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 5

www.americanlaboratory.com
Pittcon
2012: Laboratory Instrumentation and Equipment

Product Showcase
by J. Hunt...........................................................................................pg 20
The wide variety of lab equipment and instrumentation featured at Pittcon is
showcased in this review.
Conference Review
Focus on Separation Science at Pittcon
2012: Advances in
Gas Chromatography
by R.L. Stevenson................................................................................pg 12
This comprehensive review of separation science products introduced at Pittcon
2012 includes a number of GC systems and columns.
Conference Review
New Developments in Supercritical Fluid Chromatography (SFC) at
Pittcon
2012: 20/20 Vision?

by R.L. Stevenson............................................................................pg 28
Novel 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
Pittcon
2012 Roundup of Spectroscopy and Mass Spectrometry

by J. Perkel........................................................................................pg 30
This review presents new product launches in spectroscopy and
mass spectrometry.
Conference Review
What Is This?
This months 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
Advances in Liquid Phase Separation at Pittcon
2012
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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by B. Foster..................................................................................pg 6
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Editors Page
M
icro 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 chasm
Historically, atomic force microscopy (AFM)
has been the gateway for Raman microscopy,
but the emphasis at Pittcon was on the optical
Major manufacturersfrom micro Raman in-
dustry leaders Renishaw (wwwrenishawcom)
and Horiba (wwwhoribacom) to Bruker
Optics (wwwbrukeropticscom), Jasco (www
jascoinccom), Kaiser Optical Systems (www
kosicom), and Thermo Fisher Scientific (www
thermofishercom)all featured fully inte-
grated systems, typically centered on Olym-
pus BX research-level microscopes (www
olympusamericacom) (WITec [wwwwitec
de] and CRAIC Technologies [wwwmicro-
spectracom], 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
2012
by Barbara Foster
In Figure 2, for example, a rubys 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
perspectivesin 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 user
Micro Raman is not just for the research
lab, however B&W Tek (wwwbwtekcom)
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 (wwwenwaveoptcom) takes a simi-
lar approach with the Sense line, which
uses fiber optics and video to connect Ra-
man to laboratory-based stands
Figure 1 - Nanodiamond in polymer matrix: a) 1 m 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 (wwwbayspeccom) 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
intevaccom), uses a free-space design to cre-
ate a unique modular system that mounts
atop virtually any microscope The system
comes in two wavelength variations532
nm and 785 nmand 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 students
BioTools (wwwbtoolscom) 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 adjunct
Horibas 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
EDITORS 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 (wwwanasysinstrumentscom), 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 Renishaws new StreamLineHR.
Figure 3 - B&W TEKs 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.
April 1720, Munich
Hall A3, Booth 233/332
Revolutionize your pipetting.
New Picus electronic pipette.
The smallest, the lightest, the most precise.
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 throughput
Renishaw debuted the RA800 series, a
new automated platform for health care,
developed with partner Renishaw Diag-
nostics (wwwrenishawdiagnosticscom)
in Glasgow, Scotland One variant is al-
ready in use with Renishaw Diagnostics
Ltd. (RDL), where it forms part of RDLs
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 25 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
Renishaws 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 (wwwrtabiz), which targets the high-
throughput arena with its SERS 96-well
plates, capillaries, and vials
EDITORS PAGE continued
Summary
From 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
Reference
1 Tuschel, D Molecular spectroscopy work-
bench: Raman crystallography in theory
and in practice Spectroscopy Mar 2012,
27(3); wwwspectroscopyonlinecom
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: bfoster@
the-mip.com; 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 Shimadzus
most advanced gas chromatograph mass spectrometer.
Descended from the GCMS-QP2010 Plus, it features
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Improved data collection speed makes this the perfect
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ecology mode saves power and carrier gas consumption
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The GCMS-QP2010 Ultra
features:
Maximum scan speed of 20,000 u/sec
achieved with patented technology
500:1 S/N in EI mode
Rapid GC oven cool-down from 350 to 50
in 2.7 minutes
Twin-Line MS Systemeliminates the need
to swap columns
Ecology mode significantly reduces
operating costs
With the GCMS-QP2010 Ultra, Shimadzu offers a new
solution for increased productivity, reduced running
costs and less environmental impact. The GCMS-
QP2010 Ultra is without question the best single
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Order consumables and accessories on-line at http://store.shimadzu.com
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Learn more about Shimadzus GCMS-QP2010 Ultra.
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Shimadzus GCMS-QP2010 Ultra: The Ultimate in GCMS Performance
Ultra Fast, Ultra Sensitive
F
or gas chromatography (GC), the
big news at Pittcon
2012 was
the absence of Agilent (www
agilentcom) and PerkinElmer
(wwwperkinelmercom) 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 worlds largest meeting
in separation science Slowly at first, the
focus shifted: At Pittcon 2012, spectros-
copy clearly dominated the exhibition
New gas chromatographs
SCION GC/MS systems
Bruker (wwwbdalcom) 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 didnt
take long The new SCION SQ (single
quadrupole) and TQ (triple quadrupole)
GC/MS systemswhich won the Pittcon
Editors Silver Awardutilize 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
Focus on Separation Science at Pittcon
2012:
Advances in Gas Chromatography
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 30 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/MS
Entry-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 (wwwssishimadzucom) 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
(18391894) and Genzo Shimadzu, Jr
(18691951) 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 GC
In 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 afliates unless otherwise noted.
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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 analyzer
In 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 (wwwellutiacom) 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 NO
2
* 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 NO
2
*, which decays rapidly by emitting light at
600 nm Detection sensitivity compared to carbon is 10
7
The detec-
tion limit is <2 pg/sec
CALIDUS micro GC
Last year at Pittcon, Falcon Analytical (wwwfalconfastnet) 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 (wwwsgscom) 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 (wwwjusticeinnovationscom) now controls and takes
data from the CALIDUS
GC sample preparation
Success in assays by GC often requires selecting appropriate sample
preparation Thus, several firms introduced new technology to fill
application niches
LC-GC 9000
According to Brechbhler (wwwbrechbuhlerch), 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 MS
n
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 (wwwthermofisher
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/TMS
Over the last five+ years, Torion (wwwtorioncom) 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-GC
Defiant Technologies (wwwdefiant-techcom) 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
sampler
Static 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 (wwwteledynetekmar
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 gases
Eclipse 4660 purge-
and-trap sample
concentrator/4551A water
autosampler
Good 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 (wwwoico
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
Brechbhler 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 preparation
Power-Prep GPC
Of course, LC in the form of gel perme-
ation chromatography (GPC) has been
used for decades for off-line sample prep
for GC Gilson (wwwgilsoncom) contin-
ues to promote a GPC feeding a fraction
collector, which then serves as an autosam-
pler for GC Fluid Management Systems
(wwwfmsenvironmentalcom) 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, wwwussilicacom),
and C18 Cleanup with GPC reduces sol-
vent, expensive glassware, and operator
time compared to manual methods
Static headspace sampling
Master static headspace
sampler
Headspace 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 (wwwdanispait) 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 AM
Color profile: Disabled
LGX50 sample preparation module for GC
Sampling liquids for dissolved gases is a real engineering chal-
lenge since gasliquid interfaces must be avoided Attempting
to move a liquid too quickly produces cavitation, compromis-
ing the sample With these constraints in mind, EST Analytical
(wwwestanalyticalcom) introduced the LGX50 sample prepara-
tion module for GC via the US EPAs 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 gases
CDS Analytical (wwwcdsanalyticalcom) 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 pyrolyzer
Pyrolysis 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 001 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. (wwwmarkescom) 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
02 ng by heating the transfer lines to 200 C With GC/MS, the de-
tection limits are less than 01 ppb Using the selected ion monitoring
(SIM) mode on the MS reduces the detection limit to less than 10 ppt
Model 2012 air sampler
The Model 2012 air sampler from CDS Analytical is optimized for
the collection of volatile organics according to US 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 Manifolds
In chromatography, smaller is generally better Airgas, Inc. (www
airgascom) 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
(wwwgerstelcom) 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 T
max
of 220 C
Sample drying
PowerVap Concentrator
Dryng 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-L or 1-mL autosampler
vial, which is attached to the bottom of
the larger sample tube
MultiPurpose Sampler
A similar sample-drying module was intro-
duced by GERSTEL GmbH & Co. (www
gersteluscom) 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 (999999 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 syringes
Diamond Design
As detection limits in GC/MS get smaller,
chromatographers are discovering design
problems that had not been seen before
Take the common syringeSGE (wwwsge
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 extraction
SPE-Xpress
US EPA Method 1664 for oil and grease
just got easier with the introduction of the
SPE-XPress from Environmental Express
(wwwenvexpcom) 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 GC
Gas 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 (wwwf-dgscom)
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 23-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
chromatography
Rtx
-BAC columns
New columns for assay of blood alcohol
from Restek (wwwrestekcom/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 CGC
Secondary columns in GCGC need
to be fast (ie, short) and with broad
selectivity Restek introduced the Rtx
200 series (wwwrestekcom/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 columns
Because of high selectivity, alumi-
na is often preferred for separating
light petroleum factions containing
C2C5, including olefins Restek
RT
-Alumina BOND/MAPD PLOT

columns (wwwrestekcom/catalog/
view/11267) provide rapid separation
More samples...in less time...
with better data and USEPA approval!
On April 17, 2012 the USEPA
Administrator signed a Methods
Update Rule (MUR) approving new
test methods for analysis of NPDES
wastewater samples. ASTM Method
D 7511-09e2 for total cyanide analysis
is included in the MUR.
www.oico.com, 800.653.1711
OI Analytical is a brand of Xylem, whose 12,000 employees are addressing
the most complex issues in the global water market. 2011 Xylem Inc.
OI Analyticals CNSolution
TM
3100 Cyanide Analyzer performs
ASTM D 7511-09e2 and eliminates the 2-hour distillation step
required in older methods. Now thats something to celebrate!
of hydrocarbons up to a T
max
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 columns
Metal columns are more robust and hence
suitable for portable instruments Restek
metal MXT
-Q-BOND and MXT-S-BOND

PLOT phases (wwwrestekcom/chromatogram/
view/GC_PC1184) were developed for the
assay of oxygenated solvents Columns are
available in tight 35- or 70-in coils
Triart Hybrid columns
YMC America, Inc. (wwwymcamericacom)
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 m 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
technology
One 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 Id 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
Im sure that we will see much more on
nano stationary phase technology in the
near future
Column hardware
SilTite -union
For 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 (<05 g) designed
to couple GC columns in a temperature-
programmed oven Cool spots must be
avoided The SilTite -union uses SGEs
double cone ferrule to make the seal
without wrenches for fused-silica capillar-
ies This should be particularly useful in
GCGC or creating mixed column sets,
including guard columns
SilTite ferrules for GC injectors and
detectors are available in graphite, Vespel

(DuPont, www2dupontcom), and SGEs
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: rlsteven@comcast.net.
P
ittcon
2012 was held March 1115, 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 preparation
Automated sample preparation
workstation
The new Omni LH96 automated workstation from Omni Inter-
national (wwwlh96com) 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 applications sample prep, such as pharmaceutical, drug dis-
covery, proteomics, sample processing, and nanotechnology
Protein quantitation system
EMD Millipore (wwwmilliporecom) launched the new Direct
Detect bio-molecular quantitation system for the measurement
of protein quantity in a sample as low as 02 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 system
The new SPRIworks HT from Beckman Coulter (www
beckmancoultercom) 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)
Ultracentrifuge
Beckman 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
Pittcon
2012: Laboratory Instrumentation and

Equipment Product Showcase
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.
Lab
Supplies
from
Amazon?
Centrifuges
Balances
Microscopes
Stirrers
Shakers
Glass Labware
Bottles
Beakers
Condensers
Dessicators
Pipettes
Pipettors
Titrators
Electrodes
pH meters
Refractometers
Spectrophotometers
Hygrometers
Tubes / Vials
Jars
Funnels
Flasks
Carboys
Filters
Homogenizers
Baths
Ovens / Incubators
Lab Furniture
Chemicals
Tongs
Stir bars
Tweezers
Ladles
Syringes
Syringe Pumps
Spoons and Scoops
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LABORATORy INSTRUMENTATION AND EqUIPMENT continued
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
Sonicator
The new Q55 Sonicator from Qsonica
(wwwsonicatorcom) 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
measurement
The FlowCAM PV Series imaging par-
ticle analysis system from Fluid Imaging
Technologies (wwwfluidimagingcom) 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
(wwwmicromeriticscom) 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 25 mm
The WAVE Series electroacoustic and con-
ductivity pore analyzers from Quantachrome
Instruments (wwwquantachromecom) were
demonstrated at Pittcon These pore charac-
terization systems can measure pore size
range of 10 nm5 m, +01 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 mill
The Ultra Centrifugal Mill ZM 200
(Figure 2) with a new cyclone from
RETSCH (wwwretschcom) 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 (wwwspexsampleprepcom)
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 05 to 100 g for various applications,
such as pharmaceuticals, materials testing,
pathology, and environmental
Laboratory evaporator
The RapidVap Vertex evaporator from
Labconco Corporation (wwwlabconco
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 concentrator
Labconco 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
Dual beam microscope
FEI Company (wwwfeicom) 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 system
The new HI 90 hyperspectral imaging system from Bruker Cor-
poration (wwwbrukercom) 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 8501440 cm
1
spectral range
Laboratory instrumentation
Automatic biochemistry analyzer
Newly introduced at the conference, the YSI 2900 biochemistry
analyzer from YSI Inc. (wwwysilifesciencescom) 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 calorimeter
TTP Labtech (wwwttplabtechcom) 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 210 min With only
as small as a 15-L sample, this flow calorimeter cuts down on the
zeta potential, and 05% porosity resolution of various sample types
in chromatography, materials, or environmental applications
Malvern Instruments Ltd. (wwwmalverncom) 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 001 to 3500 m
The new CAMSIZER XT particle analyzer from RETSCH en-
ables the measurement of particle sizes from 1 m 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/imaging
Microscope Digital Camera
The new BLC line of Microscope Digital Cameras with an LCD
tablet was introduced by Carltex Inc. (wwwcarltexcom) 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 microscope
The Phenom proX desktop scanning electron microscope (SEM)
from Phenom-World BV (wwwphenom-worldcom) is a three-
dimensional imaging system with magnification of 8045,000
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 samples 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 equipment
Laboratory vacuum pump
KNF Neuberger Inc. (wwwknfcom) 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 15 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 pump
Vacuubrand (wwwvacuubrandcom) 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 (05 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 Hood
The new UniMax Floor Mounted Fume Hood was announced
by HEMCO Corporation (wwwhemcocorpcom) 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 laboratorys requirements
Glassware washer
The System4Lab glassware washer cleaning solution (Figure 5) was
showcased by Miele (wwwmiele-procom) 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
Refractometer
The new Pro-Juice refractometer from Bellingham + Stanley
(wwwbs-ltdcom), 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 system
Markes International (wwwmarkescom) 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 US EPA Method TO-14/15
compliant With a detection limit of <01 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 meter
Senova Systems Inc. (wwwsenovasystemscom) 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 system
BrandTech Scientific Inc. (wwwbrandtechcom) 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 system
Metrohm USA (wwwmetrohmusacom) 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
Titrator
The Ti-Touch Titrator Series from Metrohm USA was also fea-
tured These new compact titrators for routine analysis are available
and an application support laball under
a five-year limited warranty
Laboratory counting scale
Adam Equipment (wwwadamequipment
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 system
RephiLe Bioscience Ltd. (wwwrephile
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 30120 L/hr, whereas the reverse os-
mosis water system can product 50150
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 consumables
Certified reference
standards
SPEX CertiPrep (wwwspexcertiprep
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
UltraWAVE
milestonesci.com/ultrawave
866-995-5100
BENCHTOP HIGH THROUGHPUT
MICROWAVE DIGESTION SYSTEM
NO VESSEL
CLEANING
EASY TO
USE
CHALLENGING
SAMPLES
FASTEST
RUN TIMES
MIXED
BATCHES
HIGH
THROUGH-
PUT
PRODUCTIVITY TOOLS
Transforming
Metals Prep!
Figure 5 - System 4Lab glassware washer. Watch video at http://goo.gl/ycmmF.
Laboratory software
The ACD/Spectrus Workbooks by
Advanced Chemistry Development, Inc.
(wwwacdlabscom) 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
Conclusion
Pittcon, 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 1721, 2013
Compare and learn more about these new
products and other laboratory equipment
at wwwlabcomparecom
Jeanely Hunt is Content Editor for American Laboratory/
Labcompare; e-mail: jhunt@americanlaboratory.com.
Contact us for a free trial copy of Quansoft
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T
hirty 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 (wwwwaterscom)
clearly has the vision now Waters has
enjoyed 20/20 vision in the past, so lets
check back in 2020
ACqUITy UPC
2
Waters added a Pittcon Editors Gold

Award to its collection of plaques from
prior years The new ACQUITY UPC
2

(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 UPC
2
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, CO
2
is more
compatible with MS than most any other mo-
bile phase, and is much less expensive
New Developments in Supercritical Fluid
Chromatography (SFC) at Pittcon
2012:
20/20 Vision?
Conference Review
During the Q&A following the formal
introduction, Art Caputo, President of
Waters, predicted that UPC
2
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!
Lets look at the advantages first: Waters
believes that UPC
2
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-
strumentsSFC 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 (eg, capillary
columns replacing packed columns) in GC is
only about 3% per year
New preparative SFC
Chiral separations are the most often-
cited advantage of SFC, both on the ana-
lytical and preparative scale JASCO (www
jascoinccom) 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 P
max

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 07, 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 columns
In 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 SB
In support of the UPC
2
, Waters introduced
three columns and promised one more
Each is specifically optimized for SFC
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A new generation of glass
reduces the interaction
of analytes and the glass
TM
Ge t Be t t e r
Re sul t s.
Detectlowabundanceanalytesnormallyadsorbedbyglass
PreventspHchangesinvialsbeforeinjectionevenhourslater
Preventssamplehydrolysisthatcanoccurinyourvials
Nomeniscuswhenwaterisusedasthemainsolvent
NotCoatedorSilanized
PatentPending
Advanced Quality (AQ) vials and inserts manufactured with RSA Glass have
reducedsurfaceactivityduetotheeliminationofthelayerofsilicathatresultswhen
vials are normally manufactured and many of the surface metals that contaminate
analysisandhavedetrimentaleffectsonyourresults.
When using ordinary borosilicate glass autosampler vials and inserts, sample
diluents (such as water) can de-protonate the many hydroxyl groups on the wall of
your vial which produces a negative charge on the glass.Theacidic functionality
of these silanols has been known to cause adsorption of basic compounds, change
thepHofthesamplesolutionand/orhydrolyzesomesusceptiblecompoundsmaking
themundetectable.Thesurfacemetalcontaminantscancauseprecipitation,chelation
orotherchangesinyoursampleswhileinthevial.
WithRSAGlassvialsandinsertsthereisvirtuallynolosstothevial,nopH
shiftingorotherproblemsthusmakingyouranalysismorereliable,lottolot,runto
runanddaytoday.Avoidfrustrationofunreliabledata.
RSA autosampler vials and glass inserts are manufactured without
using any coating of any type making them an excellent choice for LC, LCMS,
GC and GCMS compared to coated vials for many applications.
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Is your data at risk
due to the reactivity
of your autosampler vials?
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The Advantage
G
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t
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.
Thedatatablebelowillustratesthepowerandusefulnessof
RSAglassvialsforchromatography.Thedatacoloredgreen
inthechartshowshowtypicalglassvialsonthemarkettoday
willadsorbbasiccompounds.Whenyouranalytesareinlow
abundance, ordinary glass vials can greatly skew your data.
VialsmadewithRSAglasswillprovidemorereliabledata
andnotskewit.
Methodology Synopsis & Analysis: a test solution was placed in 3

sets of vials named (N1, N2 & N3) from each of the brands listed.
The starting concentration of the test compounds was 5ug/ml.
After standing in the vials for four hours, the fnal concentration of
the analyte, as determined by HPLC, is reported for each group. The
percent loss was calculated and is reported (% Loss) as well. The
difference in the results between RSA glass vials and the others is
one indication of the benefts of using RSA glass.
A second illustration of the benefts of RSA glass vials, is
shownbelowandiscoloredred.Thisdatashowsleadingvials
onthemarkettodaymaychangethepHofyoursamplesdue
totheirsurfacechemistrywhereRSAglassdoesnot.
Methodology Synopsis & Analysis:
Methodology Synopsis & Analysis: DI water (pH 5.45) was placed
in the same brands of vials as previously stated and several pH data
points were taken at the start and randomly during a 4 hour test
period. The data reported below in red is the ending pH readings
from this Test. This simple test and other more extensive tests have
shown that RSA
glass vials do not cause any changes in the pH

of the sample solutions during the test period. Market leading vials
can cause changes by more than 1.25 pH units.
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Adsorption & pH Change Comparison To Market Leaders
STARTINGPOINTS:AdsorptionTest;5ug/mlChlorhexideneinwater;pHTest;DIWaterpH5.45.
RSAGLASSVIALS:ReducedSurfaceActivityGlassVials.
MICROSOLVBRANDVIALS:ourleadinglineofautosamplervialsandinsertsonthemarkettoday.Madewithpharmaceuticalgradeglass.
BASIKBRANDVIALS:ourpopularbrandofeconomyautosamplervialsforwhenqualityissuesaremostlylimitedtoftandform.
BRANDF:aleadingbrandofautosamplervialsresoldbymanylaboratorysupplydealers.
BRANDNistheleadingbrandofautosamplervialssoldthroughdealersandprivatelabeledbysomeofthelargestinstrumentcompanies.
N1 N2 N3 AVG % LOSS pH

Starting Points 287.8 287.0 286.1 287 0.00 5.45

RSA Glass 283.5 287.2 287.21 286 0.35 5.50
MicroSolv Brand 234.9 235.2 239.1 236 17.62 6.15
Basik Vials 157.7 158.7 159.9 159 44.64 6.0
Brand F 114.3 223.2 57.3 132 54.14 6.65
Brand N 168.8 149.9 146.5 155 45.96 6.94
Green=SampleAdsorptionTestRed=pHChangeTest
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Compare RSA
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Vials for your chemistry
not just for your autosampler!
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INSERTS AQ
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VIALS AQ
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9509S-WAV-RS 2mlvials,amber9mmscrewtopw/writeonpatch.
9512C-0CV-RS 1.5mlvials,clear,MaxRecoverycenterdrainingsnaptop.
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9512C-0CV-T-RS 1.2ml,MRQvials,clear,snaptops.
9512S-0CV-T-RS 1.2ml,MRQvials9mm,clear,screwtops.
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SCREW CAPS AQ
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9509S-3WAP-RS 2mlamberwriteonvialsandlightblueAQRscrewcapsw/preslitsilicone/PTFEsepta.
9509S-3WCP-RS 2mlclearwriteonvialsandlightblueAQRscrewcapsw/preslitsilicone/PTFEsepta.
9512C-1MP-RS 1.2mlclearMRQvialsandbluesnapcapsw/silicone/PTFEsepta.
9512C-3MP-RS 1.2mlclearMRQvialsandbluesnapcapsw/preslitsilicone/PTFEsepta.
9532S-1CP-RS 300ulfusedinsertvialsandlightblueAQRscrewcapsw/silicone/PTFEsepta.
9532S-3CP-RS 300ulfusedinsertvialsandlightblueAQRscrewcapsw/preslitsilicone/PTFEsepta.
9512S-1CP-RS 1.5mlMaxRecoveryVials,clearandlightblueAQRscrewcapsw/silicone/PTFEsepta.
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9512S-1MP-RS 1.2mlMRQVials,clearandlightblueAQRscrewcapsw/silicone/PTFEsepta.
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9512C-0CV-RS
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9509S-WAV-RS
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9502S-02N-RS
9512C-0CV-T-RS
9512S-0CV-RS
9532C-0CV-RS
9502C-30CB
9509S-10C-B
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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: rlsteven@comcast.net.
1) The BEH 2-EP (ethylpyridine) is bonded to a 17-m 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 21 50 to 150 mm Particle size is 17
m Midyear, Waters plans to introduce the HSS C18 SB surface
chemistry on 18-m high-strength silica All four phases will also be
available in 35-m diameter
GreenSep Basic SFC
Last year, ES Industries (wwwesindcom)
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-m silica spheres Pore diameter is
120 Compared to GreenSep Ethyl Pyri-
dine, the imidazole phase provides much
stronger retention and improved selectivity
for separation of amine-containing analytes
GreenSep Silica
Silica 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 18 m and as large as 20 m
COSMOSIL 3-hydroxyphenyl
Nacali USA, Inc. (wwwnacalaiusacom) 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 classification
It 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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T
his 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
) (wwwpittconorg/
exhibitors/attendstatsphp) 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 years 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 spectrometer
picoSpin-45L
The picoSpin-45L benchtop NMR spec-
trometer (wwwpicospincom), available
from Cole-Parmer (wwwcoleparmercom),
is a 45-MHz NMR weighing just 105 lb (47
kg) Intended primarily for educational labs,
reaction monitoring, and QA/QC laborato-
ries, the fully integrated, compact device (7
575 115) 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 L) 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-
Pittcon
2012 Roundup of Spectroscopy and

Mass Spectrometry
Conference Review
ciate at Cole-Parmer You can use regular
solvents as long as they dont 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, picoSpins 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 spectrometer
MicroNIR
The MicroNIR spectrometer from JDSU
(wwwjdsucom) 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
(9501650 nm and 11502150 nm), the
MicroNIR supports real-time evaluation,
field testing, and on-line process monitoring
to allow lower-cost sampling
Electron magnetic
resonance spectrometer
AffirmoEX
Also releasing a benchtop instrument for
the education market was Oxford Instru-
ments Magnetic Resonance (OIMR)
(wwwoxford-instrumentscom) which, with
Active Spectrum Inc. (wwwactivespectrum
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 1125 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 97 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/OES
SPECTROBLUE
SPECTRO Analytical Instruments (www
spectrocom) 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 instrument
RT100 LIBS
Applied Spectra (wwwappliedspectracom) 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 spectrometer
INPHAZE
The new INPHAZE from eDAQ (wwwedaqcom) 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
Spectrofluorometers
FluoroLog
EXTREME and FluoroCube EXTREME

HORIBA Scientific (wwwextremefluorescencecom) announced
what it calls the worlds first commercial integrated supercontin-
uum powered spectrofluorometers The systems pair HORIBA
Scientifics FluoroLog
(for steady-state fluorescence) (wwwhoriba

com/scientific/products/fluorescence-spectroscopy/steady-state/
f luorolog/f luorolog-r-our-modular-spectrof luorometer-522/)
and FluoroCube (for fluorescence lifetime) (wwwhoribacom/
scientific/products/fluorescence-spectroscopy/lifetime/fluorocube/
fluorocube-our-compact-benchtop-spectrofluorometer-825/) spectro-
fluorometers with the SuperK EXTREME white light laser from
NKT Photonics (wwwnktphotonicscom) 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 Its difficult to get
these instruments to work together reliably, he says Thats why the
integrationis so valuable
Raman instruments
Also 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
Cells
Micro Volume Analysis
Fiber Optical Systems
Calibration Standards
Micro Flow Channels
Precision is not a matter of opinion, but the result of leaving not even the
slightest detail to chance. That is why the TrayCell is uniquely precise and
among the first choice for many users in the field of bio analytics. Learn
more about Hellma precision: call 516-939-0888 or visit www.hellmausa.com
Sample volume 0.5 l 10 l!
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SPECTROSCOPy AND MASS SPECTROMETRy continued
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 1000
The Verifier Process System 1000, a Ra-
man analyzer for use in pharmaceuticals
and chemical manufacturing, was show-
cased by Mustard Tree Instruments (www
mustardtreecom) 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 Raman
Other 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-2-785/1064
Rigaku Raman Technologies (www
rigakuramancom) also unveiled a hand-
held, Wi-Fi-enabled Raman device, the Xan-
tus-2-785/1064, which the company calls
the worlds first dual wavelength handheld
Raman analyzer
The compact (138 cm 274 cm 98
cm), 81-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. (wwwbwtekcom) 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 explainsa 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 Its a completely standalone instrument
UV-Protective Eye
and Face Wear
Specially designed to
protect users against
unwanted UV exposure.
UV Transilluminators
Deliver superior irradiance uniformity and UV intensity
for all viewing and photodocumentation needs.
UV Bench and Display Lamps
Lamps with various wattages and UV
wavelengths provide both high intensity
and wide area of light coverage.
UV Crosslinkers
Provide accurate, error-free and super-fast
membrane crosslinking and sample UV dosing.
AccuMAX Digital Meters
Advanced microprocessor-controlled units
with software-driven functions. Ensure max-
imum accuracy and reliability in measurement
of UV and visible light sources.
MiniMAX UV Viewing Station
Space-saving mini-cabinet and UV lamp
combination makes the perfect portable
UV viewing station. Light weight and compact.
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Miniature UV Pencil Lamps
Double-bore quartz lamps used for wave-
length calibration and emission. Custom
lamps for OEM applications also available.
Thermo Fisher Scientific (wwwahurascientific
com/truscan) and the PinPointer from Ocean
Optics (wwwoceanopticscom) Many other op-
tions can be found at wwwlabcomparecom
XRF instruments
NEX QC VS
Applied Rigaku Technologies (www
rigakuedxrfcom) 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 13-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
GoldXpert
Olympus Innov-X (wwwolympus-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 spectrophotometers
NanoDrop Lite
Thermo Fisher Scientific (wwwthermofisher
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 L 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 thats 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 16 115 cm, the result-
ing package is fully containedtheres
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-2700
Making their Pittcon debuts were
Shimadzu Scientific Instruments (www
ssishimadzucom) 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 Shimadzus 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
modules
Axiom Analytical (wwwgoaxiomcom)
and Symbion Systems (wwwgosymbion
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 flexibly coupled diamond
and conventional ATR probes and mul-
tipass Raman probes for more than 10
enhancement in sensitivity
FTIR systems
FTIR sealed liquid cell
International Crystal Laboratories
(wwwinternationalcrystalnet) 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 005 mm
to 5 mm
MB-Rx Reaction Monitor
ABB (wwwabbcom) showcased its MB-
Rx Reaction Monitor, an FTIR analyzer
for real-time, in situ monitoring of chemi-
cal reactions Measuring 435 cm 280
cm 372 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 0005% and
000005%, the UV-2600 and UV-2700
can measure up to 5 and 85 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 Cell
Starna Scientific Ltd. (wwwstarnacom)
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 05-, 02-, and 0125-mm pathlengths
Using sample volumes down to 06 L
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
4500
AB SCIEX (wwwabsciexcom) 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
SCIEXs 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 companys 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 (wwwphenomenexcom)
columns, multiple reaction monitoring
(MRM) transitions, and retention times for
each compound The user simply selects
the desired pesticides, and the systems
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 Q
Thermo 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 Exactive
The 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
SCION TQ
Launched in July 2011, the SCION TQ
GC/MS/MS system from Bruker Daltonics
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(http://scionhasarrivedcom) 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 05
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 Brukers 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 Brukers ionBooster next-generation
high sensitivity electrospray ion source, which the company claims
can yield 5100-fold improvements in sensitivity
LAESI
DP-1000
Winning 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 OH bonds of untreated aqueous (eg, 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 mapthat is, a mass spec-
tral imageof 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 (wwwwaterscom) mass spectrometers At Pittcon,
Waters and Protea (wwwproteabiocom) announced a co-marketing
agreement to make the DP-1000 available to new and existing users
Nasco Whirl-Pak Division
American Laboratory
May 2012
AL1205
AL1205
Conclusion
Naturally, 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 WE Moerner, Chair of the Department of Chemistry at Stan-
ford University and this years winner of the Pittsburgh Spectroscopy
Award, has spent nearly three decades developing the single-molecule
spectroscopy techniques underlying one of todays 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 machineswe can learn a lot by going to the single
molecule level, he says
Well 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: jeffrey.perkel@gmail.com.
of Waters SYNAPT G2 and SYNAPT G2-S mass spectrometers run-
ning under MassLynx
control
expression Compact Mass Spectrometer
Advion Inc. (http://advioncom/biosystems /expression) announced
the commercial availability of its expression Compact Mass Spec-
trometer (CMS) Measuring just 106 216, 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 <07 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 (wwwalmscocom), the mass spectrometry di-
vision of Markes International Ltd. (wwwmarkescom), 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 (www1stDetectcom) announced the intro-
duction of the MMS-1000 miniature mass spectrometer, an ion
trap mass spectrometer measuring just 75 125 9 and weigh-
ing less than 17 lb With a sensitivity of 1 ppt and a resolution of un-
der 05 Da FWHM, the MMS-1000 delivers rapid MS/MS detection
of trace levels of volatile compounds in around 5 sec
Microchannel plates
PHOTONIS USA (wwwphotoniscom) 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 tour
Phenomenex and AB SCIEX kicked off a 30-city cross-country bus tour
called the MASS-tastic Voyage 2012, a mobile labmodeled on the semi-
tractor trailers used to haul NASCAR carsshowcasing 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 US three times before terminating in Vancouver at ASMS 2012
in May (See wwwmasstasticvoyagecom for a complete schedule)
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E
ight years have passed since Waters (wwwwaterscom)
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 chromatographs
Chromatographers at Thermo Fisher Scientific (www
thermoscientificcom) have extended the P
max
of the Dionex
(wwwdionexcom) 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-m-
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 525 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 platform
Nanospray 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
apmaldicom) introduced the The-LCP thermally stabilized
platform for high-temperature nano LC separations Running at
an elevated temperature increases the separation efficiency In
Advances in Liquid Phase Separation at
Pittcon
2012
Conference Review
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 LCs
Analytical Technologies Ltd. (ATL) (wwwais-indiacom) 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 components
Occasionally, I attend a press conference where the sub-
ject matter is completely different than expected This year,
SFC Fluidics
(wwwsfc-fluidicscom) 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 flow to deliver accurate, pulse-free flow over the
nL to L range It is small (~1 in
3
) and lightweight, and P
max

is 300 psi The pump operates by applying a voltage across a
porous membrane The ions drag water of hydration across
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the membrane The volume increases, but is confined, so the
pressure increases A second impermeable flexible membrane
separates the osmotic section from the delivery fluid, 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, wwwgelifesciencescom) for
separating proteins, including bovine serum albumin (BSA), ov-
albumin, myoglobin, and transferrin SFC components should
also be useful in flow injection analysis
Recycling module
From 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) (wwwjaicojp/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 14,
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 HPCE
Despite 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.
(wwwbiopticcomtw) 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 25-min separations with
high detection sensitivity (4 bp resolution at 50500 bp
range) from a 96-well plate Average %RSD in migration time
is less than 075% 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 interface
PostNova Analytics (wwwpostnovacom) and Malvern Instruments
Ltd. (wwwmalverncom) 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 34 times Targeted applications include pro-
teins, ie, aggregates, and nano particles of gold, silver, and carbon
HPLC detectors
QD detector for ion chromatography
At 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 worlds 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 Detector
Many 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 (wwwmetrohmcom) 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/MS
IONICS Mass Spectrometry Group (wwwionicsca) 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 51500 m/z Dynamic range is
better than 10
6
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/MS
Ion mobility spectrometry (IMS) is par-
ticularly useful in separating isomers
Excellims Corp. (wwwexcellimscom)
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 LCLC
and SFCLC, 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 10
2
to 10
3
Typical
applications include separation of skeletal
peptide isomers, diastereomers, cistrans
isomers, and carbohydrates
The most significant figure of merit for
HPLC detectors is usually the noise level
SCINCO (wwwscincocom/en) intro-
duced the DAD-208 diode array detector
with a noise level of 25 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 2155 L The
company is looking for OEM partners
Flow splitter for detectors
Splitting column flow between detec-
tors is a technique that sounds good in
concept but is frustrating in practice
Analytical Scientific Instruments, Inc.
(ASI) (wwwhplc-asicom) 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 15, 525, and 2590 Flow ranges
of the side stream (in L/min) are 01
05, 0525, 25125, and 125625
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 module
Now 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
ssishimadzucom) 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 <00015%; %CV
is <1% for 05-L injections and <02% for
injection volumes greater than 5 L Mini-
mum cycle time is 14 sec
Chromatography simulation
and method development
software
DryLab
4 from Molnr-Institute (www

molnar-institutcom) 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. (wwwcamagcom)
introduced the DBS-MS 500 for sam-
ple prep for MS For DBS, the dried
cards from Whatman (wwwwhatman
com) or ID Biological Systems (www
id-biologicalcom) 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
DryLabs 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 system
In the booth of Bischoff Chromatog-
raphy (wwwbischoff-chromde), 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 prep
Dried blood spots
sampling systems
Despite decades of experience with
dried blood spot (DBS) sampling for
phenylketonuria (PKU), the FDA has
800-452-7265 (United States) 812-235-6167 (International)
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QuEChERS
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Ideal economical sample prep mixer for the
QuEChERS method. Entire racks of 15ml or
50ml tubes can be shaken vertically, or full
tubes can be shaken horizontally.
placed in the sample rack for archiving
One study showed that the %CV for
560 replicate DBS samples was 28%
with the CAMAG systems Manual ex-
traction had a %CV of 457%
Protein digestion platform
Digesting proteins with enzymes is
one of the common techniques in pro-
teomics Shimadzu has teamed with
Perfinity Biosciences (wwwperfinity
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
|H|||||1 |||1||l1|\ 44 H|\ /|l/
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 a
legacy HPLC (i.e., P
max
of about 6000 psi) should select columns
packed with 3.6-m particles. One running UHPLC should take
advantage of the 1.7-m particles. These columns provide un-
expectedly high column efficiency and resolution compared to
even 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-m particles. In HPLC, maximized peak
capacity (peak count) is achieved with long columns packed with
larger-diameter particles. The tradeoff is much, much longer
run time.
Kinetex
phenylhexyl ligands
Bonded to Phenomenex Kinetex
particles, phenylhexyl ligands

(www.phenomenex.com/Products/HPLCDetail/Kinetex/
Phenyl-Hexyl) are useful in separating moderately polar analytes
such as chlorophenols, steroids, phthalates, and geometric iso-
mers. An animation of the phase showed a benzene ring con-
TLC/MS interface
TLC 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 the
TLC plate and eluting the material in a tube, then transferring the
liquid into the MS, which is cumbersome by todays 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 is
located with cross-hairs. An arm lowers and presses the solvent in-
let/outlet probe over the target spot. The solvent is metered in and
passes up the outlet directly to the MS. The on-line nature of the
operation gives a throughput of a spot per minute.
LC columns
Aeris Core-Shell HPLC/UHPLC columns
Aeris 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
ISO Guide 34 17025 9001

You Set the Standards
We make them!
AAAAAAAAAAAAcccccccccccccccccccccccccccccccccccccccccuuuuuuuSSSSSSSSSStttttttaaaaaaannnnnndddddddddddddaaaaaaaaaaaaaaaarrrrrrrrrrrddd.com 20 20 20 20 220 20 200000 20 20 20 20 20 20000 220 20 220 200 200 220 2200 20 200 2220 2 3- 3333333333- 3-- 333333 7777778 778 788888888 7788 788 788 7888 778 78 778 778 778 7788 78 7866666666- 666- 66-- 6- - 6666- ---- 66- 66666666 52 552 552 52 52 5555552 52 2 52 52 222 52222 52 2222222 52 2222222222222 00 90 0 90 90 90 90 90 90 90 90 90 0 90 90 90 990 000 990 9990 0 9990 99999990 00 990 999990 9 8880 80 80 80 80 80 80 80 80 8000 80 80 8000 80 800000 80 800 8000 80000000 8000000 800 80000 800000000 80 80 800000 8000 8000 800 888800 8 0000000000- 0- 00000000000- 0000- 0000000- 000-- 0------- 0-44444444444444 44 444444 444444 444 44444 44444444 4444444 44444444444 444 44444 44444 444444 4444444 4444 442- 2- 2 5552 52 52 22 52 2 52990 90 90 90
nected to the Kinetex core shell particle via an n-hexane tether
As with the Aeris Core-Shell, columns packed with 26-m parti-
cles provide good separation efficiency for HPLC (~6000 psi) in-
struments Columns packed with 17-m 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 UHPLC
Since 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 (wwwphenomenexcom/Products/
HPLCDetail/SecurityGuard%20ULTRA), which is specifically
designed for UHPLC columns from any vendor (www
phe nome ne x c om/Pr oduc t s /HPLCDet a i l /Ki net e x /
Phenyl-Hexyl) The columns are rated to 20,000 psi They are
small (<03 L) and not a significant source of extracolumn
band broadening
Ultra HPLC columns
Restek (wwwrestekcom) extended its Ultra HPLC column line with
three new surface chemistries The Ultra line is based on 3- or 5-m
spherical silica with 100- 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 (wwwrestekcom/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 (wwwrestekcom/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 (wwwrestekcom/catalog/view/32171)
USLC columns
The section describing DryLabs 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 (wwwrestekcom/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 27-m Halo particles
The CN provides a stable, reversed-phase
packing suitable for basic, acidic, or neu-
tral analytes (wwwsigmaaldrichcom/
analytical- chromatography/analytical-
productshtml?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 analytes
The sub-2-m market offering is expand-
ing as more vendors add new station-
ary phases Fortis HILIC from Fortis
Technologies (wwwfortis-technologies
com) is now available in columns packed
with 17-m 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 ERLIC
Deamidation of asparagine and gluta-
mine residues in proteins occurs natu-
rally In vivo deamidation is believed to
play a role in cataracts and Alzheimers
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 phase
Nacalai USA, Inc. (wwwnacalaiusacom)
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 = 07) 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 phase
ES Industries (wwwesindcom) 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
interactions The stationary phase
is a proprietary ligand bonded to 18-
m porous silica This provides excellent
column efficiency and speed The new
phase offers unusual but stable selectiv-
ity, which provides robust methods
Ascentis
Express
Supelco (wwwsigmaaldrichcom) intro-
duced three surface chemistries to the
Ascentis
line of Fused-Core columns for

HILIC (wwwsigmaaldrichcom/analytical-
chromatography/analytical- products
html?TablePage=104698603) For Ascen-
tis Express F5, a PFP group is bonded to
27-m Halo particles via a propyl tether
The PFP phase can function as a reversed-
phase packing with selectivity It also
functions in the HILIC mode when the
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Dr Andrew Alpert, President and Founder of PolyLC Inc. (www
polylccom), 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 columns
IonPac columns for
ICS-4000/5000
To 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-m-diam particles packed into
04-mm-id tubes Prior columns uti-
lized 55- or 9-m-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
AS18-4m 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 US EPA Methods 3000(A) and
3001 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 AS18-4m column with the ben-
efit of reduced run time with no loss
in resolution The IonPac AS18-4m
column is available in capillary for-
mat, 04 150 mm (wwwdionexcom/
en- us/product s/col umns/i c- r f i c/
hydroxide- selective- packed/ionpac-
as18-4um/lp-111535html)
Similarly, the AS11-HC-4m column
and the CS19-4m capillaries are also
packed with 4-m particles in capil-
lary format The improved efficiency
obtained with smaller particles allows
use of 23 times higher flow rate with
constant resolution, but reducing run time by the reciprocal
factor When operating at the standard flow rate of 0010 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 flow
rate of 0030 mL/min, a high-pressure capillary IC system such
as the ICS-5000 or ICS-4000 is required
MAbPac SCX-10 columns
Screening monoclonal antibodies just got faster by reducing the
diameter of the column particle to 3 or 5 m diam from 10
m MAbPac SCX-10 columns from Dionex are effective for
The new CentriVap
micro IR
The right size vacuum concentrator for
smaller applications. When your sample throughput, bench
space and budgets are small, the new CentriVap micro IR ts just right.
Even better, what it lacks in size it makes up for in features and
accessorieseverything you need to start concentrating is included.
Infrared-emitting (IR) glass lid directs heat to the samples
to speed evaporation
Built-in PTFE-coated diaphragm vacuum pump and chamber
Rotor for 24 microcentrifuge tubes (1.5 ml each)
CentriZap micro IR strobe light to view samples while rotor spins
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5-m 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- m-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 packings
A 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, 550 m) Six pore diam-
eters are available from 50 to 500 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 column
Adenosine 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 (wwwimtaktusacom) 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 columns
Surfactant 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
Hydraulic Laboratory Presses
and Ac ces so ries
Carver, Inc.
1569 Morris St., P.O. Box 544
Wabash, IN 46992-0544 USA
Tel: 260-563-7577
Fax: 260-563-7625
Free New
Catalog
Standard models
with 12 to 100 ton
ca pac i ty. Manual
and au to mat ic.
Ded i cat ed
ap pli ca tions.
Detailed spec i fi -
ca tions in clud ed.
Custom de sign
avail able.
100th ANNIVERSARY
1912-2012
ISO 9001:2008 Certified
www.carverpress.com
Nanomicro UniPS beads are made of
polystyrene/divinylbenzene copolymer
Particle diameters start at 2 m and ex-
tend to 60 m Photomicrographs sup-
port the claim of monodisperse particle
distribution The company also offers
polyacrylic particles in three size cuts
from 20 to 60 m 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
phases
SiliaPrepX
SiliCycle (wwwsilicyclecom) 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
cartridges
Early 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
(wwwthermoscientificcom/ecomm/
ser vl et /newsdet ai l ? storeId=11152&
contentId=54068&ca=sola-spe)
LC fittings
EXP
fittings from Optimize Tech-

nologies (wwwoptimizetechcom) 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 13 L 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
L 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 (wwwnews-medicalnet/news/
20120312/Thermo- Fi sher- Sci enti f i c-
launches- Acclaim-Surfactant-Plus-and-
MAbPac - SCX- 10- chr omat ogr aphy -
columnsaspx?page=2)
orders@surmodics.com | 952-500-7200 | www.surmodics.com
ProteinStabilizers/Blockers
BioFXSubstrates/StopReagents
Diluents/Buffers/IHCReagents/AccessoryReagents
DIARECTAutoimmune/InfectiousDiseaseAntigens
BioFXAntibodies/Streptavidin
MicroarraySlides/Surfaces
SurModics In Vitro Diagnostics
The Gold Standard in Diagnostic Assay Components
SurModics Am Lab May 2012 third pg square.indd 1 4/18/2012 4:14:11 PM
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 standards
In 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 2013
Next 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 1721, 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: rlsteven@comcast.net.
Check valves
Decades 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 (wwwidexcorp
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 valves
IDEX introduced three new valves with 6, 7, and 10 ports for
next-generation UHPLC applications Rheodyne TitanHT
Find products from leading manufacurers
Compare features and specications
Watch videos
Get quotes
www.labcompare.com
Product research made easy
Benchtop Basics: Tips for Buying pH Meters
and Balances
by Caitlin Smith
M
ost 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 electrochemistrywhen
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 meters
A 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 options
Another 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 0001400 The HI 4521 pH/
Conductivity (USP) Bench Meter from
Hanna Instruments (Smithfield, RI) has a
pH range from 2000 to 20000 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 range
While 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 meters
Like 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-
powered by
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 001999 mS/cm,
while the SevenMulti S70 Luxury Con-
ductivity Meter (Mettler-Toledo) has a
range of 00011000 mS/cm
Benchtop conductivity
meter and portable
conductivity meter choices
Benchtop 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 001990 mS/cm,
and the HI 98188 Waterproof Portable
EC/Resistivity/TDS/NaCl and Temper-
ature Meter from Hanna Instruments
measures 01000 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
Conclusion
Electrochemistry equipment such as pH
meters, conductivity meters, and balances
provide essential, everyday measurements
ELECTROCHEMISTRy PRODUCTS continued
Analytical Balances
Few 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 001 or 01 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 items 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 120250 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 Loui s, MO), OHAUS (Parsi ppany,
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 options
Researchers 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
alternatives
Those 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 (ie,
with a 005-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 21032,000 g,
while the Denville Scientific Precision Top
Loading Laboratory Balance has a capacity
of 1504500 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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Available on the
AL
AL
that researchers could not function with-
out Hopefully the considerations dis-
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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: caitlin.smith@comcast.net.
Mass Spectrometers for Use in
Clinical Diagnostics
by T. Keith Brock
T
he 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
buyers clinical needs
Mass spectrometers:
Background and features
Mass 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
spectrometry
Ion 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 techniques
Regardless 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 analysis
Once 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 analysis
Once 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 requirements
Throughput
There 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 selectivity
The 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
powered by
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 accuracy
Precision 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 01 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 software
Mass 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
Validation
Once the buyers 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 points
Conoley 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
Conclusion
When purchasing a mass spectrometer, cer-
tain regulatory issues (ie, 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
Reference
1 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: biobrock@gmail.com.
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 Features
Checklist
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
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
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of traditional glassware for measuring polymer intrinsic viscos-
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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
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