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O
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Mass Cytometry:
An ICP-MS Approach
for Single-Cell Analysis
An Interlaboratory Comparison
Study for Arsenic Determination
New Spectroscopy Products
at Pittcon 2015
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ycled P
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on
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8 Spectroscopy 30(5)
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CONTENTS
COLUMN
May 2015
Volume 30 Number 5
Atomic Perspectives . . . . . . . . . . . . . . . . . . . . . . . 14
Mass Cytometry: An Evolution in ICP-MS
Enabling Novel Insights in Single-Cell Biology
New developments in mass cytometry are enabling advances in the study of cellular
functions such as apoptosis, cell signaling pathways, the cell cycle, and DNA damage.
Farah Virani and Scott Tanner
FEATURED ARTICLE
2015 Review of Spectroscopic Instrumentation . . . . . . . . . . . . . . . . . . .
24
Our annual review of products introduced at Pittcon or during the previous year, broken
down into the following categories:
Accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Atomic Spectroscopy . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Mass Spectrometry . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Mid-IR . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
NIR . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
NMR . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Raman . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
UVVisible. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
X-ray . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
26
28
28
35
37
39
41
41
41
41
46
ON THE WEB
WEB SEMINARS
Demystifying Sample Preparation
for Trace Metal Analysis: How
Automation Can Make Light Work
of the Sample-to-Results Workflow
Daniel Kutscher, PhD, and Sanja Asendorf,
Thermo Fisher Scientific
The Diversity of UV/Vis/NIR
Techniques for Nanomaterial
Characterization:
Jeffrey Taylor and Chady Stephan,
PerkinElmer, Inc.
New Ways of Automating Analysis in
Confocal Raman Imaging
Thomas Dieing, PhD, WITec
What Does USP Chapter <2232> on
Elemental Contaminants in Dietary
Supplements Mean for You?
Robert Thomas, Scientific Solutions
spectroscopyonline.com/SpecWebSeminars
Like Spectroscopy on Facebook:
www.facebook.com/SpectroscopyMagazine
Follow Spectroscopy on Twitter:
https://twitter.com/spectroscopyMag
Join the Spectroscopy Group on LinkedIn
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PEER-REVIEWED ARTICLE
An Interlaboratory Comparison Study for the Determination
of Arsenic and Arsenic Species in Rice, Kelp, and Apple Juice . . . . . . . . . . .
48
DEPARTMENTS
News Spectrum:
Near-Infrared Hyperspectral Imaging Detects Peanut Contamination . . . . . . . . . . . 12
Is There a Spectroscopy App for That?
The APE Optics Calculator. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
Products & Resources . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62
Calendar . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65
Showcase and Ad Index . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 66
Spectroscopy (ISSN 0887-6703 [print], ISSN 1939-1900 [digital]) is published monthly by UBM Life Sciences 131 West First Street,
Duluth, MN 55802-2065. Spectroscopy is distributed free of charge to users and specifiers of spectroscopic equipment in the United
States. Spectroscopy is available on a paid subscription basis to nonqualified readers at the rate of: U.S. and possessions: 1 year (12
issues), $74.95; 2 years (24 issues), $134.50. Canada/Mexico: 1 year, $95; 2 years, $150. International: 1 year (12 issues), $140; 2 years (24
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College of Pharmacy
Barbara S. Larsen DuPont Central Research
and Development
Ian R. Lewis Kaiser Optical Systems
Rachael R. Ogorzalek Loo University of California Los Angeles, David
Geffen School of Medicine
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Wave goodbye
The ED-XRF analyzer that performs like a WD-XRF at much lower cost.
Once you see SPECTRO XEPOS HE ED-XRF spectrometers in action, youll send your pricey wavelength dispersive
X-ray uorescence model packing. The affordable SPECTRO XEPOS provides comparable performance for critical
applications from rapid screening analysis to precise product quality control. Its very likely the industrys most powerful
benchtop energy dispersive X-ray uorescence tool. Its unique TURBOQUANT software analyzes unknown samples without extensive
setup, supplying fast, accurate results. And its probably the only benchtop ED-XRF utilizing 60 kV source excitation optimized
with advanced excitation geometry for maximum energy generation, resulting in low detection limits and ultimate precision.
ED
XRF
http://xrf.spectro.com/xepos
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8005485809
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News Spectrum
Near-Infrared Hyperspectral Imaging
Detects Peanut Contamination
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ABB Inc.
Measurement & Analytics
Phone: +1 418-877-2944
Email: ftir@ca.abb.com
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14 Spectroscopy 30(5)
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Atomic Perspectives
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rangement and to order cells according to their developmental timing. The intensity of expression of these cell lineage
markers provides insight into the unique cell differentiation
pathway of hematopoietic cells and detects multiple pathways across a number of cell subsets (2,3).
The mass cytometer provides researchers with a tool to
examine normal and diseased cells and interrogate the cells
to understand biological processes. The addition of cytokines and drugs to stimulate or suppress specific markers
provides a more complete picture of the pathway-specific
signaling responses in various cell types (3). Cancer-specific
panels of markers are designed to provide a deeper understanding of the intracellular biology involved in the progression of cancers and drug response (including resistance) and
can be expected to lead to more-informed treatment decisions in the future.
Isotope Resolution
Mass cytometry provides an advantage over current flow
cytometry methods by obviating the need for fluorescence
compensation because of spectral overlap of fluorochromes.
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2015 Thermo Fisher Scientic Inc. All rights reserved. All trademarks
are the property of Thermo Fisher Scientic Inc. and its subsidiaries.
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90
100
80
90
70
80
Intensity
Intensity
100
60
50
40
30
Ba
La
Nd
Sm
Er Tm
Yb
Lu
Dy
Gd
Eu
Pr
Ho
Tb
70
60
50
40
30
794
771
748
725
702
679
656
633
610
587
564
541
518
495
472
449
426
10
403
20
10
380
20
138
143
148
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158
163
168
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178
Wavelength
Figure 1: An eight-parameter flow cytometry experiment illustrating the spectral overlap between the fluorochromes. Mass cytometry involves
the collection of mass spectral data in distinct channels with 1 amu space between each channel.
Figure 2: The periodic table highlighting the lanthanide-transition group of elements (pink),
the live-dead cell markers (dark grey), and the mass tag cell barcoding metal (light gray) used
in mass cytometry experiments. Rh, Ir, and Pt are used for the determination of cell viability in
mass cytometry, and Pd isotopes can be used for mass tag cell barcoding (MCB).
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Instrumental Components
The mass cytometer technology
(CyTOF 2, Fluidigm Corporation)
discussed in this column installment
consists of five major components
including sample introduction, the
inductively coupled plasma (ICP), the
ion optics and time-of-flight (TOF)
analyzer, and the detector. Sample in
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Spectroscopy 30(5) 17
Value
1500 W
17 SLPM
1.0 SLPM
~0.2 SLPM
~0.7 SLPM
0.045 mL/min
Direct in-line
low flow
TOF
76,800 spectra/s
Nebulizer gas
(~0.3 L/min)
Make-up gas
(~0.7 L/min)
Figure 3: The cell suspension is injected into the nebulizer as argon gas flows through the
nebulizer and spray chamber, carrying the sample to the ICP torch. A makeup gas is used to
optimize the plasma conditions independently of the optimization of the nebulizer gas, which
impacts the integrity of individual cells.
None
89209 amu
n Choose k
Barcode Scheme
k=3
10*
20*
* = n!/(k! [n - k]!)
To ICP torch
200 C
Liquid cell
suspension
(45 L/mL)
Torch
RF load coil
Vaporization
Plasma
Atomization
To interface
Figure 4: The vaporization, atomization, and ionization of cell droplets in the high-temperature argon
plasma. Cells are extracted through a vacuum interface on their journey to the TOF mass analyzer.
website: www.RigakuEDXRF.com
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Ionization
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(b)
(a)
(c)
(d)
(e)
(g)
Element
(h)
Element C
(f)
Element A
Figure 5: Mass cytometry workflow: (a) Cells labeled with metal-conjugated antibodies in
solution are injected into (b) the nebulizer. They are aerosolized and reduced to single cellcontaining droplets. (c) The cells are directed to the ICP torch, where they are vaporized,
atomized, and ionized in the plasma. (d) The high pass optic removes the low-mass ions and
the photons, resulting in an ion cloud that enters (e) the TOF mass analyzer. The ions are
separated based on their mass-to-charge ratio and are accelerated to the detector. (f) The
detector measures the quantity of each isotope for each individual cell in the sample; data are
generated in (g) an FCS format and (h) analyzed.
HSC MRP
CMP
Pro-B
Pre-B I
Pre-B II
Monoblast
NK NKT
Monocyte
Pro-monocyte
Pre-DC
GMP
Plasmacytoid DC
Myelocyte
Promyelocyte
CD38mid CD3- platelet
CD38- CD3- platelet
CD38mid CD3mid - platelet
Naive CD8+ T
Memory CD8+ T
Native CD4+ T
Memory CD4+ T
Immature B
Mature B
IL-3R + mature B
Plasma cell
Erythroblast
Erythrocyte
-16
16
Figure 6: The SPADE analysis of human hematopoietic cells in human bone marrow samples.
CD34 (shown here) was used to define the T-cell lineages. Adapted from reference 15 with
permission from Elsevier.
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Principles of Operation
The single-cells associated with the
specific isotope-tagged antibodies are
injected into the ICP and subsequently
vaporized, atomized, and ionized.
Figure 4 depicts the ICP and the
formation of ion clouds from individual cells stained with metal-labeled
antibodies. The particles in the
sample that are introduced into the
plasma are ionized to produce an ion
cloud. The ion cloud associated with
individual particles, which includes
the ionized metal tags that report on
the protein content of the cells, diffuses as it flows in the plasma. At the
point of extraction, the ion cloud is
approximately 2 mm in diameter and
is flowing at a velocity of approximately 10 m/s. The plasma is extracted
through a three-aperture plasmavacuum interface, such that the ion cloud
produces a transient pulse of cellassociated particles that is pseudoGaussian with a half width of ~200
s. After the ions are largely separated
from the un-ionized plasma gas, they
pass through a high pass optic that
transmits ions above ~80 amu that
are then directed toward the TOF
analyzer, wherein they are separated
according to their mass-to-charge
ratio. The signal from the detector is
digitized by an analog-to-digital converter (ADC) and the data in time are
converted to mass and integrated into
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Spectroscopy 30(5) 19
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RAMAN
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20 Spectroscopy 30(5)
May 2015
See the
Invisible...
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up to 20 different samples using barcoding while eliminating the doublets for rapid unbiased sample deconvolution. Table II shows the barcode scheme as applied to
mass cytometry.
Interpretation of Data
After the data have been collected and are ready for analysis there are several options for interpretation of mass cytometry data. Currently, two platforms are the most commonly used to support cytometry data: Cytobank (10) and
FlowJo (11). Data can be imported into Cytobank, and several forms of data interpretation can be carried out within
this platform. Cytobank provides users the ability to look
at large datasets in parallel. Researchers can manipulate,
analyze, and share these large datasets. FlowJo allows users
to manipulate datasets in a variety of ways: gate the data
and remove outliers, select from various types of graphs,
and change individual parameters. Users can isolate single
cell types from a population and then overlay bivariate
two-dimensional (2D) scatter plots of combinations of all
the parameters in the experiment.
Data collected from mass cytometry experiments contains extremely high dimensionality; therefore, supervised methods of data analysis may require significant
involvement of the data analyst. There are several methods
that researchers can use to interrogate data obtained in
mass cytometry experiments that are unsupervised and
hypothesis-generating (6). This type of computer-assisted
gating and clustering of populations may provide users
with a better view of the bigger picture. Lets review three
of the types of software used in recent publications: PCA,
SPADE, and viSNE.
PCA takes data collected with a large number of
variables for a single population and reduces it to a few
interpretable linear combinations. This condenses the dimensionality of the dataset to provide a low-dimensional
picture. This method was used by Newell and colleagues
(12). Metal-encoded tetramer probes were used to stain
human peripheral blood samples and these were examined
using 25 metal-labeled antibodies to cell differentiation
and signaling molecules. The subpopulations of CD8+
memory T-cells were gated by known surface marker phenotypes in CD8+ memory T-cells in human peripheral
blood samples. Data from subpopulations of cells was
clustered according to phenotypic and functional characteristics. The results of the study illustrated the diversity
of memory cells and the changes in expression levels of
markers as the cells transition from effector memory cells
to central memory cells.
Another example of algorithms that cluster larger cohorts of samples, SPADE, provides a platform to cluster
data in multidimensional space and reduce it to a 2D representation using the minimum spanning tree algorithm.
This methodology provides a means to extract hierarchical
data from high-dimensional mass cytometry analysis in an
unsupervised manner. The tool has been integrated into
both FlowJo and Cytobank and provides the ability to in-
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May 2015
Spectroscopy 30(5) 21
PIKE
Gas Cells
A World of Spectroscopy
Sampling Solutions
PIKE Technologies
www.piketech.com
tel: 608-274-2721
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22 Spectroscopy 30(5)
Final Thoughts
Mass cytometry builds on the capabilities of ICP-MS to exquisitely detect
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References
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MAGPRO
X-RAY SOURCE
MOXTEK
I N NOVATI NG S OLU TI O N S
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Accessories
Many of the improvements to existing instruments often
have to do with sample handling. Accessory manufacturers
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2014 PerkinElmer, Inc. 400298_01. All trademarks or registered trademarks are the property of PerkinElmer, Inc. and/or its subsidiaries.
ONE RUN
LETS YOU
SEE IT ALL
Nanoparticle concentration, composition, size and distribution,
dissolution and agglomeration tracking all in under a minute.
Nanoparticles unique characteristics and increasing usage in
consumer products will inevitably lead to their release into the
environment. Characterizing them required hours of analysis
time and manual calculations until now. Te NexION 350 ICP-MS single-particle
analyzer combines best-in-class data acquisition rates with proprietary sofware to deliver
full characterization in one run thats 60 seconds or less. Want to understand more from your
nanoparticle research? Just give us a minute.
www.perkinelmer.com/NexIONnano
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26 Spectroscopy 30(5)
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Milestone, Inc.
Newport
Ocean Optics
Ondax
PANalytical
PerkinElmer, Inc.
Photonis
Prism Analytical Technologies
Quantum Northwest
Questron
Real-Time Analyzers, Inc.
Rigaku Raman Technologies
RPMC Lasers
Savillex
SciAps, Inc.
Shimadzu Scientifc Instruments
Accessories
Components
Accessories, atomic, and UVvis
Raman
NIR and X-ray
Accessories, atomic, and UVvis
Accessories
Mid-IR
Accessories and UVvis
Accessories
NIR
Raman
Components
Accessories
Atomic
Atomic, mass spectrometry, and UVvis
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ZZZKRULEDFRPVFLHQWLF
email: adsci-specty@horiba.com
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Atomic Spectroscopy
The growth of laser-induced breakdown spectroscopy (LIBS) is a welcome trend in the atomic spectroscopy
field. The ability of lasers to generate
the analyte emission simplifies sample
preparation in many cases, even while
decreasing the total sample size needed
for the analysis. The limits on accuracy
and detection currently mean that
ICP, graphite furnace, and atomic absorption (AA) remain stalwarts in the
field and continued development of
these is visible in several new products
but LIBS is proving capable in handheld instruments and laboratory tools,
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Components
As part of the trend toward specialpurpose analyzers, we note that various
component suppliers are providing applications-specific building blocks. For
example, companies such as Attodyne,
RPMC, and Cobolt are showing a wide
array of lasers. Similarly, Andor and
Teledyne Judson are making detectors
available as a prominent part of their
product offerings and McPherson
provides spectrometer components.
Vendors can compile these blocks
into their interpretation of the market
needs, producing devices specific for
oil analysis and pesticides. Much of
the innovation in instrument design
involves incorporating these tools,
such as with electron-multiplying
charge-coupled devices (EMCCDs) and
specific lasers being built into Raman
spectrometers by a variety of vendors.
Although some special-purpose analyzers are being developed through
specialty instrumentation companies
(such as Real-Time Analyzers), others
are being developed by the component manufacturers (Ocean Optics) or
larger, general-purpose manufacturers.
We also saw a variety of other offerings from component suppliers. Avantes
is manufacturing a compact stabilized
halogen light source for visible to nearinfrared applications; Bayspec supplies
lasers of several different wavelengths;
Cobolt has lasers of various wavelengths
that offer direct intensity modulation
capability; JMScience lamps are manufactured using a new manufacturing
process that results in lower prices and
extended lifetimes; Newport supplies a
modular NIR, mid-IR, terahertz spectrometer engine; RPMC Lasers is promoting deep-UV lasers; and VUV Analytics has a vacuum ultraviolet (VUV)
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30 Spectroscopy 30(5)
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CEM
Corporation
Glass
Expansion
Product
Name
Measurement Mode
Discover SP-D
Gold
Microwave digestion
system
N/A
IsoMist XR
Programmable
temperature spray
chamber
N/A
N/A
N/A
T-SST
Guided Wave
Turbidity
Probe
Transpiration
Control
Technology
Vapor probe
Transfectance
single-sided transmission
process probe
Turbidity probe
Stabilized certifed
reference standards
Transmission, 90
backscatter
Milestone,
Inc.
Ocean Optics
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N/A
Monolithic diamond
ATR accessory
ATR
IRT5000/7000
Series
FT-IR microscopes
Transmission
Spinsolve
Reaction
Monitoring
Kit
Automatic sample
handler
N/A
N/A
Jasco
Magritek
G-SST
Inorganic
Ventures
Product Type
Ethos UP
Microwave digestion
system
SERS
Substrates
SERS substrates
Spirit
Sampler
Beverage brand
recognition and
authentication system
N/A
ADV
How to excel ?
ask@panalytical.com - www.panalytical.com/zetium
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Photonis
Quantum
Northwest
Product
Name
Spotlight
150i and
Spotlight
200i
Ion Beam
Imaging
Profler
Product Type
Microscope
qCHANGER 6
Automatic sample
handler/sample cell
holder/controller
QLab Pro
Sample preparation
apparatus
QPrep
Sample preparation
apparatus
Measurement Mode
N/A
N/A
N/A
N/A
N/A
N/A
N/A
N/A
N/A
N/A
Questron
Fume
Scrubbing
System
Vulcan
C-Flow
Fume scrubber
Sample preparation
apparatus
PFA nebulizer
Savillex
PFA Cyclonic
Spray
Chamber
Specac Inc.
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Atlas
Autotouch
Spray chamber
Hydraulic press
ADV
2015 HARRICK SCIENTIFIC PRODUCTS, INC. ALL RIGHTS RESERVED. ILLUSTRATION: ISTOCK.COM/MAIRGIOLD88
Scientific Products
the
NEXT
GENERATION
ConcentratIR2
>>>>>>>>
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harricksci.com/ConcentratIR2
ADV
34 Spectroscopy 30(5)
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May 2015
Spectral
Systems LLC
Spex
Certiprep
Starna Cells
StellarNet
Product
Name
ArmIR
Product Type
Measurement Mode
Transmission
30 mL ICP
and ICPMS Single
Element
Standards
Standards
ICP and
ICP-MS
Starna FTIR
Polystyrene
Wavelength
Reference
Material
Standards
Mid-IR
reference
material
Starna USP
<857> UV
Qualifcation
Kit Standards
Standards
UV reference standards
StellarScope
Fluorescence
Fluorescence
spectrometer-tomicroscope
Fluorescence microscopy
StellarScope
Raman
Raman spectrometer-tomicroscope
Refection
ASX-560
Automatic sample
handler/preparation unit
N/A
N/A
ATR
ATR
TGA
N/A
Teledyne
CETAC
MVX-7100 L
Thermo
Fisher
Scientifc
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Workstation
Thermo
Scientifc iD7
Accessory
FT-IR spectrometer
ATR accessory
Thermo
Scientifc
Smart iTX
Accessory
FT-IR spectrometer
ATR accessory
Thermo
Scientifc
TGA-IR
Module
Verder
Scientifc, Inc.
EMAX
Thermogravimetric
analysis (TGA)
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Mass Spectrometry
Seven manufacturers presented new MS
May 2015
Spectroscopy 30(5) 35
Product Name
Product Type
Measurement
Mode
NanoLIBS
LIBS analyzer
LIBS
i-Libs
LIBS analyzer
LIBS
Same as above
FluoroMax Plus
Spectrofuorometer
N/A
Ultima
Fluorescence
lifetime system
Fluorescence,
TCSPC (timecorrelated single
photon counting)
Flame
Spectrometer
UVvis fame
spectrometer
N/A
Spark-VIS MicroSpectrometer
UVvis sparkmicrospectrometer
N/A
PinAAcle 500
AAS
Z-100
LIBS
Laser ablation
Horiba Scientifc
Ocean Optics
PerkinElmer, Inc.
SciAps, Inc.
ICPE-9800 Series
SPECTRO Analytical
Instruments
StellarNet
SPECTRO ARCOS
PortaLIBS
Fluorescence
spectrofuorophotometer
Fluorescence
N/A
LIBS
Shimadzu Scientifc
Instruments
RF-6000
High-resolution
ICP-OES
spectrometer
LIBS
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Product Name
Product Type
Measurement
Mode
Shamrock 193i
Motorized and
modular
Czerny-Turner
spectrograph
Transmission,
absorption,
refection, and
scattering
193-mm focal length, adaptive focus, dual-grating turret with RFID technology, astigmatism-corrected optical
design, dual detector outputs, USB interface, silverprotected coated optics option.
Zyla HF
Attodyne Lasers
Motorized
spectrograph
Motorized
spectrograph
Transmission,
absorption,
refection,
scattering and
diffraction
N/A
<10 ps pulses, up to 4 W with over 150 J of pulse energy, long term power stability <1% noise, high beam
quality with M2 <1.3, trigger 01 Mhz, serial interface,
compact optical head, fully detachable control unit, up
to 10-m umbilical, air cooling, >20,000-h lifetime, available in 1064-, 532-, and 355-nm versions.
N/A
APL Series
Picosecond lasers
AvaLight-HALS-Mini
Halogen light
source
FX (Fixated)
Form-holding
fber-optic
jacketing
N/A
RamSpec OEM
Raman
scattering
Cobolt MLD
633-nm laser
633 nm, up
to 80 mw,
TEM00
All Cobolt MLD lasers feature direct intensity modulation capability and can be modulated up to 150 MHz
with up to 10,000,000:1 extinction ratio. Manufactured
to ensure reliability and robustness. The 06-01 Series
offers a standardized compact form factor and a wide
wavelength span in a plug-and-play format.
Cobolt MLD
647-nm laser
647 nm, up
to 120 mw,
TEM00
Same as above
Cobolt
Flamenco
660-nm laser
660 nm,
TEM00
Same as above
Cobolt Jive
561-nm laser
561 nm,
TEM00
Same as above
Cobolt Samba
532-nm laser
532 nm,
TEM00
Same as above
Lamps
Lamps
Atomic, UV
vis spectroscopy
These lamps are manufactured using a new manufacturing process that results in lower prices and extended
lifetimes. The lamps are available for several instrument
manufacturers.
Standoff
detection
Avantes
BaySpec
Cobolt
JMScience
McPherson
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Tunable UV
Raman Filter
Tunable UV
Raman flter
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Spectroscopy 30(5) 37
Product Name
MIR8035
Product Type
Modular NIR,
mid-IR, terahertz
spectrometer
Newport
Light source
power supply
OPS series
Tunable Light
Source (TLS)
"LUV" series:
Light intensity
controller
266280 nm
CW laser sources
Measurement
Mode
Flexible
N/A
N/A
TLS Series wavelength-tunable sources deliver up to 0.7nm resolution of monochromatic light from 250 nm to
2400 nm. These are designed for researchers who need
the fexibility of a modular design with the simplicity
of an integrated system. Requires no setup. Simple and
compact design ensures an economical price.
N/A
Compact deep UV source, monolithic cavities technology, inherently stable and robust to vibrations. 10 mW
of continuous wave optical power for the 280-nm LUV,
up to 20 mW of CW power, single mode collimated
beam, power adjustment 0% to 100%, USB computer
interface, multimode fber coupling option; beam
diameters available: 0.3, 0. 6, or 0.8 mm.
N/A
N/A
N/A
N/A
RPMC Lasers
Lapa-80
Teledyne/Judson
DPSS laser
Enhanced
Detector
DLP2010NIR
Integrated LWIR
HgCdTe + lens
Texas Instruments
DLP NIRscan
Nano evaluation
module (EVM)
VUV Analytics
VGA-100
Out-of-box
development tool
for prototyping
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See Table V and the on-line information for more details about these
products.
Mid-Infrared
While most IR vendors, such as Bruker,
Jasco, Thermo Fisher, and PerkinElmer,
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Product Name
1st Detect
iONTRAC
BaySpec
Process monitor
mass spectrometer
Chemicals to be monitored or potential threats and contaminants can be preprogrammed and the abundances
reported in real time. Unlike other process analyzers, the
MS or GCMS ion trap mass analyzer allows the iONTRAC to always
measure an entire stream or environment so that data are
always available to excursion events and to determine the
presence of unanticipated contaminants.
MS with electron ionization (EI) ion
source and
FAPA (plasma)
ionization
probe.
Mass
spectrometer
MA3100
Ion mobility
spectrometer
(HPIMS) add-on
for Thermo
Scientifc mass
spectrometers
Ion mobility
drift time
(fight time)
GA2100
Mobile highperformance
ion mobility
spectrometer
Ion mobility
drift time
(fight time)
Compact SIMS
Workstation
Mass
spectrometer
N/A
PTR-QiTOF
Mass
spectrometer
PTR-TOF 1000
TOF mass
spectrometer
SFESFCMS
IONICON
Analytik
Shimadzu
Scientifc
Instruments
Measurement
Mode
Portabiltiy
Excellims
Corporation
Hiden Analytical
Product Type
Nexera UC
Unifed
chromatography
SFESFCMS
system
Waters Xevo
G2-XS QTof
TOF mass
spectrometer
N/A
Xevo TQ-S
micro
Quad MS
N/A
Waters Full
Spectrum
Molecular
Imaging System
Imaging mass
spectrometer
N/A
Waters
Corporation
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Spectroscopy 30(5) 39
Product Name
LaserSense
Product Type
Measurement
Mode
QCL mid-IR
spectrometer
Block
Engineering
LaserWarn
Open-path
chemical
detection
system
Open-path
IR absorption
spectroscopy
LUMOS
FT-IR
microscope
Transmission,
refection,
and ATR
Mid-IR/far-IR
spectrometer
Transmission,
refection,
and ATR
An FT-IR spectrometer covering the mid and far infraredTHz spectral ranges in one step. Bruker offers a new
wide range MIR-FIR DLaTGS detector as well as a mid-IR/
far-IR beamsplitter. Together, these form the basis of the
unique VERTEX FM FIR-MIR extension for the VERTEX 70
and VERTEX 70v vacuum systems, which cover 6000 cm -1
down to 50 cm -1 in one step without any beamsplitter or
detector change.
FT-IR
spectrometers
Transmission,
ATR, diffuse
refectance,
specular
refectance,
grazing-angle
refectance,
refection
absorption,
photoacoustic
GCIR:
transmission
in gas cell
Bruker Optik
GmbH
VERTEX FM
Jasco
FTIR-4000/6000
Series
Prism Analytical
Technologies
MAX
Mid-IR
spectrometer
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NIR
Application specificity in NIR historically
has been achieved via the calibration model,
in contrast with most other technologies
that use custom or dedicated hardware.
NIR vendors are now also coming to the
use of dedicated hardware as well as software and calibrations. For example, ABB is
providing a precalibrated unit for crystallinity in polyethylene terephthalate (PET)
bottles. Art Photonics has an instrument
designed to measure and control moisture
in media. Bruker has a unit for precise measuring of weight, thickness, diameter, and
hardness of tablets that is fully compliant
with current United States Pharmacopeia
(USP) and European Pharmacopoeia (EP)
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40 Spectroscopy 30(5)
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Art Photonics
Avantes
Product Name
Product Type
Measurement
Mode
MB3600-CH80
PET packaging
analyzer
Transmission
MoiSens
NIR spectral
fber moisture
sensor
AvaSpecNIR-HSC
NIR
spectrometer
Tandem IIIA
FT-NIR
spectrometer
TANGO
FT-NIR
spectrometer
i-Spec Plus
NIR
spectrometer
Bruker
Optik GmbH
Guided Wave
NIR-O
MicroNIR
PAT
JDSU
PANalytical
(ASD Inc., a
PANalytical
company)
Real-Time
Analyzers, Inc.
Si-Ware Systems
StellarNet
NIR
spectrometer
NIR
spectrometer
This instrument is designed to measure and control moisture in media. Implemented with rapid scan of specifc
Transmission LED wavelengths to illuminate media and collect signal
and refection from either diffuse refection or transmission mode. Mode
selection is determined by media type using Trans-Flex or
diffuse refection fber probe for selected media.
Refection
Transmission
Refection
N/A
Portable
spectrometer
A truly portable full-range, handheld, compact spectrometer. Features integrated internal light source, on-board
GPS, voice audio recorder, internal white reference,
lightweight rechargeable batteries, automated internal
wavelength validation, integrated computer and LCD with
push-button navigation, and a PC-based project and data
management software ecosystem.
QualitySpec
Trek
NIR
spectrometer
Benchtop
Fuel Quality
Analyzer
NIR fuel
analyzer
Transmission
Portable
Fuel Quality
Analyzer
NIR fuel
analyzer
Transmission
NeoSpectra
(Generation:
SWS62221)
NIR
spectrometer
Transmission
or diffuse
refectance
probes can be
attached
StellarCase NIR
NIR
spectrometer
Refection
Compact core sensing module, low cost embedded solution, designed for high volume production, semiconductor
manufacturing, wide spectral ranges, fast data processing,
alignment-free optics, operation in harsh environment,
and selectable resolutions and scan time.
A rugged and fully integrated portable case system for
material identifcation and composition analysis. Interior
spectrometer instrumentation preconfgured for open
and measure application. With a press of the Analyze
button match results or sample percent composition can
be displayed on the screen instantaneously.
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Spectroscopy 30(5) 41
Product Name
Product Type
Measurement
Mode
Aspect Imaging
AI-60
High-resolution
NMR system
NMR
SpinPulse CX-20
Time-domain
NMR
NMR
Cosa Xentaur
Corporation
Thermo Fisher
Scientifc
PicoSpin
Reactionmonitoring
accessory for
benchtop NMR
trometer. StellarNet has a system for material identification and composition analysis,
which can also be preconfigured for open
and measure application.
See Table VII and the on-line information for more details about these products.
NMR
Nuclear magnetic resonance (NMR) spectroscopy has not been prominent at Pittcon
for several years. Indeed, in some years,
general scouting of the exhibit floor did not
reveal any manufacturers of NMR instruments. However, recent advances in magnet
technology have enabled manufacturers to
replace the huge electromagnets of yesteryear with (relatively) small, permanent
magnets with suitable characteristics (uniformity) to allow the NMR measurement
to be (relatively) easily moved from one site
to another, thereby making it portable
(though this does not quite meet the definition of portable as defined above as not
needing a truck).
NMR is going through some major
changes. With the withdrawal of a major
player in the high-field magnet sector (Agilent), most of the development and change
is coming in the small, benchtop, or fixedmagnet arena, almost a diametric shift
back to the roots of NMR. A number of
vendors, such as Thermo Fisher, Magritek,
and Anasazi, provide small NMR units. A
common theme this year is cryogen free,
while competition is developing around
carbon-13 capabilities and reaction monitoring. Unfortunately, only two vendors
responded to our request for detailed information about their units for this review,
so we cannot present examples of all the
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capillary
system
Raman
Developments in Raman spectroscopy were
prevalent at this years Pittcon. Raman vendors showed an array of new tools covering
different aspects of the applications space.
Several companies provide instruments
that adapt to existing microscopes.
Bayspec has the worlds first dual-band
portable Raman instrument, as well as
a high-resolution dispersive 1064-nm
Raman spectrometer. Bruker uses sequentially shifted excitation to minimize
fluorescence interference. B&W Tek has a
portable Raman spectrometer with a high
quantum efficiency cooled (25 C) CCD
array detector. Edinburgh Instruments
offers its Nanosecond Transient Absorption spectrometer, which features several
alternate measurement modes including
LIBS. Jasco has a Raman instrument for
temperature- or atmosphere-controlled
measurements. Metrohm provides the
only handheld Raman instrument in the
market with a laser class I safety feature.
Ondax uses a 976-nm source for reduced
autofluorescence. Rigaku eliminates fluorescence interference by using 1064-nm
excitation. TechnoSpex Pte. Ltd. integrates
Raman spectroscopy into existing upright
Software
This years review includes software products from seven companies. ACD Labs
provides a single interface for delivery of
multitechnique analytical results, with automatic capture of raw data. Autoscribe
Informatics, Inc., has a workflow generator and recorder. CAMO, Inc., provides
a software package for modeling and
monitoring of batch processes or systems
with time dependency. CEM has software
that allows wireless real-time monitoring
and instrument control from outside the
laboratory. Fiveash Data Management
(FDM) can provide a Raman library of
more than 200 multicomponent sets of
ATR spectra of drugs (including drugs
of abuse) in one spectral library as well as
more than 845,000 two-component ATR
spectra. Horiba has a spectroscopy suite
for Horiba Raman microscopes that has
several add ons available. Magritek also
has new software for its Spinsolve NMR
spectrometer.
See Table X and the on-line information for more details about these products.
UVVis
UVvisible spectroscopy is one of the most
mature of the common spectroscopic technologies. Nevertheless, 17 manufacturers
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BaySpec
BioTools
Product Name
Product Type
Measurement
Mode
Dual-band
Agility
Raman
analyzer with
active trigger
probe
Raman
scattering
The worlds frst dual-band portable Raman instrument, enabling users to measure real-world samples. Measurements
can be conducted in a light tight chamber using liquid vial,
solid down, solid side, solid up, rotating, or fber-optic probe.
RamSpec-HR
1064-nm
Raman system
1064-nm
laser Raman
MovingLab
Dual band
portable
Raman
microscope
532-, 785-,
and 1 064-nm
laser Raman
-BioRAMAN
and Mobile-Raman
Raman
spectrometer
Raman
scattering
BRAVO
Raman
spectrometer
Dispersive
Raman
scattering
i-Raman Pro
Raman
spectrometer
Raman
scattering
LP980
Nanosecond
transient
absorption
spectrometer
Transient
absorption,
laser-induced
fuorescence,
LIBS, and
Raman
measurements
Bruker Optik
GmbH
B&W Tek
Edinburgh
Instruments
Jasco
Metrohm
Raman
scattering,
temperature
Raman
NRS-4100 Series spectrometers
or atmosphere
controlled
measurements
Metrohm
Instant Raman
Analyzer
Mira
Ondax
THz-Raman
Microscope
System
Rigaku
Progeny ResQ
TechnoSpex
Pte. Ltd.
uRaman
Thermo Fisher
Scientifc
Gemini
HyperFlux PRO
WITec GmbH
apyron
A frst of its kind on the market, the LP980 allows for the measurement of transient absorption, laser-induced fuorescence
and phosphorescence, Raman spectroscopy and LIBS all in one
instrument.
The Mira Basic package with the vial holder is the only handheld Raman instrument in the market with a laser class I safety
feature. The Mira packages offer three quick-change inserts,
Raman
which can be rapidly exchanged within the base system. FeaRaman
refectance
and scattering tures an integrated vial holder, samples are inserted in small
vials that are then simply inserted into the Mira spectrometer
for measurement.
A 976-nm source for reduced auto-fuorescence, avoiding the
need for InGaAs detectors. Using the TR-MICRO-976 and XLFCLM-976 to deliver clear low-frequency Stokes and anti-Stokes
Confocal
Confocal
spectral analysis over a range of 5500 cm-1 when used with
Raman
Raman
microscope
conventional Si detector-based spectrographs, enabling reliable identifcation of molecular structure characteristics of
fuorescent materials.
1064-nm
excitation measures colored solids and liquids as well
Handheld
substances through containers, eliminating fuorescence
with optimal as
Raman
interference. Offers the industrys most comprehensive library
docking
spectrometer
with over 12,000 compounds including CWAs, explosives, TIC
station
and TIM, and narcotics.
Integrates Raman spectroscopy into existing upright microscope functions: DIC, phase contrast, dark feld. All compact
and affordable. Multiple wavelength, stackable module; giving
Raman
Raman
users the fexibility to connect to the different types of detecspectrometer
scattering
tors via optical fber cable. The spectrometer may range from a
compact to a high-end research-grade spectrometer.
ATR and Ra- The frst and only handheld integrated Raman and FT-IR
Handheld Raman and mid- man scatter- instrument.
ing
IR analyzer
The HyperFlux PRO is anon-line and at-line process Raman
Raman
Transmission analyzer designed for real-time, remote, and unattended
spectrometer
operations.
Automated
Raman
imaging
Refection
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Spectroscopy 30(5) 43
Product Name
Product Type
Measurement
Mode
ACD/Labs
Solution for
Open Access
Labs
N/A
N/A
Matrix Gemini
LIMS Builder
Workfow
generator and
recorder
N/A
CAMO
Software
Unscrambler X
Batch modeling
engine
N/A
iLink for
MARS6
Networking for
MARS6 microwave digestion
systems
N/A
ATR spectral
Library
N/A
ATR spectral
library
N/A
FDM ATR
Polymers
Germanium
N/A
FDM Software
Development
Kit
N/A
The FDM SDK is a tool for instrument companies to implement spectral library search features directly into their FT-IR
and Raman software packages. The SDK provides functions
for searching spectra and chemical names from all of the
FDM FT-IR and Raman spectral libraries. Eight algorithms
are available. Source code examples are provided.
LabSpec 6
Spectroscopy
suite for Horiba
Raman microscopes
N/A
LabSpec 6.3 is an upgrade to Horiba Raman systems. Optional add-on modules: ParticleFinder, multivariate analysis,
3D volume and surface rendering, database searching, and
multiwell.
SWIFT V.2
Imaging module
for Horiba
Raman microscopes
N/A
SWIFT v2 module allows user to obtain confocal Raman images with the click of a button. It is an alternative to optical
imaging techniques and can be used to survey 3D sample
structures and surface features. SWIFT is suitable for use
with all lasers from UV through to near infrared on Horiba
Scientifc Raman instruments.
Spinsolve
Expert
NMR software
N/A
ACD/Labs
CEM
Corporation
Fiveash Data
Management,
Inc. (FDM)
Horiba
Scientifc
Magritek
N/A = not applicable
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B&W Tek
CEM
Corporation
Product Name
Exemplar Pro
iFlash
Product Type
UVvisNIR
spectrometer
Flash
photometer
Measurement
Mode
N/A
A UVvis spectrometer utilizing a low stray light CzernyTurner spectrograph, with a cooled (25 C), high quantum
effciency, back-thinned (BT) CCD detector. It also features a
built-in shutter allowing for dark scan measurements even
while illuminated. It can provide spectra over the entire
1901100 nm spectral range
N/A
GratingWorks
Concavus
Dual beam
UVvis
spectrometer
A dual-beam version of the previous Concavus spectrometer. Spectral resolution is 0.22 NA, and athermal characTransmission teristics of less than 0.15 nm wavelength shift over 1050 C
and
temperature range. The dual-beam spectrometer compenrefectance sates lamp intensity fuctuation in real-time. The system
uses a single concave grating for both beams and exhibits
very low stray light. Can be customized for OEM use.
Hanby
Petroanalysis
Hydrocarbon
ID
UVvis
spectrometer
Absorbance
Refectance
Headwall
Photonics, Inc.
Industrial
Test Systems
NanoHyperspec
eXact iDip
Imaging
spectrometer
V-700 Series
UVvis spectrophotometers
Transmission, diffuse,
and specular
refection
TIDAS S MSP
Hyperspec
UVvisNIR
spectrometer
Transmission,
refectance,
and
fuorescence
Fast scanning by coupling to camera,provides the combination of spectral data with spatial information. Adaptability
with nearly any model microscope opens a wide feld for
applications in life and material sciences.
Clean Monitor
Process
Technology
UVvis
spectrometer
with RVP
fowcell
In-line UVvis spectroscopy for rinse monitoring of clean-inplace (CIP) processes with reproducible variable path (R.V.P.)
fowcell. This in-line CIP analyzer provides quick feedTransmission length
back, reduces dead-time, and ensures optimal cycle times,
thereby saving costs. High sensitivity and fast response time
allow the monitoring of cleaning processes in real time.
Deep UV
Luminescence
Spectrophotometer
Deep UV
luminescence
spectrophotometer
Transmission,
refection,
fuorescence,
luminescence,
and phosphorescence
Ocean Optics
STS
Developers Kit
Developer's kit
for laboratory
analysis, process
applications,
and handheld or
portable use
N/A
PerkinElmer,
Inc.
LAMBDA
265/365/465
UVvis
spectrometers
N/A
Jasco
J&M Analytik
McPherson
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Spectroscopy 30(5) 45
Product Name
Product Type
Measurement
Mode
PAS 1010
Pulsed-laser
photoacoustic
spectrometer
Pulsed-laser
photoacoustic spectroscopy
UV-1280
Simultaneous
ICP and atomic
emission
spectrometer
UV-3600 Plus
UVvisNIR
spectrophotometer
Quantum
Northwest
Shimadzu
Scientifc
Instruments
N/A
PSR+
Field-portable
UV-vis
spectrometer
Refectance,
absorption,
transmission, and
direct energy
(radiance and
irradiance)
SR-1901PT
spectroradiometer
Spectroradiometer
Irradiance
UVvisNIR
spectrophotometer
N/A
UV-470-151
spectrometer
UVvis
spectrometer
Transmission,
refectance,
absorbance,
color measurement,
emission, and
fuorescence
StellarNet
SILVER-Nova
UVvis
spectrometer
Absorbance,
transmission,
refectance,
and radiometery
Tec5USA Inc.
Multichannel
Spectrometer
System
Integrated UV
visNIR spectrometer system
and fber-optic
switch
Spectral
Evolution
SR-4500
spectroradiometer
Spectrum
Scientifc Inc.
N/A
a spectral curve or fingerprint of the hydrocarbon; this system combines the concept
of a dedicated analyzer (a trend discussed
above) with the concept of an automated
analyzer. Headwall Photonics, Inc., has a
completely integrated VNIR (4001000
nm) hyperspectral sensor. Industrial Test
Systems had the first photometer in the
water quality testing market to provide twoway wireless connection. Jasco showed its
new V-780 UVvisNIR instrument with a
single monochromator, dual-grating, dual-
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detector design, and an InGaAs NIR detector, which is part of a five-instrument set of
distinct models. J&M Analytik showed fast
scanning by coupling to a camera. McPherson showed deep UV spectrophotometry,
as well as VUV excitation and broadband
emission measurement capability. Ocean
Optics, instead of an instrument, showed
its spectral sensing platform essentially
a developers kit containing simple tools for
integrating spectroscopy into your system.
PerkinElmer has a family of benchtop-
ADV
46 Spectroscopy 30(5)
w w w. s p e c t r o s c o p y o n l i n e . c o m
May 2015
Product Name
Product Type
Applied Rigaku
Technologies,
Inc.
NEX QC
QuantEZ
Energydispersive X-ray
spectrometer
Measurement
Mode
EDXRF
EDAX, Inc.
XLNCE
SMX-BEN
X-ray
spectrometer
N/A
Nondestructive coating thickness measurement technology. Features include: an array of choices for X-ray optics
and primary flters; the latest generation of silicon drift
detectors; analysis software platform for empirical and
fundamental parameters (FP) analyses and a large analysis
chamber with motorized X-Y-Z sample stage.
PANalytical
Zetium
XRF
N/A
SPECTRO
xSORT Alloy
Handheld XRF
spectrometer
N/A
N/A
Designed for advanced metals analysis. Features new topof-the-line silicon drift detector (SDD), the xSORT Alloy
Plus provides reliable, high-productivity measurement and
analysis. Obtain metal grade analysis in only 2 s for most alloys; 10 additional seconds to sort light elements such as
magnesium, aluminum, silicon, phosphorus, and sulfur.
N/A
SPECTRO
Analytical
Instruments
SPECTRO
xSORT Alloy
Plus
Handheld XRF
spectrometer
SPECTRO
xSORT
Non-Alloy
Handheld XRF
spectrometer
X-ray
Unfortunately, neither of us is an expert in
X-ray technology or its applications. Further, there are only four manufacturers that
contributed to our review, so we have little
basis for comparisons or detecting trends.
All we can realistically do is to present the
information we obtained and allow those
of our readers who have the necessary expertise to evaluate the instruments. They
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On-Line Appendixes
Additional product details appear online in the appendixes, at www.spectroscopyonline.com/2015-review:
Appendix I: Accessories
Appendix II: Atomic spectroscopy
Appendix III: Components
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ADV
48 Spectroscopy 30(5)
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May 2015
An Interlaboratory Comparison
Study for the Determination of
Arsenic and Arsenic Species in
Rice, Kelp, and Apple Juice
An interlaboratory comparison study for the measurement of arsenic species in rice, kelp, and
apple juice was carried out. The purpose of the study was to enable participating laboratories
to evaluate their analytical capability to determine inorganic arsenic, arsenite, arsenate, monomethylarsonic acid, and dimethylarsinic acid, assess the intercomparability of the data generated, and look for any correlation trends between the results and the analytical procedures
used. Approximately, 66% of laboratories achieved an overall score of 3 (good) or 4 (outstanding), based on the absolute Z-value statistical analysis procedure, indicating that there was generally good agreement between the labs reporting arsenic speciation data for food matrices.
However, only 15% of laboratories achieved an overall score of 4, which could be indicative
that further method development needs to be carried out to achieve a higher level of consistency across multiple laboratories worldwide using different analytical procedures.
Michelle L. Briscoe, Tamas M. Ugrai, Joel Creswell, and Annie T. Carter
his interlaboratory comparison study for the determination of arsenic and arsenic species in rice, kelp, and
apple juice was initiated to provide a reliable means
for laboratories to evaluate their competency in the analysis of arsenic species in these matrices, as well as a metric
for assessing the intercomparability and validity of the data
generated by different laboratories. An additional objective
of the study was to look for any correlation trends between
the matrices analyzed, species determined, and the analytical
procedures used by the different participating laboratories.
The study materials included white rice flour, brown rice
flour, kelp powder, and apple juice. Participants were asked to
analyze the samples for arsenic (As) species using the methods that are commonly used in their laboratory. Participants
were asked to report results for as many of the following analytes as possible, based on their analytical methodology: total
As in the sample, total arsenic in the speciation extract (if
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May 2015
Spectroscopy 30(5) 49
Solvent
reservoirs
Vacuum degasser
Column
oven
-
Autosampler
Column
LC pump
Sample
introduction
ICP-MS system
Computer
25,000
AsB
DMA
As(III)
Response (counts/s)
20,000
MMA
15,000
10,000
As(V)
5000
200
400
600
800
1000 1200
Retention time (s)
1400
1600
1800
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Process
Control
Process
Development
Process
Trending
Production,
Pilot Or Lab
tornado-spectral.com
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Get to Know
Metrohm
Titration
50 Spectroscopy 30(5)
120%
100%
80%
60%
40%
20%
0%
White rice
As(III)
Ion Chromatography
Brown rice
As(V)
(a)
(b)
10
5
Number of labs
2
1
Mean score
nm
(d)
15
Number of labs
Number of labs
15
(c)
Number of labs
20
Spectroscopy
Process
DMAs
Juice
AsB
Figure 3: The mean arsenic speciation results for each matrix as a fraction of the total arsenic in the extract.
Electrochemistry
Laboratory
Kelp
MMAs
10
5
0
2
1
Mean score
nm
16
14
12
10
8
6
4
2
0
2
1
Mean score
nm
2
1
Mean score
nm
15
10
5
0
Figure 4: Numbers of laboratories per mean score for the four samples studied. Note: nm = not
measured.
Table I: Details of the sample preparation methods used to determine total As
Number of
Labs
% of Total Labs
Microwave digestion
27
71
Hotblock or hotplate
21
Other
Table II: Details of the sample preparation methods used to determine total As
www.metrohm.com
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Number of Labs
% of Total Labs
ICP-MS
35
92
HGFAA
HR-ICP-MS
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May 2015
Spectroscopy 30(5) 51
Inorganic As
As(III) arsenite
As(V) arsenate
MMA monomethylarsonic acid
DMA dimethylarsinic acid
Other arsenic species, such as AsB, or unknown arsenic
species were also reported by some laboratories.
All results were reported to an independent third party,
EcoChem, Inc., which is a data validation company that had
no role in the study other than data management. At EcoChem, the dataset was compiled, and a unique identifier was
assigned to each laboratory before it was transmitted to Brooks
Rand Labs. Following the release of the study results (6), each
participating laboratory received its own unique identifier, but
identifiers were not disclosed to any other parties, including
Brooks Rand Labs. This research design ensured there would
be no bias by the preparers of this report against any participating laboratory and that participants could submit data with
the comfort of anonymity.
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52 Spectroscopy 30(5)
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Number of Labs
% of Total Labs
HNO3 extraction
26
63
H2O extraction
HCl extraction
Methanol extraction
Other
15
n choose k
Barcode Scheme
k=3
4 (excellent)
0.000.50
3 (good)
0.511.00
2 (acceptable)
1.011.50
1 (poor)
1.512.00
0 (unacceptable)
% of Total Labs
HPLC
37
90
HG-CT-GC*
25
Other
20
Number of labs
Number of Labs
Number of Labs
% of Total Labs
37
90
HG*-AAS
HG-AFS
HG-ICP-MS
15
10
5
0
2
Mean score
As. Tables III, IV, and V give a breakdown of the As speciation extraction,
separation, and detection methods,
respectively.
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Z = |(X M)|/F
May 2015
Spectroscopy 30(5) 53
[1]
and
800,000
F = Q/1.349
[2]
700,000
where Z = the absolute Z-value assigned to each result for the purpose
of assigning a rating; X = the reported
value; M = the median value reported
by all laboratories (excluding values
below the reported detection limit); F
= the F-pseudo-sigma (approximates
the standard deviation of traditional
statistics when the data has a Gaussian
distribution); calculated by dividing the
interquartile range (or fourth-spread) by
1.349. The 1.349 value is derived from
the number of standard deviations that
encompasses 50% of the data; and Q =
the interquartile range (the difference
between the first quartile and third
quartile of a set of data).
Participating laboratories were requested to report undetected (u) values
as being less than their detection limit.
600,000
The next
Overlap of AsB/DMA/As
As (V)
500,000
400,000
300,000
200,000
MMA
100,000
0
200
200
200
200
200
200
1400
Figure 6: Chromatogram of the separation of different arsenic species on an ESI CF-Cr-01 column,
showing the AsB, DMAs, and As(III) being coeluted (chromatogram provided by unidentified
participating laboratory).
EVOlutionary step
for spectrometry
Gigabit Ethernet
More memory
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ADV
54 Spectroscopy 30(5)
May 2015
Analytical Results
The results reported by each laboratory for each of the material types can be found in the final Brooks Rand Labs report
(6), along with the median (M) value, the mean value, the Fpseudo-sigma (F) value, and number of laboratories reporting results above their detection limit (n) for each parameter.
The complete data set will not be reported in this article,
but a summary of the M values for each analyte are listed in
Table VII. Values in parentheses were associated with F values that were greater than the M values, or with datasets with
less than seven results; therefore, the variability in the data
was too high or the number of results was too small to use
Starna Cells
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w w w. s p e c t r o s c o p y o n l i n e . c o m
Participating Laboratories
Of the 47 laboratories that agreed to participate in this study,
46 of them received the study materials; one laboratory in
Mexico was not able to import the materials. Of the 46 laboratories that received the study materials, 41 datasets were
received from 39 laboratories (two laboratories reported data
by two methods). The list of the participating laboratories
can be found in the final report. Of the participating laboratories, only 11 laboratories reported all of the requested
parameters in every material type. Nearly half of the laboratories (20 out of 41) did not report results for both total
arsenic in the sample and total arsenic in the extract; therefore, extraction efficiencies for those laboratories could not
be calculated. In fact, four of the laboratories (numbers 6, 19,
26, and 27) did not report any total arsenic data.
Of the 39 participating laboratories, approximately onethird of them were from outside of North America. Of the
North American participants, all were from the United
states, with the exception of one laboratory from Canada.
Of the laboratories from the United States, nine (38%) were
private commercial or industry testing laboratories, eight
(33%) were state laboratories representing seven states, five
(21%) were laboratories associated with the U.S. Food and
Drug Administration (FDA), and two (8%) were university
laboratories. There were eight participating laboratories from
Europe (21%) representing five countries. In addition, there
were four participants from Asia and one each from Australia and New Zealand. Table VIII summarizes the regional
participation in this study.
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May 2015
Spectroscopy 30(5) 55
Extraction Efficiency
For the determination of arsenic species
in any solid food matrix, a successful
extraction method must meet three important criteria:
It must be capable of extracting all the
arsenic species from the matrix.
It must preserve both oxidation and
complexation states, unless only the
inorganic species are of interest.
It must be able to produce a solution
that is compatible with the separation
s mplify.
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56 Spectroscopy 30(5)
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160
Extraction efciency (%)
140
120
100
80
60
40
20
0
12 27 31 08 38 25 05 04 26 24 33 32 16 21 23 30 22 35 29 01 39 14 36 07
Laboratory number
Methanol extraction
H2O extraction
Enzymatic extraction
HNO3 extraction
Figure 7: The mean extraction efficiency for total arsenic in the solid samples (rice and kelp
samples), with extraction methods indicated by pattern and the mean extraction efficiency
indicated by the solid black line.
As(V)
60
As(III)
50
40
30
20
10
0
Methanol extraction
Enzymatic extraction
Enzymatic extraction
Enzymaticextraction
H2O extraction
H2O extraction
HCl extraction
HCl extraction
HNO3 extraction
HNO3 extraction
HNO3 extraction
HNO3 extraction
HNO3 extraction
HNO3 extraction
HNO3 extraction
HNO3 extraction
HNO3 extraction
HNO3 extraction
HNO3 extraction
HNO3 extraction
HNO3 extraction
HNO3 extraction
HNO3 extraction
HNO3 extraction
HNO3 extraction
HNO3 extraction
HNO3 extraction
HNO3 extraction
Concentration (g/kg)
70
Extraction technique
45
40
35
30
25
20
15
10
5
0
Median
L031
L040
L021
L013
L032
L026
L031
L007
L039
L037
L015
L009
L004
L023
L010
L020
L038
L036
L024
L014
L022
L031
L017
L025
Concentration (g/kg)
Laboratory number
H2O extraction
HCl extraction
HNO3 extraction
Enzymatic extraction
Figure 9: DMA in brown rice displayed by laboratory number and extraction procedure.
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10,000
1000
100
10
1
L0
4
L0 0
1
L0 6
1
L0 3
1
L0 2
3
L0 7
3
L0 1
3
L0 8
0
L0 5
1
L0 5
1
L0 4
0
L0 4
2
L0 4
3
L0 6
0
L0 7
2
L0 5
2
L0 2
1
L0 0
2
L0 7
3
L0 4
0
L0 8
2
L0 3
3
L0 5
39
100,000
Laboratory number
(b) 100,000
10,000
1000
100
10
1
L0
12
L0
29
L0
31
L0
13
L0
24
L0
36
L0
23
L0
35
L0
14
L0
15
L0
10
L0
27
L0
38
L0
04
L0
40
L0
16
L0
11
L0
22
Brown Rice
The results and characteristics for white
rice flour and brown rice flour were
found to be very similar; therefore, the
white rice data are not shown separately
in this section.
The median result for As(III) in
brown rice was found to be 33 g/kg.
This is exemplified in Figure 8, which
shows inorganic arsenic values displayed
by extraction method. The laboratories
that reported As(III) results within 20%
of the median value were well distributed between those that used methanol, water, enzymatic, and nitric acid
extraction methods. However, only 12
laboratories reported As(V) results at
Spectroscopy 30(5) 57
(a)
May 2015
Laboratory number
Methonal extraction
H2O extraction
HCl extraction
HNO3 extraction
Enzymatic extraction
Other
Figure 10: (a) DMA and (b) MMA results for the kelp powder sample for the individual laboratories,
displayed by extraction technique (note: graphs use a logarithmic scale).
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58 Spectroscopy 30(5)
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May 2015
70,000
Concentration (g/kg)
60,000
50,000
40,000
30,000
20,000
As(III)
10,000
As(V)
Hamilton PRP X100
Hamilton PRP X100
Hamilton PRP X100
Hamilton PRP X100
Not specied
Dionex IonPac AS7
Hamilton PRP X100
Dionex IonPac AS16
Hamilton PRP X100
HG-AAS
Hamilton PRP X100
Hamilton PRP X100
Dionex IonPac AS7
Hamilton PRP X100
C18 column
Hamilton PRP X100
Not specied
Hamilton PRP X100
Supelcosil LC-SCX
Agilent G3288-80000
Not specied
Supelclean LC-SAX
Hamilton PRP X100
Hamilton PRP X100
Hamilton PRP X100
Hamilton PRP X100
Hamilton PRP X100
Separation technique
25
20
15
10
5
0
Supelclean LC-SAX
Polymethacrylete column
Hamilton PRP X100
Hamilton PRP X100
Hamilton PRP X100
Hamilton PRP X100
Hamilton PRP X100
Hamilton PRP X100
Hamilton PRP X100
Hamilton PRP X100
Hamilton PRP X100
Dionex IonPac AS7
Hamilton PRP X100
Not specied
Hamilton PRP X100
Hamilton PRP X100
Hamilton PRP X100
Hamilton PRP X100
Hamilton PRP X100
Hamilton PRP X100
HGAAS
Hamilton PRP X100
C18 column
Hamilton PRP X100
Hamilton PRP X100
Hamilton PRP X100
Not specied
Hamilton PRP X100
Supelcosil LC-SCX
Agilent G3288-80000
Hamilton PRP X100
Not specied
Concentration (g/kg)
Figure 11: Wide range of results for inorganic As in kelp, displayed by separation and column technology.
As(V)
As(III)
Separation technique
Figure 12: Inorganic arsenic in apple juice (direct injection into the HPLC column) by separation technique.
Table VII: A summary of the median values (M) for each analyte of each studied material
in g/kg (ppb)
M Values
(g/kg)
Total
Total
As in
As in
Sample Extract
As(III)
As(V)
Inorganic
MMAs
As
DMAs
AsB
White rice
four
40.70
39.90
25.91
(6.49)
30.15
(2.86)
8.49
ND
Brown rice
four
52.46
54.00
33.00
11.15
38.90
(2.75)
7.71
ND
Kelp powder
63,700
59,335
(3790) 20,924
23,763
(1530)
(1467)
3837
Apple juice
16.64
14.57
13.95
(0.60)
(0.35)
ND
1.84
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12.50
kg. However, the relative standard deviation (RSD) was 70% from those reporting laboratories. For this reason, it is very
difficult to assess the true value of As(V)
in the brown rice sample, with such a
large number of nondetected results.
The MMA results in rice were negligible, with very few laboratories reporting results, and because all the reported
results were at or near their detection
limits, these data are not shown. It is
also important to emphasize that only
half of the laboratories participating in
the study were able to quantify DMA
in rice with a median concentration of
7.7 g/kg. Most laboratories that reported DMA in the rice flour used a
nitric acid digestion. The DMA data in
brown rice are shown in Figure 9.
Kelp
The kelp was included in the study because of the recognized high level of arsenic typically associated with this matrix.
In addition, there are many less common
organic arsenic species found in kelp. The
DMA results in particular varied widely
with a range of 33137,068 g/kg. Of
the 23 laboratories that reported DMA,
nine laboratories reported results of less
than 1000 g/kg, while 10 laboratories
reported results in the 100010,000 g/
kg range, and four reported results over
10,000 g/kg. The MMA results also varied widely with a range of 2148,186 g/
kg. Of the 18 laboratories that reported
MMA, eight reported results of less than
1000 g/kg, five reported results in the
100010,000 g/kg range, and five laboratories reported results over 10,000 g/
kg. The DMA and MMA results for the
individual laboratories displayed by extraction technique are shown in Figures
10a and 10b (note: graphs use a logarithmic scale).
Chromatographic
Separation Procedures
As mentioned earlier, after arsenic is
extracted from the solid matrices, most
participating laboratories used a method
in which the oxidation states are separated by liquid chromatography and
then quantified using ICP-MS. The
challenges of this technique are achieving good chromatographic separation of
the individual species, preventing coelu-
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Spectroscopy 30(5) 59
% of Total
Participants
North
America
25
64
Europe
21
Other
15
120
Percentage of participants
(%)
Region
Table IX: The mean scores for each analyte for all material types
100
80
60
40
Mean
Score
Number of Data
Points Used for
Scoring
Total As in
sample
2.6
136
As(III)
Total As in
extract
2.7
79
Data reported
As(III)
2.6
88
As(V)
2.8
72
Inorganic As
2.7
122
Analyte
DMA
2.9
49
All analytes
2.6
546
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20
As(V)
DMA
MMA
Not measured
Non detect
Figure 13: The variability of the detectability of the submitted speciation results for brown rice, as
a percentage of the participating laboratories (note: white rice gave very similar results).
Table X: The number of laboratories receiving each score for each of the sample matrices
analyzed in the study, along with the mean score for each matrix
Assigned
Score
Brown Rice
Flour
Kelp Powder
Apple Juice
All Matrices
14
12
15
15
13
21
10
11
Not
measured
2.7
2.5
2.9
2.6
2.6
Mean score
Figure 11 shows the wide range of results for inorganic As in kelp, displayed
by separation and column technology.
The As(V) values are more consistent,
with an RSD of 40% covering a range of
values of 75020,000 g/kg, whereas the
As(III) values gave an RSD of 122% with
a much broader range of nondetectable
to 40,000 g/kg. The As(III) results were
disproportionately related to the separation procedure that gave high total inorganic As results. The high As(III) results
could potentially have been because of
peak misidentification or coelution because of the presence of AsB in the kelp.
Quantification of Apple Juice
In this study, 70% of the laboratories reported that they injected the apple juice
directly into the HPLC column, without
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60 Spectroscopy 30(5)
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Percentage of participants
(%)
120
100
80
60
40
20
0
As(III)
Data reported
As(V)
DMA
Not measured
MMA
Non detect
Figure 14: The variability of the detectability of the submitted speciation results for kelp powder,
as a percentage of the participating laboratories.
Percentage of participants
(%)
120
100
80
60
40
Overall Conclusions
20
0
As(III)
Data reported
As(V)
DMA
Not measured
MMA
Non detect
Figure 15: The variability of the detectability of the submitted speciation results for apple juice,
as a percentage of the participating laboratories.
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With such a large volume of data generated, it was possible to draw some overall
conclusions, based on correlation patterns between different matrices, species of interest, extraction procedures,
and chromatographic separation and
detection techniques used. For example, methods including a nitric acid hot
block assisted extraction and a Hamilton
PRP-X100 column were by far the most
dominant speciation methods, used by
24 out of the 39 participating laboratories. There was no other method that
was followed by more than 10% of the
laboratories. The dominance of this analytical scheme, comprising over half the
data reported, could possibly bias the
mean values of the study to that method.
For inorganic As, which is the most
important form to be measuring from
a human health risk perspective, statistically valid results were achievable for
all four matrices, with almost 80% of all
laboratories reporting values that were
within one standard deviation of the most
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Spectroscopy 30(5) 61
(2) US Food and Drug Administration, US FDA Laboratory Methods, Elemental Analysis Manual,
Arsenic Speciation in Rice and Rice Products
Using High Performance Liquid Chromatography-Inductively Coupled Plasma-Mass Spectrometric Determination, Section 4.11 (Online,
FDA, Rockville, Maryland, 2012) http://www.
fda.gov/Food/FoodScienceResearch/Labora-
Acknowledgments
This original study and subsequent
paper was made possible by the dedicated effort and input of many people.
Michela Hernandez at EcoChem, Inc.,
received, organized, anonymized, and
archived all of the data. The format of
the study was based on the report for
the 2012 Brooks Rand Instruments
Interlaboratory Comparison Study for
Total Mercury and Methylmercury
(9), authored by Joel Creswell, Virginia
Engel, Annie Carter, and Colin Davies.
Many members of Brooks Rand Labs
contributed to the success of this project. Annie Carter audited the accuracy
of the calculations and statistical analysis that appear in this report. Samantha
Dillon and Cory Wright assisted with
assembling and shipping of the kits of
study materials. Margaret Shultz coordinated the distribution of information
and corresponded with participants as
shipping issues arose. Tamas Ugrai
and Christabel Escarez performed the
screening analyses of more than 20
products to ensure total arsenic concentrations were suitable for this study.
All funding associated with producing
this intercomparison study and the associated report was provided by Brooks
Rand Labs. The authors would also
like to acknowledge the help of Robert
Thomas of Scientific Solutions for the
writing and preparation of this manuscript for publication.
Milled white rice and brown rice flour
were provided by the Dale Bumpers National Rice Research Center (part of the
USDA Agricultural Research Service) in
Stuttgart, Arkansas. Additional logistical assistance in obtaining and shipping
the rice flours to Brooks Rand Labs was
provided by Agilent Technologies and
the University of California, Davis.
References
(1) J. Kirby, W. Maher, M. Ellwood, and F. Krikowa,
(5) United States Geological Survey (USGS) Standard Reference Sample Project, Office of Water
Quality, Branch of Quality Systems. http://bqs.
usgs.gov/srs/SRS_Spr04/statrate.htm (accessed June 11, 2014).
(6) M. Briscoe, J. Creswell, and A. Carter, Interlaboratory Comparison Study for Arsenic Speciation
in Food and Juice, Brooks Rand Labs Report.
(Online, 2013) http://www.brooksrand.com/
wp-content/uploads/2014/02/Report+for+B
RL+As+Spec+in+Food+Intercomp+2013.pdf
(accessed June 11, 2014).
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Compact UV spectrometer
Harricks high-temperature
reaction chamber for Raman
microscopy is designed
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Raman instrumentation.
According to the company,
the chamber allows
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Compact UV spectrometers
from Mightex are designed with
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According to the company, the
spectrometers cover a range of
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Glass Expansion,
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Mightex,
Pleasanton, CA;
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Spectral sensor
Spectroscopy module
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PIKE Technologies,
Madison, WI;
www.piketech.com
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Packaging analyzer
Tornado Spectral
Systems, Inc.,
Toronto, Canada;
www.tornado-spectral.com
XRF kit
Raman spectrometer
Spectroscopy 30(5) 63
Avantes, Inc.,
Broomfield, CO;
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Amptek Inc.,
Bedford, MA;
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Horiba Scientific,
Edison, NJ; www.horiba.com
Microwave digestion
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PerkinElmer, Inc.,
Waltham, MA;
www.perkinelmer.com/PinAAcle500
ICP-OES system
LCMS-MS system
Bruker Corporation,
Moxtek, Inc.,
Orem, UT;
www.moxtek.com
Billerica MA;
www.bruker.com/BRAVO
The Z-500 and Z-100 laserinduced breakdown spectroscopy (LIBS) analyzers from
SciAps are designed with a
class 1M pulsed laser (4 mJ/
pulse) and a high-resolution,
wide-range spectrometer.
According to the company, the
analyzers Android-based operating system provides an intuitive, app-driven platform. Apps available for the instruments include
Alloy Analysis, Geochem, Empirical, and ProfileBuilder.
SciAps,
Woburn, MA;
www.sciaps.com
Hainault, UK;
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Calendar of Events
May 2015
2223 Symposium on
Molecular Spectroscopy
Fukuoka, Japan
bunshi.c.u-tokyo.ac.jp/e-index.html
June 2015
711 OSA Topical Meeting:
Imaging and Applied Optics
Arlington, VA
www.osa.org/en-us/meetings/optics_
and_photonics_congresses/imaging_and_
applied_optics/
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July 2015
510 EUROMAR 2015
Prague, Czech Republic
euromar2015.org
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May 2015
S
New Accessory Catalog!
www.piketech.com
Ad Index
ADVERTISER
PG#
ADVERTISER
PG#
57
OptiGrate Corporation
ABB Analytical
13
PANalytical, Inc.
31
Amptek
PerkinElmer Corporation
25
PIKE Technologies
Avantes BV
53
52
Bruker Optics
19
Rigaku Corporation
17
Glass Expansion
29
SciAps
33
Specac
47
Spectral Systems
51
11
Horiba Scientific
27, CV4
CV3
20, 21, 66
Metrohm USA
50
Mightex Systems
Milestone , Inc.
10
Moxtek, Inc.
23
55
66
15
CV2, 3, OUTSERT
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^'^
/ntnit
RamanShift[cm]
RamanShift[cm]
Measured with
LabRAM HR Evolution
(data courtesy of :
HORIBA Jobin Yvon SAS)
Wavelengths
in Production (nm)
405, 442, 458, 473, 488,
491, 514, 532, 552, 561,
568, 588, 594, 632, 660,
785, 830, 980, 1064, 1550
+1 (407) 542-7704
info@optigrate.com
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ZZZKRULEDFRPVFLHQWLF
email: adsci-specty@horiba.com
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