a general-purpose phase that provides good retention, peak shape, and selectivity . 2) The BEH phase pro-vides stronger interactions with polar groups, such as phospholip-ids, than the 2-EP phase . 3) The CSH Fluoro-Phenyl column uses Waters charged surface hybrid technology to bind fluorophenyl li-gand . This phase is recommended for weak acids, bases, and neutrals . Columns range in size from 2 .1 × 50 to 150 mm . Particle size is 1 .7 μm . Midyear, Waters plans to introduce the HSS C18 SB surface chemistry on 1 .8-μm high-strength silica . All four phases will also be available in 3 .5-μm diameter .

GreenSep™ Basic SFCLast year, ES Industries (www .esind .com) also introduced columns optimized for SFC, which offer superior selectivity, peak shape, and durability . The most recent introduc-tion, GreenSep™ Basic, binds imidazole to 3- or 5-μm silica spheres . Pore diameter is 120 Å . Compared to GreenSep Ethyl Pyri-dine, the imidazole phase provides much stronger retention and improved selectivity for separation of amine-containing analytes .

GreenSep SilicaSilica is a commonly used stationary phase for SFC . All too often, the separations show tailing or broad peaks . This may be due to trace metal impurities in the silica . ES In-dustries selected high-purity silica for the GreenSep Silica columns . Packed columns are available with nominal particle size as small as 1 .8 μm and as large as 20 μm .

COSMOSIL 3-hydroxyphenylNacali USA, Inc. (www .nacalaiusa .com) in-troduced the COSMOSIL 3-hydroxyphenyl column, specifically optimized for SFC of beta blockers . Compared to the 2-ethylpyri-dine stationary phase, the elution orders are reversed for pindolol and atenolol with the same SFC mobile phase .

SFC column classificationIt appears that the ideal stationary phases for SFC may be different than HPLC . The problem is how to scout and classify them . To help in this curation, David Kohler and Matt Przybyciel of ES Industries de-veloped a range of test probes that help classify and select columns with maximum diversity in selectivity . If SFC is in your

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This past March, some 15,754 peo-ple from 90 countries descended on Orlando, Florida, for the annual Pittsburgh Conference

on Analytical Chemistry and Applied Spectroscopy (Pittcon®) (www .pittcon .org/exhibitors/attendstats .php) . As always, the conference is an opportunity for tech-nology vendors to get face time with their customers, and for researchers to glimpse the latest and greatest those companies have to offer . This year’s Pittcon featured 948 exhibitors, from A&D Weighing to Zoex, promoting products to support a range of technologies and industries . Here, American Laboratory rounds up some of the more interesting product launches in spec-troscopy and mass spectrometry .

NMR spectrometerpicoSpin™-45LThe picoSpin™-45L benchtop NMR spec-trometer (www .picospin .com), available from Cole-Parmer (www .coleparmer .com), is a 45-MHz NMR weighing just 10 .5 lb (4 .7 kg) . Intended primarily for educational labs, reaction monitoring, and QA/QC laborato-ries, the fully integrated, compact device (7” × 5 .75” × 11 .5”) features a permanent (as op-posed to superconducting) magnet, mean-ing it requires no liquid nitrogen or helium, and uses a standard AC adapter so that it can be easily moved around and plugged in where needed . An Ethernet port facilitates data collection .

The picoSpin-45L requires no NMR tubes; samples (20 μL) are injected into a user-replaceable capillary sample loop, and though it requires relatively concentrated samples (>1 M for dissolved solids or >1% v/v liquids), it does not require deuterated solvents, says Alex Zhang, Marketing Asso-


Conference Review

ciate at Cole-Parmer . “You can use regular solvents as long as they don’t interfere with the molecules you are monitoring,” he says .

The picoSpin cannot handle proteins or “other molecules with multiple chiral cen-ters,” Zhang says . However, according to Jeff Sherman, picoSpin’s Director of Global Sales, the system offers “typical resolution of 60 ppb” 1H and 19F spectra for small mol-ecule work, making it “an outstanding tool for routine organic analysis .”

NIR spectrometerMicroNIR™The MicroNIR™ spectrometer from JDSU (www .jdsu .com) is a lightweight, extremely compact (45 mm diam × 42 mm high), near-infrared spectral engine that utilizes a linear variable filter (LVF) as the dispersing element . Available in two wavelength ranges (950–1650 nm and 1150–2150 nm), the MicroNIR supports real-time evaluation, field testing, and on-line process monitoring to allow lower-cost sampling .

Electron magnetic resonance spectrometerAffirmoEX™Also releasing a benchtop instrument for the education market was Oxford Instru-ments Magnetic Resonance (OIMR) (www .oxford-instruments .com) which, with Active Spectrum Inc. (www .activespectrum .com), introduced the AffirmoEX™ bench-top electron magnetic resonance (EMR) spec-trometer . As its name suggests, EMR is like NMR but focuses on unpaired electrons rath-er than nuclei . It is typically used to monitor free radicals and the oxidation state of transi-tion metals . The basic technology has been

by Jeffrey M. Perkel


around for decades, says OIMR Product Mar-keting Manager John Paul Cerroti . Yet, until recently, EMR required costly, massive, and complicated equipment and dedicated per-sonnel . As a result, the technology has been slowly dying; today, says Cerroti, “Very few universities have a working EMR .”

Measuring 10” × 10” × 11 .25” and weigh-ing just 14 lb (6 kg), the AffirmoEX is small enough to fit on a benchtop and features an easy-to-use touchscreen inter-face and two USB ports for data storage . Its small size, says Cerroti, stems from two advances: small, powerful rare-earth mag-nets, and cell-phone technology that can produce gigahertz frequencies in a minia-turized package .

Commercial EMRs use frequencies ranging from about 3 to 260 GHz . The AffirmoEX functions at 9 .7 GHz (X-band) and, according to Cerroti, specifically targets two key application areas besides education: transportation, to monitor lubricating oils used in airplanes, trains, and automobiles; and food preparation, to quality-check cooking oils .

ICP/OESSPECTROBLUESPECTRO Analytical Instruments (www .spectro .com) showcased its SPECTROBLUE inductively coupled plasma optical emission spectrometer (ICP/OES), first launched in September 2011 . The SPECTROBLUE compact, midrange spectrometer is ideal for environmental laboratories looking for an economical, high-throughput spectrom-etry system . It has an air-cooled design; thus there is no need for an expensive, external water-based cooling system . Furthermore, its sealed optic system eliminates gas purging .


Laser-induced breakdown spectroscopy instrumentRT100 LIBSApplied Spectra (www .appliedspectra .com) demonstrated a series of new applications for its RT100 LIBS, a laser-induced breakdown spectroscopy (LIBS) instrument first displayed at Pittcon 2011 . LIBS is like ICP/OES, except the plasma is generated by a laser rather than an Rf generator .

According to General Manager Jong Yoo, LIBS technology is not new, but “in terms of product development, right now is a really vibrant time,” due largely to advances in miniaturization and detection . This year, the company highlighted some new applications being pursued by both its in-house scientists and collaborators, from forensics (differentiating types of paint or glass, for instance), to iden-tification of “conflict minerals” like tantalums, to RoHS (Restriction on Hazardous Substances) .

Electrical impedance spectrometerINPHAZEThe new INPHAZE from eDAQ (www .edaq .com) is a high-resolution electrical impedance spectroscopy (HiRes EIS) system for the study of thin films and layers . It provides a rapid and sensitive method to reveal the nano-structural layers of samples .

SpectrofluorometersFluoroLog® EXTREME and FluoroCube EXTREMEHORIBA Scientific (www .extremefluorescence .com) announced what it calls the “world’s first commercial integrated supercontin-uum powered spectrofluorometers .” The systems pair HORIBA

Scientific’s FluoroLog® (for steady-state fluorescence) (www .horiba .com/scientific/products/fluorescence-spectroscopy/steady-state/f luorolog/f luorolog-r-our-modular-spectrof luorometer-522/) and FluoroCube (for fluorescence lifetime) (www .horiba .com/ scientific/products/fluorescence-spectroscopy/lifetime/fluorocube/fluorocube-our-compact-benchtop-spectrofluorometer-825/) spectrofluorometers with the SuperK EXTREME white light laser from NKT Photonics (www .nktphotonics .com) to create the FluoroLog EXTREME and FluoroCube EXTREME, respectively .

According to Ishai Nir, director of the fluorescence division at HORIBA Scientific, the white light laser replaces the high-powered xenon arc lamps typically found in steady-state spectrofluorometers, and the many diode lasers often used in fluorescence lifetime instru-ments, offering picosecond pulse rates and relatively uniform, tun-able excitation at wavelengths ranging from about 450 nm to 2400 nm . That means users can access a broader range of fluorophores than they otherwise might, and tweak their experimental conditions more precisely to separate overlapping emission signals .

Users could always purchase a spectro-fluorometer and white light laser, Nir says . The integration, though, is not trivial, as it requires precise timing, resolution, and software control . “It’s difficult to get these instruments to work together reliably,” he says . “That’s why the integration…is so valuable .”

Raman instrumentsAlso generating buzz at Pittcon were handheld Raman spectrome-ters . Handheld Raman analyzers enable users to analyze materials on site, whether running QA checks on chemicals on a pharmaceutical company loading dock, or identifying counterfeit or illegal drugs in the field .

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as Composition-B produces a single broad fluorescent peak at 785 nm, but a diagnostic series of discrete peaks at 1064 . Target appli-cations include raw material identification, reaction monitoring, narcotics and counter-feit drug detection, and homeland security .

Verifier™ Process System 1000The Verifier™ Process System 1000, a Ra-man analyzer for use in pharmaceuticals and chemical manufacturing, was show-cased by Mustard Tree Instruments (www . mustardtree .com) . Launched in January, the VPS-1000 is a laptop-sized device that is de-signed specifically to fit in the most compact pharmaceutical and chemical processing locations . The powerful, rugged analyzer carries out sensitive real-time testing of liquids, powders, solids, gels, suspensions, and emulsions under many harsh condi-tions and hygienic environments .

More handheld RamanOther commercial handheld Raman analyzers include the Thermo Scientific TruScan® from

B&W Tek also plans to introduce an app so that live readings can be monitored remotely .

Xantus-2-785/1064Rigaku Raman Technologies (www .rigakuraman .com) also unveiled a hand-held, Wi-Fi-enabled Raman device, the Xan-tus-2-785/1064, which the company calls “the world’s first dual wavelength handheld Raman analyzer .”

The compact (13 .8 cm × 27 .4 cm × 9 .8 cm), 8 .1-lb Xantus-2 can excite samples at both 785 nm (as most handhelds do, using a CCD detector) and 1064 nm (using an InGaAs detector) . According to Product Marketing Manager Elizabeth Yarbrough, this dual-wavelength capability means the device can obtain a Raman reading even with samples that fluoresce at 785 nm .

“In the pharmaceuticals industry, you can see 30% more material at 1064 nm than at 785 nm, because so much of it fluoresces at 785 nm,” she says . The same is true of explosives; the explosive mixture known

NanoRam™B&W Tek Inc. (www .bwtek .com) rolled out its NanoRam™ handheld Raman spectrometer . The 1-kg NanoRam looks a bit like a Nintendo handheld game system, but with an iPhone-like user interface . According to Marketing Manag-er Robert Chimenti, that makes the NanoRam exceptionally easy to learn . At Pittcon, he says, users could figure out how to use it in seconds, without documentation . “Think of it like a voltmeter,” he explains—a tool to facilitate end users’ applications rather than as an analytical research instrument, per se .

The NanoRam features a cooled charge-cou-pled device (CCD) detector for greater stabil-ity and signal-to-noise ratios, and real-time Wi-Fi connectivity . This means that data can not only be offloaded to databases or to su-pervisors for go/no-go decisions, but also that method, library, and software updates can be pushed to the instruments as needed . That said, Chimenti notes that each NanoRam can function as a standalone unit if desired . “You can create and manage libraries, develop meth-ods . It’s a completely standalone instrument .”

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Thermo Fisher Scientific (www .ahurascientific .com/truscan) and the PinPointer from Ocean Optics (www .oceanoptics .com) . Many other op-tions can be found at www .labcompare .com .

XRF instrumentsNEX QC VSApplied Rigaku Technologies (www .rigakuedxrf .com) has added to its energy-dispersive X-ray fluorescence (EDXRF) in-strument line with the NEX QC VS . The VS is an optional variation of the NEX QC low-cost benchtop EDXRF launched at Pittcon 2011 . The NEX QC features a 4-W, 50-kV X-ray source for nondestructive el-emental analysis from sodium to uranium . The VS options incorporate collimators to focus the X-ray beam down to 14, 8, or 3 mm, plus a 1 .3-megapixel complementary metal oxide semiconductor (CMOS) cam-era and light-emitting diode (LED) lighting for accurate beam placement .

With an icon-based “modern touchscreen interface,” the NEX QC VS was designed for two specific applications, says Product Manager Scott Fess: RoHS screening of tox-ic metals in plastics, and jewelry analysis for recycling and valuation .

GoldXpertOlympus Innov-X (www .olympus-ims .com) presented the portable, countertop GoldXpert XRF analyzer . The simple-to-use XRF analyzer provides a cost-effective way to obtain alloy chemistry and karat classification with one nondestructive and nonintrusive test . Among its many features, the analyzer is able to identify and characterize alloys such as silver and platinum, as well as point out poison ele-ments within samples .

UV-VIS spectrophotometersNanoDrop™ LiteThermo Fisher Scientific (www .thermofisher .com) launched its NanoDrop™ Lite at the International Plant & Genome XX Confer-ence in San Diego in January, but showed it off to a far wider audience two months later at Pittcon .

The NanoDrop Lite is an application- specific variant of the more full-featured NanoDrop 2000/2000c and NanoDrop 8000, all of which can measure UV ab-sorbance in samples as small as 1 μL . But whereas the 2000 and 8000 models can acquire full spectra, the NanoDrop Lite is designed specifically to measure absor-bance at 260 and 280 nm, values that are used to quantify and assess the purity of nucleic acids .

“That gives the ability to create a simpler and smaller version of the NanoDrop 2000, and that’s what the NanoDrop Lite is,” says Simon Nunn, Global Mar-keting Director for Molecular Spectros-copy at Thermo Fisher Scientific . The NanoDrop Lite features the same cu-vette-free “pedestal” design of its more full-featured cousins, says Nunn, but in-stead of a broad spectrum light source and detector array, the NanoDrop Lite uses LEDs and a simple silicon photodi-ode detector .

Measuring just 16 × 11 .5 cm, the result-ing package is fully contained—there’s no need to attach it to an external PC—and “literally fits in the palm of your hand,” Nunn says . An optional printer prints labels for refrigerator and freezer test tubes .

UV-2600 and UV-2700Making their Pittcon debuts were Shimadzu Scientific Instruments’ (www .ssi .shimadzu .com) newest UV-VIS spec-trophotometers, the UV-2600 and UV-2700 . (Both officially entered the market in September 2011 .)

The 2600 is a single monochromator in-strument capable of reading out to 1400 nm; with two monochromators, the 2700 delivers ultralow stray light across a more conventional range to 900 nm . Both have a smaller footprint than do their prede-cessors, the UV-2450 and UV-2550, says Product Manager Mark Talbott, and both feature Shimadzu’s proprietary “Lo-Ray-Ligh” diffraction gratings, “which pro-vide a broader scan range with lower stray light values .”

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intuitive software interface, and is an ef-fective plug-and-play solution that can be used at any time without the need for con-sumables or maintenance .

ATR probes/interface modulesAxiom Analytical (www .goaxiom .com) and Symbion Systems (www .gosymbion .com) displayed high-performance at-tenuated total reflectance (ATR) probes and interface modules for the Bruker Alpha™ FTIR . Features include maxi-mum sensitivity for mid-IR analysis and interchangeability with Bruker Quick-Snap™ modules . The Sl-Alpha1 inter-face module is optimized for use with ATR probes and flow cells . The compa-nies also offer f lexibly coupled diamond and conventional ATR probes and mul-tipass Raman probes for more than 10× enhancement in sensitivity .

FTIR systemsFTIR sealed liquid cellInternational Crystal Laboratories (www .internationalcrystal .net) featured a heated variable-pathlength cell for FTIR spectrophotometers that can be heated to 200 °C . A programmable ramp and soak temperature controller with RS232 serial cable computer interface is provid-ed with the cell . The cell pathlength can be adjusted continuously from 0 .05 mm to 5 mm .

MB-Rx Reaction MonitorABB (www .abb .com) showcased its MB-Rx Reaction Monitor, an FTIR analyzer for real-time, in situ monitoring of chemi-cal reactions . Measuring 43 .5 cm × 28 .0 cm × 37 .2 cm, the MB-Rx is small enough to fit in a chemical fumehood . The moni-tor features a rugged insertion probe and

With stray light values of 0 .005% and 0 .00005%, the UV-2600 and UV-2700 can measure up to 5 and 8 .5 absorbance units, respectively . That makes the 2700 especially effective for highly absorbent materials, such as sunglass polarizers, welding helmets, and so on . “Anything that has very low transmission, or that is highly absorbing, the 2700 would have good potential for,” Talbott says .

DMV-Bio CellStarna Scientific Ltd. (www .starna .com) displayed its new Starna Demountable Mi-cro-Volume (DMV) Bio Cell, an ultralow-volume cell for use in most UV-VIS spec-trophotometers . The DMV-Bio is available in 0 .5-, 0 .2-, and 0 .125-mm pathlengths . Using sample volumes down to 0 .6 μL across a wide range of concentrations, the cell delivers accurate and reproducible mea-surements on existing spectrophotometers .


Mass spectrometers and accessories TripleQuad™ 4500 and QTRAP® 4500AB SCIEX (www .absciex .com) intro-duced two 4500 series LC/MS/MS systems, the TripleQuad™ 4500 and QTRAP® 4500 . The two instruments are both LC-based triple quad instruments, but the Q3 in the QTRAP 4500 can function either as a quadrupole or as a linear ion trap for greater sensitivity . The 4500 series spectrometers build on AB SCIEX’s popular API 4000 . According to Product Manager Brent Lefebvre, they have been optimized to handle faster ultra high-performance liquid chroma-tography (UHPLC) systems and feature design elements of the company’s higher-end 5500 spectrometers, including faster electronics, better sensitivity, and “a curved ion path for a smaller footprint .”

Lefebvre says AB SCIEX is targeting the 4500 series at a few key applied markets, including food, environmental, clinical re-search, and forensic toxicology . One key ap-plication, he says, is pesticide screening, in which customers might need to screen for hundreds of compounds in a single run .

Normally, says Lefebvre, optimizing such a method can be laborious . In this case, the company has done much of the work already, developing canned iMethods™ that specify sample preparation protocols, Phenomenex (www .phenomenex .com) columns, multiple reaction monitoring (MRM) transitions, and retention times for each compound . The user simply selects the desired pesticides, and the system’s scheduling software does the rest, configur-ing the instrument to specifically scan for each pesticide at the correct retention time . “If you follow our method, you can do one injection and screen for 400 pesticides,” Lefebvre says .

iCAP QThermo Fisher Scientific showcased the Thermo Scientific iCAP Q ICP/MS, an er-gonomically designed, quadrupole ICP/MS that utilizes right-angle positive ion deflection (RAPID) lens technology for the separation of ions and neutrals . The ICP/MS features proprietary QCell technology .

Q ExactiveThe Thermo Scientific Q Exactive benchtop LC/MS/MS from Thermo Fisher Scien-tific combines high-performance quadrupole precursor selection with high-resolution, accurate-mass Orbitrap detection, offering a maximum scan speed of 12 Hz and mul-tiplexing capabilities . Resolving power is up to 140,000 .

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(http://scionhasarrived .com) won the 2012 Pittcon Editors’ Choice Silver Award . Featuring a model 436 or 451 GC on the front end and a triple-quad mass analyzer on the back end, the SCION TQ features several design innovations, according to Marketing Director Meredith Conoley, including a parallel (not orthogonal) GC inlet, a “heated q0 ion guide” for eliminating interference from neutrals in the source flow, and a “lens-free design” that reduces maintenance requirements .

According to Conoley, one key application is pesticide identification in food . The SCION TQ, he says, can typically detect pesticides at 0 .5 ppb or lower, some two orders of magnitude below typical regulatory requirements . That makes the system “analytically robust,” he says, and also provides “headroom or foot room” in case those requirements become more stringent in the future .

As a result of Bruker’s Compound-Based Scanning (CBS) experimen-tal design software, developing methods to identify those pesticides en masse is easier as well . Users can forgo much of the pain of optimizing complex MRM studies, selecting instead the compounds they wish to detect and letting the software work out retention and dwell times, optimal fragmentation ions, and so on .

“We basically allow users to go through our library, select which components they will analyze, and all the rest of the work is done,”

Conoley says . “So you are going from weeks of work [optimizing the method], down to a few hours .”

Also unveiled at Pittcon was Bruker’s ionBooster™ “next-generation high sensitivity” electrospray ion source, which the company claims can yield 5–100-fold improvements in sensitivity .

LAESI® DP-1000Winning the Bronze Award at Pittcon 2012 was the LAESI® DP-1000 ionization source from Protea Biosciences (http://proteabio .com/LAESI) . LAESI (laser ablation electrospray ionization) is an ionization method in which a midinfrared laser (2940 nm) excites the O–H bonds of untreated aqueous (e .g ., biological) samples under ambient conditions, ablating the sample, which is then ionized in an electrospray . It can be used to raster across a sample, such as a leaf, in situ, producing a two-dimensional spatial map—that is, a mass spec-tral image—of molecular abundance . By ablating repeatedly, users can also generate 3-D maps as well, for instance to show metabolite abundance in the various layers of a tissue .

The LAESI DP-1000 is compatible with Thermo Fisher Scientific and Waters (www .waters .com) mass spectrometers . At Pittcon, Waters and Protea (www .proteabio .com) announced a co-marketing agreement “to make the DP-1000 available to new and existing users


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ConclusionNaturally, even this extensive list represents just a sampling of the many technologies launched or showcased at Pittcon 2012 . And new techniques are in development, for instance on the single-molecule level . W .E . Moerner, Chair of the Department of Chemistry at Stan-ford University and this year’s winner of the Pittsburgh Spectroscopy Award, has spent nearly three decades developing the single-molecule spectroscopy techniques underlying one of today’s hottest life-science technologies: super-resolution, single-molecule microscopy .

Bulk spectroscopic analyses are not going away, Moerner says . But they will be ever more complemented by single-molecule studies, ac-cording to him, at least in the life sciences, as researchers work to understand how enzymes, antenna proteins, and other biological macromolecules-proteins work . “Given that cells are factories made of individual machines…we can learn a lot by going to the single molecule level,” he says .

We’ll find out just how much we can learn when Pittcon 2013 con-venes March 17 in Philadelphia .

Jeffrey Perkel, Ph.D., is a Contributing Writer for American Laboratory/

Labcompare; e-mail: [email protected].

of Waters’ SYNAPT G2 and SYNAPT G2-S mass spectrometers run-ning under MassLynx® control .”

expression™ Compact Mass SpectrometerAdvion Inc. (http://advion .com/biosystems /expression) announced the commercial availability of its expression™ Compact Mass Spec-trometer (CMS) . Measuring just 10 .6” × 21 .6”, the expression CMS is a personal single-quadrupole mass spectrometer that is small enough for chemical fumehoods and laboratories that have limited space . Featuring easily interchangeable electrospray ionization (ESI) and at-mospheric pressure chemical ionization (APCI) sources for LC/MS, a mass range of m/z 10 to m/z 1200, and a resolution of <0 .7 m/z units, the expression CMS was developed for the discovery research and process development synthetic organic chemistry market, enabling real-time reaction monitoring and compound identification .

BenchTOF-dx™ALMSCO International (www .almsco .com), the mass spectrometry di-vision of Markes International Ltd. (www .markes .com), showcased the BenchTOF-dx™ benchtop time-of-flight mass spectrometer . Intended for GC/MS, the BenchTOF-dx has applications in the food and bever-age and petroleum industries, environmental analysis, and drug testing . The TOF/MS provides full-range spectra at the sensitivity levels of quad-rupole instruments running in selected ion monitoring (SIM) mode .

MMS-1000™1st Detect Corporation (www .1stDetect .com) announced the intro-duction of the MMS-1000™ miniature mass spectrometer, an ion trap mass spectrometer measuring just 7 .5” × 12 .5” × 9” and weigh-ing less than 17 lb . With a sensitivity of 1 ppt and a resolution of un-der 0 .5 Da FWHM, the MMS-1000 delivers rapid MS/MS detection of trace levels of volatile compounds in around 5 sec .

Microchannel platesPHOTONIS USA (www .photonis .com) announced in February the availability of a new long-life, low-noise (L3N) option for its micro-channel plates, which among other things, are components in time-of-flight detectors . Applications in which the background noise of the particular application is lower than the noise of the detector can especially benefit from the low noise option .

MASS-tastic Voyage 2012 bus tourPhenomenex and AB SCIEX kicked off a 30-city cross-country bus tour called the MASS-tastic Voyage 2012, a mobile lab—modeled on the semi-tractor trailers used to haul NASCAR cars—showcasing sample prepara-tion and chromatography columns from Phenomenex and liquid chro-matography systems and mass spectrometers from AB SCIEX . According to Phil Koerner, Senior Technical Manager at Phenomenex, the bus hosted “well over” 800 visitors at Pittcon, the first stop on a voyage that will cross the U .S . three times before terminating in Vancouver at ASMS 2012 in May . (See www .masstasticvoyage .com for a complete schedule .)

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Eight years have passed since Waters (www .waters .com) introduced the ACQUITY UPLC® . This is a long life cycle for a groundbreaking instrument . Already, ven-dors are offering components (tubing, valves, and fit-

tings) that will enable operation of next-generation ultra high- performance liquid chromatographs (UHPLCs) at 30,000 psi or so . The components will be expensive, since stronger alloys will be required to replace 316 stainless steel . While we wait for the next generation of liquid chromatographs, we can take a look at the noteworthy advances that have been made in instruments, col-umns, applications, and components for liquid phase separation .

Capillary ion chromatographsChromatographers at Thermo Fisher Scientific (www . thermoscientific .com) have extended the P

max of the Dionex

(www .dionex .com) ICS-5000 capillary ion chromatography system to 5000 psi . This includes the very popular RFIC™ (Reagent-Free™ Ion Chromatography) capability . More pressure facilitates faster separations using columns packed with 4-µm-diam particles . The ICS-5000 still uses the IC Cube module, which integrates sample and mobile phase handling in a small, convenient, chromatography-efficient package . With capillaries, mobile phase consumption is only 5 .25 L/yr in 24/7 operation . With RFIC, the mobile phase reservoir is refilled with pure water . This facilitates walk-up-and-inject operation . In addition to conductivity, the ICS-5000 is compatible with UV-VIS, MS, and the new Thermo Scientific QD . Control is via Chromeleon chromatography software .

Not all labs need the flexibility offered by the ICS-5000, so Thermo Fisher Scientific introduced the Dionex ICS-4000 capillary ion chromatography system, which also uses the IC Cube module and offers “always on” operation, 5000-psi capability, and multi-ple detector options . The 4000 has a smaller footprint than the 5000 . Chromeleon software manages the I/O and operation .

Nano LC platformNanospray electrospray ionization (ESI) detection typically provides superior detection in proteomics research . However, plumbing the components together (injector, column, ESI in-terface, and mass analyzer) is often frustrating . MassTech (www .apmaldi .com) introduced the “The-LCP” thermally stabilized platform for high-temperature nano LC separations . Running at an elevated temperature increases the separation efficiency . In


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one case, only 137 peptides were found for a protein digest with a column temperature of 20 °C . However, at 65 °C, the peak count increased to 303 . Some of the improvement is attributed to efficiency and some to an increase in recovery . Another study showed that running at 60 °C greatly improved consistency of relative peak heights, enabling quantitative protein profiling .

Modular LCsAnalytical Technologies Ltd. (ATL) (www .ais-india .com) is a new name to Pittcon in HPLC and other instruments . Products include a range of modular LCs, from several analytical systems to lab-scale prep and even larger to process-scale instruments for bioprocessing . Dedicated analyzers include ion chromatogra-phy and amino acid . Pump pressure is the most differentiating feature of HPLC . ATL offers a prep pump rated from 1500 to 4000 psi . Analytical pumps start at 6000 psi and extend up to 18,000 . Pre- and multipump gradient elution systems are also available . Detectors include refractive index, UV-VIS, diode ar-ray detection (DAD), digital amperometric, fluorescence, and evaporative light scattering . Columns range from analytical to axial compression preparative columns with diameters from 30 to 1000 mm . AnalChrom™ chromatography workstation soft-ware supports both preparative and analytical systems . The firm is represented in over 90 countries .

Low-pressure LC componentsOccasionally, I attend a press conference where the sub-ject matter is completely different than expected . This year, SFC Fluidics® (www .sfc-fluidics .com) hit me in the face . Pre-meeting promotional information led me to expect a new HPLC or perhaps an SFC system . However, after the first few minutes, I was certain there was much more . “SFC” in the company name stands for Small, Fast, Cost-effective components and systems, not supercritical fluid chromatography .

SFC is all about novel plastic components such as QuickCon-nect™ connectors, manifold, pump, and micromachined de-vices . QuickConnect fittings provide a butt-to-butt union of plastic tubing with very small dead volume . The fittings are held in place magnetically . The ePump® model 190 uses elec-troosmotic f low to deliver accurate, pulse-free f low over the nL to µL range . It is small (~1 in .3) and lightweight, and P

max

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the membrane . The volume increases, but is confined, so the pressure increases . A second impermeable f lexible membrane separates the osmotic section from the delivery f luid, which is expelled . A small controller operates the valves required for the pumping action .

The components have been assembled to make a low-pressure LC pumping system . It appears to be suitable for short columns using plastic capillary column technology with Superdex™ 75 column packing (GE Life Sciences, www .gelifesciences .com) for separating proteins, including bovine serum albumin (BSA), ov-albumin, myoglobin, and transferrin . SFC components should also be useful in flow injection analysis .

Recycling moduleFrom time-to-time, recycling chromatography reappears . Those who have been around long enough may recall that Waters promoted recycling intensely to improve resolu-tion in gel permeation chromatography (GPC) . The key is to make sure that the extracolumn band broadening, mea-sured in volume, is small compared to the peak width . Japan Analytical Industry Co., Ltd. (JAI) (www .jai .co .jp/english) in-troduced the NEXT recycling module for all of its preparative LCs . With recycling, the effluent from the column is routed to a detector and then back to the pump inlet for another pass through the column . In the ideal case, the chromatographic resolution increases by the square root of number of passes through the column . Two passes give an improvement of 1 .4, and four cycles a twofold increase, etc . JAI points out that recycling conserves solvent use and reduces the investment in columns .

DNA analyzer based on HPCEDespite the high resolving power, high-performance capillary electrophoresis (HPCE) is not in the spotlight . Indeed, it is not even on stage, or even in the audience, for that matter . Slab gel electrophoresis is still the most common technol-ogy for assaying nucleic acids and proteins . However, poly-acrylamide gel electrophoresis (PAGE) and agarose are slow, tedious, and often insensitive compared to HPCE with gel capillaries . Improved assay technology is needed, particularly for quantitative PCR of DNA . In response, BiOptic, Inc. (www .bioptic .com .tw) introduced the Qsep100 f luorescence dna-CE analyzer . The analyzer uses a pen-shaped gel cartridge, which feeds the DNA sample to a laser-induced f luorescence (LIF) HPCE . The system provides 2 .5-min separations with high detection sensitivity (4 bp resolution at 50–500 bp range) from a 96-well plate . Average %RSD in migration time is less than 0 .75% for a 10-run set from the same well . The unique optical design, which uses ball lenses, enables a price point that is much lower than currently available LIF-HPCE instruments . The Qsep100 received a Pittcon Editors’ Award honorable mention .

Field flow fractionation interfacePostNova Analytics (www .postnova .com) and Malvern Instruments Ltd. (www .malvern .com) announced an agreement that marries the PostNova AF2000 Series asymmetrical flow field flow fractionation system and the centrifugal field flow fractionation system with the Malvern Zetasizer Nano . The firms developed a field flow fraction-ation-dynamic light scattering (FFF-DLS) interface that increases the detection sensitivity by 3–4 times . Targeted applications include pro-teins, i .e ., aggregates, and nano particles of gold, silver, and carbon .

HPLC detectorsQD detector for ion chromatographyAt Pittcon 2011, a lecture by Dr . Kannan Srinivasan of Dionex described a new detector idea for ions . Compared to traditional suppressed conductivity, it was within about a factor of 10 in de-tection sensitivity, but for weak acids or bases, it was better . All ions with the same charge produced the same signal, that is, the detector responded to normality rather than molarity . A year later, Dionex is now part of Thermo Fisher Scientific, and the detector was introduced as the Thermo Scientific Dionex QD .

The QD is the world’s first charge detector for ion chromatog-raphy . It detects all ionizable species . It is recommended for de-tection of phosphates in environmental samples, organic acids in food and beverages, and amines . In some cases the relative response of the conductivity and QD detector can confirm iden-tity . The detector received a Pittcon Editors’ Award honorable mention . Also, Prof . Sandy Dasgupta (University of Texas at Arlington), who is named as inventor on the patent that is the basis of the QD, was honored with the Dal Nogare Award .

850 IC Amperometric DetectorMany of the analytes that are most suited for separation by ion chromatography lack strong chromophores or fluorophores for detection . Carbohydrates, amines, and acids are typical problem analytes . Metrohm (www .metrohm .com) introduced the 850 IC Amperometric Detector as an option to the Model 850 Profes-sional IC, 881 Compact IC pro, and 882 Compact IC plus . The detector can operate in series or in parallel with other detectors such as conductivity and UV-VIS absorbance . Detection sen-sitivity is low ng/L for electroactive analytes . Metrohm offers gold, silver, platinum, and glassy carbon working electrodes as required by the analytes . The reference and auxiliary electrodes are maintenance free . A standalone version of the detector is offered as the Model 896 Professional Detector .

quadrupole mass spectrometers for LC/MS/MSIONICS Mass Spectrometry Group (www .ionics .ca) introduced two new lines of triple quads for LC/MS . Both the Series 100 and 200 have two probe options . One option can be switched between ESI and atmospheric pressure chemical ionization

LIqUID PHASE SEPARATION continued


(APCI) detection in less than 20 msec, and the other is dedicated to one . Mass range is 5–1500 m/z . Dynamic range is better than 106 . Scan rate for the Series 200 is fast, at 27,000 data points per sec . With the Series 100, the data rate in-creases further to 50,000 pts/sec .

Ion mobility detector for HPLC and HPLC/MSIon mobility spectrometry (IMS) is par-ticularly useful in separating isomers . Excellims Corp. (www .excellims .com) introduced the AIMS2100 ESI high- performance ion mobility spectrometer as a detector module for HPLC and HPLC/MS . Adding the AIMS2100 to an LC/MS provides an orthogonal method for com-pound identification since IMS resolves isomers based on ion mobility rather than mass . Typically, the column effluent is split between the AIMS2100 and other detectors . The orthogonal nature of the detection reduces the need for LC×LC and SFC×LC, even for the most complex samples . Ionization with ESI improves detection sensitivity to the subnanogram range, especially of low-volatility analytes . Linear dynamic range is 102 to 103 . Typical applications include separation of skeletal peptide isomers, diastereomers, cis–trans isomers, and carbohydrates .

The most significant figure of merit for HPLC detectors is usually the noise level . SCINCO (www .scinco .com/en) intro-duced the DAD-208 diode array detector with a noise level of ±2 .5 × 10–6 AU . The diode has 1024 elements covering the range from 190 to 950 nm . Chromatogra-phers can select up to eight wavelengths to monitor at 50 Hz . Three flow cell op-tions have a volume of 2–15 .5 µL . The company is looking for OEM partners .

Flow splitter for detectorsSplitting column flow between detec-tors is a technique that sounds good in concept but is frustrating in practice . Analytical Scientific Instruments, Inc. (ASI) (www .hplc-asi .com) introduced the QuickSplit™ AS650 to automate flow splitting . The AS650 should open up

many new applications that would bene-fit from multiple detectors . The company points out that the QuickSplit is the first fully automated flow splitter for HPLC . It can split the column flow to deliver mi-croliter flow rates to an optical detector and nanoliter flows to an MS . Inlet and outlet flows are entered with a keypad . A four-line light-emitting diode (LED) display provides instantaneous status re-ports to the operator and to a PC for re-cording . The dynamic control keeps the split ratio constant during gradient elu-tion, where viscosity excursions can be large . Volume input ranges in mL/min are 1–5, 5–25, and 25–90 . Flow ranges of the side stream (in µL/min) are 0 .1–0 .5, 0 .5–2 .5, 2 .5–12 .5, and 12 .5–62 .5 . Key applications are expected to include proteomics and environmental, and even preparative chromatography, where a side stream is sent to the analyzer . ASI points out that the AS650 takes the guesswork out of flow splitting .

UHPLC moduleNow with UHPLC capable of giving sub-minute runs, high-throughput labs need to load and process more samples for overnight operation . To meet this need, Shimadzu Scientific Instruments (www .ssi .shimadzu .com) introduced the SIL-30ACMP multiplate autosampler as an add-on module for the Nexera MP UHPLC . The autosampler triples capacity to six 384-well plates . The specifications are impressive: Carryover is <0 .0015%; %CV is <1% for 0 .5-µL injections and <0 .2% for injection volumes greater than 5 µL . Mini-mum cycle time is 14 sec .

Chromatography simulation and method development softwareDryLab® 4 from Molnár-Institute (www .molnar-institut .com) is the latest exten-sion of the popular series of chromatog-raphy simulation and method develop-ment software . The new release extends DryLab into 3-D separations and also supports quality by quality-by-design (QbD) principles to LC method develop-



not approved sampling of other ana-lytes on dried blood spots . Without a guidance document, DBS sampling awaits approval, at least in the States, although this is not the case for some European companies . For example, CA-MAG Scientific Inc. (www .camag .com) introduced the DBS-MS 500 for sam-ple prep for MS . For DBS, the dried cards from Whatman (www .whatman .com) or ID Biological Systems (www . id-biological .com) are picked up with a new gripping tool and moved to the op-tical card recognition (OCR) module, which records the bar-code identifica-tion and spot position . The card then passes to the spotting station where the internal standard is applied . CAMAG was able to apply its decades of expe-rience with thin layer chromatography (TLC) spotting to give precise stan-dard addition . Next, the card travels to the extraction station, where it is pressed between the solvent inlet and exit ports . The card is removed and re-

ment . This can be extended to multifac-torial modeling needed to delineate the design space and ensure that the operat-ing space falls within it .

For method development using QbD, one must start with the best column . Using DryLab’s built-in Design of Experiment (DoE) module, the user selects the input parameters for optimization including mobile phase components, pH, tempera-ture, dwell volume, and run time . This will provide a list of experiments to run . After the results have been imported, Dry-Lab tracks the peaks and constructs a map of the response space in a heat map . This facilitates describing the design space . A local optimum is selected for validation experimentally . Usually the agreement between predicted and actual results is within 5% for retention time and critical pair resolution . Anecdotal reports show a reduction in method development valida-tion time by 50% . Plus, the heat map is useful in showing regulators that the assay is understood and under control . Another advantage is that method transfer between different instruments is predictable and hence easier .

Solvent gradient optimization systemIn the booth of Bischoff Chromatog-raphy (www .bischoff-chrom .de), I was introduced to a program that optimizes solvent gradients with the mixed-mode columns of Phase OPtimized LC, aka POPLC® . With POPLC, the stationary phase in the column is optimized for the sample by stacking cartridges filled with different stationary phases such as C18, C8, NH2, CN, etc . Previously, Bischoff offered software to assist in the optimi-zation of isocratic runs . Today, the com-pany has gradient elution optimization .

Sample prepDried blood spots sampling systemsDespite decades of experience with dried blood spot (DBS) sampling for phenylketonuria (PKU), the FDA has

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placed in the sample rack for archiving . One study showed that the %CV for 560 replicate DBS samples was 2 .8% with the CAMAG systems . Manual ex-traction had a %CV of 4 .57% .

Protein digestion platformDigesting proteins with enzymes is one of the common techniques in pro-teomics . Shimadzu has teamed with Perfinity Biosciences (www .perfinity .com) to design a new Perfinity Integrat-ed Digestion Platform (IDP) . This au-tomates the digestion work flow to re-duce time and improve reproducibility over manual protocols . These involve a three-day cycle time including an 18-hr digestion . With IDP, the cycle time is reduced to 30 min maximum . Perfinity explains this is accomplished through optimum automated integration of buf-fer exchange, digestion, desalting, and reversed-phase separation and simplifi-cation of the work flow .

44

LIQUID PHASE SEPARATION continued

large pore; Aeris Peptide has smaller pores and is suitable for peptides and small (<10 kDa) proteins. The other key consider-ation is the pressure rating of the instrument. One who has alegacy HPLC (i.e., Pmax

of about 6000 psi) should select columnspacked with 3.6-μm particles. One running UHPLC should takeadvantage of the 1.7-μm particles. These columns provide un-expectedly high column efficiency and resolution compared toeven porous columns with similar particle diameter. One coun-terintuitive point is that if the highest resolution is needed, then a long column can be constructed by connecting several col-umns packed with 3.6-μm particles. In HPLC, maximized peak capacity (peak count) is achieved with long columns packed withlarger-diameter particles. The tradeoff is much, much longerrun time.

Kinetex® phenyl–hexyl ligandsBonded to Phenomenex Kinetex® particles, phenyl–hexyl ligands(www.phenomenex.com/Products/HPLCDetail/Kinetex/Phenyl-Hexyl) are useful in separating moderately polar analytessuch as chlorophenols, steroids, phthalates, and geometric iso-mers. An animation of the phase showed a benzene ring con-

TLC/MS interfaceTLC is still popular in many organic synthesis labs. However,these labs also want to characterize the spots with MS. Until now, the best available technology involved scraping the spot from theTLC plate and eluting the material in a tube, then transferring the liquid into the MS, which is cumbersome by today’s standards. CAMAG introduced the TLC/MS interface for on-line transfer of compounds from TLC spots to APCI/MS, ESI/MS, or APPI/MS (atmospheric pressure photoionization-MS) interfaces. The spot islocated with cross-hairs. An arm lowers and presses the solvent in-let/outlet probe over the target spot. The solvent is metered in andpasses up the outlet directly to the MS. The on-line nature of theoperation gives a throughput of a spot per minute.

LC columnsAeris™ Core-Shell HPLC/UHPLC columnsAeris™ Core-Shell HPLC/UHPLC columns (www.phenomenex.com/Aeris/Index) from Phenomenex (www.phenomenex.com) are designed to provide rapid separation of proteins and pep-tides. They are offered in two pore sizes: Aeris Protein has the

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nected to the Kinetex core shell particle via an n-hexane tether . As with the Aeris Core-Shell, columns packed with 2 .6-µm parti-cles provide good separation efficiency for HPLC (~6000 psi) in-struments . Columns packed with 1 .7-µm particles are designed for UHPLC instruments . Users can expect outstanding speed and detection limits if their system can keep up .

SecurityGuard™ ULTRA guard columns for UHPLCSince particulates are more of a problem with narrow columns packed with very small particles, and the columns are also expen-sive, guard columns are especially recommended . These must also be designed to minimize extracolumn band broadening . Phenomenex extended the SecurityGuard™ product line to SecurityGuard ULTRA (www .phenomenex .com/Products/HPLCDetail/SecurityGuard%20ULTRA), which is specifically designed for UHPLC columns from any vendor (www .p h e n o m e n e x . c o m / P ro d u c t s / H P L C D e t a i l / K i n e t e x / Phenyl-Hexyl) . The columns are rated to 20,000 psi . They are small (<0 .3 µL) and not a significant source of extracolumn band broadening .

Ultra HPLC columnsRestek (www .restek .com) extended its Ultra HPLC column line with three new surface chemistries . The Ultra line is based on 3- or 5-µm spherical silica with 100-Å pore diameter . After the ligand is bonded, the particles are endcapped to remove the H-bonding effects of resid-ual silanols . Compared to conventional alkyl and phenyl phases, the biphenyl phase exhibits both increased retention and selectivity for aromatic and/or unsaturated compounds (www .restek .com/catalog/view/11086) . The pentafluorophenylpropyl (PFP) phase has a penta-fluorobenzyl group attached to the particle by a propyl tether . The PFP is particularly recommended for nitrogen heterocyclics and halo-genated analytes (www .restek .com/catalog/view/11087) . The Ultra Aromax column sports a proprietary surface chemistry that shows stronger retention of aromatic analytes than conventional C18 or even phenyl phases . It is particularly effective in separating steroids, tetracyclines, and drug metabolites, especially if they have some un-saturation (www .restek .com/catalog/view/32171) .

USLC™ columnsThe section describing DryLab’s QbD approach to method de-velopment and validation starts with selecting the best column . “Best” can include many attributes (availability, price, fitting compatibility, etc .), but selectivity for the analytes is prob-ably the most important . Restek introduced the USLC™ four- column set with diversity in selectivity to quickly scout for fa-vorable selectivity (www .restek .com/USLCarticle) . The phases include Ultra Aqueous C18 with an embedded polar group; Ultra IBD, also with an embedded polar group that improves separation of acids; Ultra PFP Propyl, which shows selectivity for bases; and Ultra Biphenyl, which demonstrates selectivity

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acetonitrile concentration is very high, where it shows general selectivity .

Ascentis Express ES-Cyano consists of diisopropyl-cyanopropylsilane bonded and endcapped to 2 .7-µm Halo particles . The CN provides a stable, reversed-phase packing suitable for basic, acidic, or neu-tral analytes (www .sigmaaldrich .com/analytical-chromatography/analytical-products .html?TablePage=108679944) .

Ascentis Express OH5 (Pentol) is a pro-prietary phase developed by Supelco that contains a polyol surface chemistry . This probably interacts with analytes with potential hydrogen bonding func-tional groups .

Fortis HILIC column for assay of polar analytesThe sub-2-µm market offering is expand-ing as more vendors add new station-ary phases . Fortis HILIC from Fortis™ Technologies (www .fortis-technologies .com) is now available in columns packed with 1 .7-µm particles . These are opti-mized for the assay of polar analytes with HILIC conditions . The silanol content is controlled to attract a water-rich layer on the beads . This produces retention of polar analytes that are typi-cally not retained on more hydrophobic stationary phases .

Deamidation with RPLC and ERLICDeamidation of asparagine and gluta-mine residues in proteins occurs natu-rally . In vivo deamidation is believed to play a role in cataracts and Alzheimer’s disease . It can also be promoted by the conditions of bioprocessing, storage, and proteomics digestion . Deamida-tion reduces the shelf-life of protein therapeutics . In addition to naturally occurring deamidation, deamidation sites are used in proteomics as markers for sites of N-glycosylation . Thus there is a need for an assay to differentiate between native and ex vivo or artifac-tual deamidation .

for aromatics . These all offer diverse se-lectivity patterns compared to Ultra C18, which is used as a benchmark . It is selec-tive for hydrophobic analytes .

Hydrophilic interaction chromatography (HILIC) columns COSMOSIL Triazole phaseNacalai USA, Inc. (www .nacalaiusa .com) introduced the COSMOSIL Triazole sta-tionary phase for HILIC . It demonstrates useful selectivity for anionic analytes such as oxamic acid and oxalic acid . In anoth-er example, the separation of ascorbic acid and isoascorbic acid on the triazole column was run under ion exchange con-ditions (dilute salt), and a partial separa-tion (R = 0 .7) was obtained . If the salt concentration increases to 100 mm, even this poor separation is lost entirely . How-ever, under HILIC conditions, achieved by increasing the acetonitrile to 80%, the R improves to over 4 .

Epic HILIC-PI phaseES Industries (www .esind .com) intro-duced the Epic HILIC-PI phase for the separation of polar amines . The aro-matic character of the stationary phase provides selective retention based upon π–π interactions . The stationary phase is a proprietary ligand bonded to 1 .8-µm porous silica . This provides excellent column efficiency and speed . The new phase offers unusual but stable selectiv-ity, which provides robust methods .

Ascentis® ExpressSupelco (www .sigmaaldrich .com) intro-duced three surface chemistries to the Ascentis® line of Fused-Core columns for HILIC (www .sigmaaldrich .com/analytical-chromatography/analytical-products .html?TablePage=104698603) . For Ascen-tis Express F5, a PFP group is bonded to 2 .7-µm Halo particles via a propyl tether . The PFP phase can function as a reversed-phase packing with π–π selectivity . It also functions in the HILIC mode when the

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Dr . Andrew Alpert, President and Founder of PolyLC Inc. (www .polylc .com), explained that deamidation of asparagine occurs when the amide side chain of asparagine attacks the adjacent resi-due on the C-terminal side, forming an asymmetric succinimide intermediate . The ring opens to form aspartic acid or isoaspartic acid in a 1:2 ratio . The presence and ratio of the latter two are markers of deamidation . All three isoforms can be separated by electrostatic repulsion-hydrophilic interaction chromatography (ERLIC) (PolyLC) and identified on-line by mass spectrometry . One study showed that much deamidation was artifactual and could be identified incorrectly as glycosylation sites . Dr . Alpert went on to propose an improved digestion protocol that suppress-es the artifactual deamidation .

Ion exchange columnsIonPac columns for ICS-4000/5000To take advantage of the extended pressure and flow rate capability of the new ICS-4000 and upgraded 5000, Di-onex introduced new columns packed with 4-µm-diam particles packed into 0 .4-mm-i .d . tubes . Prior columns uti-lized 5 .5- or 9-µm-diam particles . The new columns are much more efficient, and since they are also narrower, they have greater detection sensitivity for the same sample load . The IonPac AS18-4µm anion exchange column is the hydroxide-selective column of choice for compliance monitoring of inorganic anions in drinking water and wastewater samples in accordance with U .S . EPA Methods 300 .0(A) and 300 .1 . However, the cycle time is re-duced to 3 min . Other applications run on the IonPac AS18-Fast column can be easily transferred to the Ion-Pac AS18-4µm column with the ben-efit of reduced run time with no loss in resolution . The IonPac AS18-4µm column is available in capillary for-mat, 0 .4 × 150 mm (www .dionex .com/en-us/products/columns/ic -r f ic/ hydroxide-selective-packed/ionpac-as18-4um/lp-111535 .html) .

Similarly, the AS11-HC-4µm column and the CS19-4µm capillaries are also packed with 4-µm particles in capil-lary format . The improved efficiency obtained with smaller particles allows use of 2–3 times higher f low rate with

constant resolution, but reducing run time by the reciprocal factor . When operating at the standard flow rate of 0 .010 mL/min, an IC system capable of operating up to 3000 psi is suffi-cient . However, to take advantage of the fast runs, using a f low rate of 0 .030 mL/min, a high-pressure capillary IC system such as the ICS-5000 or ICS-4000 is required .

MAbPac™ SCX-10 columnsScreening monoclonal antibodies just got faster by reducing the diameter of the column particle to 3 or 5 µm diam from 10 µm . MAbPac™ SCX-10 columns from Dionex are effective for

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5-µm silica that was useful for a variety of common products, including formulations . This year, Thermo Fisher Scientific introduced an improved version called the Acclaim Surfactant Plus . The stationary phase is a mixed-mode surface chemistry with improved bonding to 3- or 5- µm-spherical silica . Com-pared to its predecessor, the new columns maintain the same selectivity with low column bleed, improved stability, and shorter analysis time .

LC column packingsA decade ago, I visited China several times . The entrepreneur-ial column vendors all struggled with the expense of procuring quality silica for HPLC columns . They had to import the column packings from Western sources . They quickly mastered bond-ing and especially packing . I wondered how long it would take for a firm to start producing chromatographic silica in China . Nanomicro Technology Co. had a booth that featured a wide range of column packings, including UniSil™ spherical silica with a nominal diameter of 2, 3, 4, 5…50 µm) . Six pore diam-eters are available from 50 to 500 Å . Nanomicro also makes bonded phases including C18, C8, C4, NH2, and HILIC .

separating antibody variants differing by only one charge . Unique surface chemistry nearly eliminates nonspecific hydro-phobic interaction, giving sharp peaks . The columns are suit-able for platform assays for identification and stability assays . A range of column diameters and lengths are offered .

Scherzo SW-C18 columnAdenosine mono-, di-, and tri-phosphates are very polar anions with broad interest due to their involvement in biological energy processes . While separation by RPLC is not successful, Imtakt USA (www .imtaktusa .com) finds that a mixed-mode anion ex-change/C18 column is quite effective . Run times are less than 10 min with gradient elution .

Acclaim™ Surfactant Plus columnsSurfactant by HPLC seems to be a natural idea until one tries it by RPLC and the frustration starts . C18 can irreversibly sorb some surfactants such as sodium dodecyl sulfate . This was the basis of “soap chromatography mode” in the early 1980s . A few years ago, Dionex introduced the Acclaim™ Surfactant columns, which had a proprietary surface chemistry on 3- or

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Nanomicro UniPS™ beads are made of polystyrene/divinylbenzene copolymer . Particle diameters start at 2 µm and ex-tend to 60 µm . Photomicrographs sup-port the claim of monodisperse particle distribution . The company also offers polyacrylic particles in three size cuts from 20 to 60 µm . A huge selection of pore diameters is available, including nonporous . Ionogens have been added to the polymeric beads to make the cor-responding ion exchange resins with the trade name Uni-IEC .

Solid-phase extraction phasesSiliaPrepX™SiliCycle (www .silicycle .com) is known for producing a wide range of prod-ucts, sorbents, scavengers, and catalyst supports, based on silica . Thus, I was surprised with the introduction of the SiliaPrepX™ line of polymer-filled tubes for solid-phase extraction (SPE) . A range of stationary phase chemistries is offered, including cation and anion exchange and two neutral sorbents . The polystyrene/divinylbenzene phase re-tains nonpolar analytes . The HLB phase presents a wettable copolymer with a balanced hydrophilic and hydrophobic surface that retains acids, bases, and neutrals . The columns are available in plastic tubes with volumes of 1, 3, to 6 mL and 96-well plates .

Fritless SOLA SPE cartridgesEarly cartridges and multitip plates for SPE used screens or frits to hold the sor-bent in place . While the frits were usu-ally selected to be inert under anticipated use conditions, they were often suspected when the mass balance was short . Chro-matographers at Thermo Fisher Scientif-ic worked to blend the frit with the plas-tic of the tube wall (polyethylene) and column packing . The result is the SOLA series of cartridges and plates . Separation modes include reversed phase, cation, and anion exchange in 1- or 2-mL tubes (www .thermoscientific .com/ecomm/

ser vlet/newsdetai l ?storeId=11152& contentId=54068&ca=sola-spe) .

LC fittingsEXP® fittings from Optimize Tech-nologies (www .optimizetech .com) and column hardware allow indefinite make-and-break cycles of fingertight connections rated to 20,000 psi . This year, the line was expanded to include very low-dead-volume stem filters, pre-column filters, trap columns, and packed-bed guard columns . Plus, some fittings are available for 1/32-in . tubing, which is widely used in small-bore capil-lary applications .

However, the item that really caught my eye was a spring-loaded auto-adjust-ing zero-dead-volume connection . The bleeding edge of current column tech-nology produces peaks with a volume

of 1–3 µL . With conventional designs, the position of the fixed ferrule can vary due to design variances, machining tolerances, and creep . Creep is ferrule movement as the tubing starts to pull out . It is difficult to detect . Whatever the source, the hidden dead volume is 2 µL per mm of mispositioning . One mil-limeter could contribute significantly to extracolumn band broadening . With the Optimize zero-dead-volume connec-tion, one pushes the tubing into the fit-ting until it bottoms out, then the nut is tightened by hand . Now you have made a zero-dead-volume connection rated to 20,000 psi . And, it took you longer to read it here than to do it, at least the sec-ond time (www .news-medical .net/news/ 20120312/Thermo-Fisher-Scientif ic -launches-Acclaim-Surfactant-Plus-and-MA bPac - SCX -10 - ch roma tog r aphy - columns .aspx?page=2) .

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valves use patent-pending metal-on-metal seal technology, which enables ultrahigh-pressure injection, selection, and switching . This sealing technology doubles the expected life-time compared to the older valves that were rated to only 15,000 psi .

Analytical standardsIn some respects, clinical diagnostics is a leading market model for analytical chemistry . Clinical labs run assays on dedicated, purpose-built analyzers . Vendors supply all reagents, standards, training, software, and postsales support, usually globally .

Clinical LC/MS is the fastest-growing market segment of chro-matography today . Vendors of traditional MS instruments

(Waters and Thermo Fisher Scientific in par-ticular) recognized the need to develop a new business model to be compatible with the established practices of diagnostics labs . Sur-prisingly, Waters discovered significant inter-est from its traditional base in pharma . These labs do not want to spend time preparing reagents, etc . Plus, assured supply and trace-able certificates of analysis were also valuable . With global R&D programs and outsourcing, the availability of common reagents and stan-dards to all laboratories is particularly desir-able since it should improve comparability and facilitate method transfer .

Pittcon 2013Next year, Pittcon moves to Philadelphia, PA, a new location for the meeting, and one that will be attractive since so many chemical and pharmaceutical companies are located within driving distance of the convention center . The dates are March 17–21, 2013 .

New gas chromatography instruments and columns are reviewed on page 12 . A review of supercritical fluid chromatography systems appears on page 28 .

Robert L. Stevenson, Ph.D., is a Consultant and Editor

of Separation Science for American Laboratory/Lab-

compare; e-mail: [email protected].

Check valvesDecades ago, I worked on exploring the pressure limits of HPLC . We found that stainless steel was not suitable at pressures at about 30,000 psi and higher . We decided to back off to a P

max of 8500 psi

to have a very large safety margin . This year IDEX (www .idexcorp .com) introduced check valves rated to 30,000 psi . The key is to use a different alloy that can take the pressure . The company also in-troduced a complete range of fittings for 1/16- and 1/32-in . tubing rated up to 30,000 psi . However, the lifetime measured in make-and-break cycles reduces to 5 as the pressure increases to 30,000 psi . Tightening fittings with a torque wrench is recommended .

TitanHT™ multiport valvesIDEX introduced three new valves with 6, 7, and 10 ports for next-generation UHPLC applications . Rheodyne TitanHT™

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Benchtop Basics: Tips for Buying pH Meters and Balancesby Caitlin Smith

Most laboratories would grind to a halt without the funda-mental measurements pro-vided by electrochemistry

and weighing instruments . Basic equip-ment like pH meters and conductivity meters are based on, or are closely related to, the heart of electrochemistry—when charged particles, such as ions or electrons, traverse an interface between two phases of matter . This interface is usually a metal (such as an electrode) and a conductive solution or electrolyte . Researchers now have many options among which to choose electrochemistry equipment . This article aims to help introduce the types of electro-chemistry tools available today . (See Box for tips on choosing an analytical balance .)

pH metersA pH meter is an irreplaceable piece of equipment for measuring the acidity or alkalinity of a solution (or a semisolid) . Usually a measuring electrode and a refer-ence electrode are connected by a meter for comparison . The hydrogen ion-sensitive measuring electrode measures a small volt-age that changes depending on the concen-tration of hydrogen ions in solution . The pH meter then displays the measurement in pH units (and in some cases, also in mV or conductivity) . Because the pH reading is sensitive to temperature, some pH meters offer a temperature compensation feature (automatic or manual) that can correct this potential source of variation .

Benchtop pH meter optionsAnother variable feature of pH meters is the measurement range . For example, the SevenEasy™ S20 pH Meter from Mettler-Toledo (Columbus, OH) has a pH range of 0 .00–14 .00 . The HI 4521 pH/Conductivity (USP) Bench Meter from

Hanna Instruments (Smithfield, RI) has a pH range from –2 .000 to 20 .000 pH (as do other Mettler-Toledo models) . Many mod-els of benchtop pH meters are available, including those offered by Hanna Instru-ments, Mettler-Toledo, Denville Scien-tific (Metuchen, NJ), Sartorius Group (Goettingen, Germany), and OMEGA Engineering (Stamford, CT) .

Handheld pH meter rangeWhile many researchers use a bench-top pH meter, others can benefit from a handheld or portable model . Since some may use them outdoors, portable models also come in sturdy, weather- resistant designs, such as the HI 9026 Rugged Waterproof pH Meter from Hanna Instruments . Other vendors of portable pH meters include Mettler-Toledo, Sartorius Group, and OMEGA Engineering . As with any portable elec-tronic laboratory instrument, it is a good idea to know in advance how long the bat-tery will last (especially if out in the field), and the method of data transfer from the instrument to the laboratory computer .

Conductivity metersLike pH meters, conductivity meters serve a fundamental purpose in many laboratories . The main function of con-ductivity meters is to measure the electri-cal conductivity of aqueous solutions (in units of mS/cm), but they can also mea-sure other quantities, such as the amount of total dissolved solid (TDS), the pH, the percentage of sodium chloride in solution, resistance, and temperature . Conductivity is also temperature-depen-dent; thus most meters offer some type of temperature compensation, whether automatic or manual . Besides giving various types of readouts, conductivity meters also vary in their ranges of mea-

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sured conductivity . For example, the EC 215R Multi-range Conductivity Meter with Automatic Temperature Compensa-tion and Analog Output (Hanna Instru-ments) has a range of 0 .0–199 .9 mS/cm, while the SevenMulti S70 Luxury Con-ductivity Meter (Mettler-Toledo) has a range of 0 .001–1000 mS/cm .

Benchtop conductivity meter and portable conductivity meter choicesBenchtop conductivity meters can be obtained from many vendors, including some who also make pH meters, such as Hanna Instruments, Mettler-Toledo, Sartorius Group, OMEGA Engineering, Metrohm USA (Riverview, FL), and Taylor Scientific (St . Louis, MO) . Simi-lar to pH meters, conductivity meters also come in portable or handheld mod-els and include all the extra features of their benchtop cousins . They also fea-ture a range of measurement capabili-ties: Portable Conductivity Meters from Sartorius measure 0 .0–199 .0 mS/cm, and the HI 98188 Waterproof Portable EC/Resistivity/TDS/NaCl and Temper-ature Meter from Hanna Instruments measures 0–1000 mS/cm . As mentioned above, for portable pH meters, it is impor-tant for the user to learn about expected battery lifetimes, and the means of data transfer from the conductivity meter to the lab computer . Portable units can be found from Hanna Instruments, Mettler-Toledo, Sartorius Group, OMEGA Engi-neering, and PID Analyzers (Pembroke, MA), among others .

ConclusionElectrochemistry equipment such as pH meters, conductivity meters, and balances provide essential, everyday measurements


ELECTROCHEMISTRy PRODUCTS continued

Analytical BalancesFew laboratories could function without the basic benchtop analytical balance for weigh-ing chemical compounds, or any small lab item . Researchers can find balances with dif-ferent ranges of measurements; therefore it is a good idea to consider not only what needs to be weighed now, but also potential future uses . Most models can read from 0 .01 or 0 .1 mg up to tens or hundreds of grams . The cost and accuracy of a balance are strongly influenced by the quality of its weighing sensor, which is inside the instru-ment and translates the item’s weight into a num-ber . The better the weighing sensor, the faster and more reproducible the balance will be . It will also provide better protection from thermal fluctuations in measurements .

Because balances come in several varieties, it is beneficial for the user to envision potential applications before purchase . The ubiquitous benchtop analytical balance features different calibration options: manual or automatic (and, in some cases, programmable) and external or motor-driven . If a balance will be situated in a particularly dusty environment, the user should consider one that has been rated for ingress protection (IP); higher IP ratings indicate better resistance to solid and liquid contamination . Other enclosures need to be considered if bio-hazardous materials will be used .

It is also important to consider the weighing range that will be most needed, since mod-els differ . For example, Precision Analytical Balances from Denville Scientific feature a capacity of 120–250 g, and Excellence Plus XP Analytical Balances from Mettler-Toledo have capacities of 120, 220, or 520 g . Many companies offer analytical balances, includ-ing Sartorius Group, Denville Scientific, Mettler-Toledo, Taylor Scientific, MIDSCI (St . Louis, MO), OHAUS (Parsippany, NJ), Scientech (Boulder, CO), Shimadzu (Columbia, MD), Tovatech (South Orange, NJ), A&D Weighing (San Jose, CA), Adam Equipment (Danbury, CT), BioMedical Solutions (Stafford, TX), Rice Lake Weigh-ing Systems (Rice Lake, WI), and Spectrum Chemical (New Brunswick, NJ) .

Portable balance optionsResearchers working in the field (or lab mem-bers whose experiments demand extra mobil-ity) may prefer a portable analytical balance . Compared to other balances, a unique feature of portable units is their ruggedness for travel . They can offer many of the same features (per-haps sacrificing some degree of precision) as benchtop models, but with more durability . Portable balance vendors include Denville Sci-entific, Mettler-Toledo, OHAUS, Shimadzu,

Adam Equipment, Rice Lake Weighing Sys-tems, Spectrum Chemical, and Terra Univer-sal (Fullerton, CA) .

Top-loading balance alternativesThose who do not need the higher accuracy and protection afforded by an analytical bal-ance may choose a top-loading balance . Gen-erally used for weighing larger amounts (i .e ., with a 0 .05-g margin of error), a top-loading balance is easy to use . However, top-loading balances provide no protection from drafts, dust, or other environmental contaminants . They do vary in their weighing capacities, though, and because of this researchers need to know what they will be used for . For example, the OHAUS Explorer Pro Preci-sion Balance has a capacity of 210–32,000 g, while the Denville Scientific Precision Top Loading Laboratory Balance has a capacity of 150–4500 g . Top-loading balances are available from many companies, including Denville Scientific, Mettler-Toledo, MID-SCI, OHAUS, Sartorius Group, Scientech, Shimadzu, Terra Universal, Tovatech, A&D Weighing, Adam Equipment, Rice Lake Weighing Systems, Spectrum Chemical, and Taylor Scientific .

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that researchers could not function with-out . Hopefully the considerations dis-cussed here will help users find the right instrument to fit their needs .

For other manufacturers and distributors, please visit www.labcompare.com

Caitlin Smith is a freelance science writer who has a Ph.D. in Neuroscience from Yale University and postdoctoral work in Electrophysiology and Synaptic Plasticity; e-mail: [email protected].

Mass Spectrometers for Use in Clinical Diagnosticsby T. Keith Brock

The relative strengths and weak-nesses associated with different mass spectrometer configura-tions can make selecting the

right instrument a challenging endeavor for a prospective buyer . This article will discuss the basic components of mass spectrometers, integral specifications, and key considerations necessary for selecting the right mass spectrometer to suit the buyer’s clinical needs .

Mass spectrometers: Background and featuresMass spectrometry measures the mass-to-charge ratio (m/z) of an ion . The mass-to-charge ratio is useful in identifying com-pounds because the molecular or atomic weight of each molecule or atom is unique and intrinsic to the sample introduced . The signal measured by the mass spectrometer is the ion current, or the flow of ions filtered by mass, received by the ion counting or A-to-D conversion detection element .1

quantitative mass spectrometryIon currents measured by the mass spectrom-eter can be made proportional to the amount of sample introduced to the instrument . Thus, quantitative measurement is made possible . In a clinical application, quantita-tive mass spectrometry strategies are central to identifying biomarkers indicative of dis-ease . Typically, quantification is achieved by measuring the ion current response of an internal standard relative to that of the test sample . Whether the mass spectrometer analysis requires quantitative or qualitative measurement, every sample analyzed should contain a known amount of internal stan-dard to be used as a reference for determin-ing the sensitivity of the assay .

Ionization techniquesRegardless of the vendor or type, all mass spectrometers share the same set of pro-cesses . The test sample must be converted to an ionized gas . Depending on the native state of the sample, different ioniza-tion techniques can be used . Samples in gas or liquid phase can be ionized by gas chromatography or liquid chromatography, respectively . Samples introduced in a solid state can be converted to ionized gas using matrix-assisted laser desorption ionization (MALDI) . MALDI uses a coherent laser to excite, vaporize, and ionize the solid-phase sample from a crystalline matrix . The effi-ciency requirements, number, distribution, and type of ion created will vary depending on the ionization method (Table 1) .

The analyte of interest and internal stan-dard should ideally be equally influenced by ion source events and the ratio of their ion currents unchanged . For this reason, the physicochemical properties of the target analyte and internal standard should be as close as possible . Naturally, the ideal choice for internal standard is a stable, isotype-labeled form of the compound of interest, with a distinguishable mass, also known as an isotopomer .

Mass analysisOnce the sample has been converted to gas-phase ions, including those indicative of the target analyte and those not of interest, they travel to the mass analyzer . Here, different ions are separated based on their mass-to-charge ratio . There is significant variation in the separation mechanism of ions (Table 1b), the details and capabilities of which cannot be fully explored within the scope of this arti-cle . The operational parameters of mass spec-trometry are conserved, such as mass scale calibration, resolution, limit of detection, limit of quantification, analytical range, pre-

cision, and ease of optimization . Important mass spectrometer specifications are given in the Mass Spectrometer Features Checklist .

Signal detection and analysisOnce filtered by the mass analyzer, ions bom-bard the ion counting or A-to-D conversion detection element . The detector gives an elec-tronic response proportional to the number of targeted ions present . This electronic sig-nal is then interpreted by a computer with bioinformatic software, which controls vari-ous instrument parameters and processes the data .

Key purchasing considerations: Defining requirementsThroughputThere are many factors that play into the number of tests that can be performed in a given time period, making overall mass spec-trometry throughput difficult to quantify . “Throughput encompasses several system performance factors, analytical speed, system sensitivity, system robustness, tune stability and overall reliability,” explained Meredith Conoley, GC & GC-MS Marketing Director at Bruker Chemical and Applied Markets Division (Fremont, CA) . “Placing too much emphasis on any one criterion, such as speed, can lead to a choice that does not deliver in another key area such as robustness . Any per-formance gains due to speed can be lost due to time spent with frequent maintenance (cleaning) or re-tuning . This results in loss of overall sample throughput .”

Sensitivity and selectivityThe sensitivity of a mass spectrometer is defined as the change in response of the measuring system divided by the corre-sponding change in stimulus . The selec-tivity of the instrument is defined as the ability to accurately measure the target ana-lyte in the presence of interferences .1 “Sen-sitivity is a very important parameter for clinical assays,” continued Conoley . “The complexity of the sample matrix requires an equal evaluation of system performance based on selectivity . Sample complex-ity and required detection limits can be the determining factors on whether one

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MASS SPECTROMETERS continued

chooses a GC-MS single quadrupole sys-tem or GC-MS triple quadrupole [TQ] . While GC-MS TQ may be a more expen-sive investment, the inherent increase in selectivity provided by MRM [mul-tiple reaction monitoring] capability of the triple quad can increase the ability to detect target analytes to the sub-ppb range in the complex sample matrix in clinical applications . Selectivity is as important a factor in system perfor-mance as sensitivity for the detection of analytes in complex matrices .”

Precision and accuracyPrecision and accuracy vary between mass spectrometer technologies and vendors . Measurement precisions of 1% can be achieved using quadrupole mass spectrometers, while precisions of better than 0 .1 ppm will require high- resolution instruments .

“One of the major challenges is that dif-ferent workflows create different kinds of

information, making reproducibility and standardization a key to confidence in generated results,” Conoley said . “Stan-dardized analysis methods and validation techniques in SOPs significantly assist in comparability of results .”

Data processing softwareMass spectrometer software controls the hardware, methods of analysis, data analysis, and result storage . “All systems will process the data they acquire but not all systems are designed with the workflow of the laboratory in mind,” Conoley pointed out . “Does it sup-port critical compliance requirements; does it support connection to my LIMS? These are key issues to investigate beyond the basics of data processing .”

Other considerations to take into account prior to purchasing a mass spectrometer are size, ease of use, instrument versatility, and quantitative (diagnostic) versus qualitative (screening) analysis needs .

ValidationOnce the buyer’s needs are well under-stood, the stakeholder should clearly define the target analytes and develop or obtain a test compound . Based on the target ana-lytes and the defined requirements, the pur-chaser should identify a mass spectrometer and the necessary components . It is criti-cal to match compatible ionization modes, resolution required, and the ionization method . Using the test compound, a dem-onstration session with vendors of interest should take place at which the vendor tests key metabolites and evaluate sensitivity, precision, ease of optimization, and data processing software . Ideally, this demonstra-tion should be paired with a parallel analy-sis using a validated method . Additionally, interinstrument comparisons should be per-formed on identical samples under identical conditions . The evaluation should be on site if possible . Lastly, instrument software, data processing, and result interpretation should be thoroughly demonstrated and explained by the vendor .

Table 1 Ionization and mass separation methodologies


Important price pointsConoley suggested that buyers not be swayed by the initial cost of the instrument . “Eval-

uate in terms of what additional technical capabilities it may bring to the workflow in terms of cost per sample, increased produc-tivity, etc .,” he said . “In terms of GC-MS, investing in a more expensive GC-MS TQ system may actually allow an overall reduc-tion in cost per sample due to reduced sam-ple prep costs, reduced sample collection costs, etc ., due to the improved quantifica-tion capability of MRM over SIM [secondary ion mass] or full scan in a GC-MS SQ [single quadrupole] .” References from laboratories that own the current model can also be help-ful when trying to understand the workload impact, reliability, and ease of use of an instrument already in use .

ConclusionWhen purchasing a mass spectrometer, cer-tain regulatory issues (i .e ., certifications and procedures) may drive selection of devices used in the clinical environment . “Users must be aware of these requirements and ensure the equipment they are purchasing has met these requirements,” Conoley said . It is also important to consider the reputa-tion of the vendor itself . Conoley points out that non-product issues must be evaluated in addition to technical needs . These include the industry knowledge and depth of experi-ence of the company .

Reference1 . Mass Spectrometry in the Clinical Laboratory:

General Principles and Guidance; Approved Guideline . CLSI document C50-A; Wayne, PA: Clinical and Laboratory Standards Insti-tute, 2007 .

T. Keith Brock, BS, is a Contributing Writer, American Laboratory/Labcompare; e-mail: [email protected]. The author would like to thank Meredith Conoley, GC & GC-MS Marketing Director, Bruker Chemical & Applied Markets Division (Fremont, CA), for his contributions to this article.

Mass Spectrometer Manufacturers

• AgilentTechnologies

• ALMSCOInternational

• Bruker

• LECO

• Shimadzu

• ThermoScientific

• HitachiHighTechnologies America, Inc .

For other manufacturers and distributors, please visit www.labcompare.com

Mass Spectrometer FeaturesChecklist

Cost

Ease of interpretation of results

Ease of use

Footprint

Ionization method

Mass accuracy

Mass analyzer

Mass range

Quantification

Reliability/ruggedness/customer service

Resolution

Scanning speed

Sensitivity

Temperature range

Throughput

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Industry News and Events Available on theALamericanlaboratory.com/ipad

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Becoming part of Abbott in 2010 has given STARLIMS, a lead-ing global LIMS provider, new resources for business expansion, customer service, new product development, and international expansion . STARLIMS acquired several long-time distribution partners: Varilab in France, two privately held businesses in Spain operating as STARLIMS Iberia, a private Dutch company operat-ing as STARLIMS Netherlands with a branch in Sweden, and its distribution partner in Israel called STARLIMS Israel, Ltd. www .starlims .com

Brookfield Engineering Laboratories has announced the pro-motion of Chris Freeman to the position of Senior Product

Manager, CT3 Texture Analyzers, a general-purpose instrument used in compression and tension testing of solid and soft-solid substances . For additional information on the CT3, visit www .brookfieldengineering .com/products/texture-analysis/ct3 .asp .

Corning Inc. has reached a definitive agreement with BD (Becton, Dickinson and Company) to acquire the majority of its Discovery Labware unit . When complete, the acquisition will augment Corn-ing’s global market access and enhance its broad portfolio of life sciences products in the areas of drug discovery tools, bioprocess solutions, and laboratory research instruments . www .corning .com .


A new recorded presentation from Malvern Instruments, which can be downloaded on-demand at http://bit .ly/MALTTVS, compares the use of Dilute Solution Viscometry (DSV) with that of traditional glassware for measuring polymer intrinsic viscos-ity . The presentation describes use of the company’s Viscotek DSV solution . Malvern Instruments is a market leader in measuring performance controlling material properties . www .malvern .com

The Sartorius technology group formally opened a new manufacturing building at its headquarters in Goettin-gen, Germany, for the production of membranes . The building offers ample room to accommodate the new plant machinery for manufacturing poly-ethersulfone membranes as well as laborato-riesand offices for more than 120 employees . www .sartorius .com

Shimadzu Scientific Instruments has announced the grand opening of the Shimadzu Center for Advanced Analytical Chemistry at The University of Texas at Arlington . Located in the university’s Chemistry & Physics Building, the center contains

$6 million of chromatography, mass spectrometry, and spectros-copy equipment, which is the largest installation of Shimadzu ana-lytical instrumentation in the Western Hemisphere . Visit www .ssi .shimadzu .com for more information .

The U .S . EPA’s Administrator recently signed a Method Update Rule (MUR) approving new methods for analysis of NPDES waste-water samples . This permits laboratories to analyze samples for total cyanide without a preliminary 2-hr acid distillation step . OI Analytical’s CNSolution 3100 Cyanide Analyzer uses in-line UV digestion to dissociate metal-cyanide complexes and measure total cyanide in minutes by ASTM D 7511-09e2 . www .oico .com

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Technology Corp . . . . . . . . . . . . . . . . . . . . . . . . . . .28 A-D . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .www .MTC-USA .comMilestone Inc . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26 . . . . . . . . . . . . . . . . . . . . . . . . . . .milestonesci .com/ultrawaveNasco . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . www .whirl-pak .comNuAire, Inc . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .www .nuaire .comOI Analytical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .www .oico .comOmega Engineering Inc . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .www .omega .comOMNI International, Inc . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22,23 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .www .omni-inc .comPeak Scientific . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . www .peakscientific .comPhotonis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .www .photonis 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