Spotlight on Analytical Applications e-Zine – Volume 14

VOLUME 14
SPOTLIGHT
ON APPLICATIONS.
FOR A BETTER
TOMORROW.
TABLEOF
CONTENTS

PerkinElmer
TABLEOF
CONTENTS
INTRODUCTION
PerkinElmer Spotlight on Applications e-Zine – Volume 14
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you may face in your application areas today.
Our Spotlight on Applications e-zine consists of a broad range of applications you’ll be
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PerkinElmer
CONTENTS
TABLEOF
CONTENTS
Energy & Industrial
• Use of the STA 8000 Simultaneous Thermal Analyzer for Melt Analysis of Alloys
• Characterizing Interaction of Nanoparticles with Organic Pollutants Using Coupling Thermal
Analysis with Spectroscopic Techniques
• Porcelain Clay Analysis Using the STA 8000 Simultaneous Thermal Analyzer
• Proximate Analysis of Coal and Coke Using the STA 8000 Simultaneous Thermal Analyzer
Food Beverage
• Determination of α-acids in Hops and Beers Using UHPLC
• Testing for Pomegranate Juice Adulteration
• Testing for the Authenticity of Milk
• Fungicide on Apple Peel Using DSA TOF
Forensics Toxicology
• Analysis of Cathinones in Bath Salts by Direct Sample Analysis TOF MS
• The Analysis of Nitroglycerin in Gunshot Residue Using DSA TOF
Pharmaceuticals Nutraceuticals
• Analysis of Paracetamol Tablets Using DSA TOF
• Practical Applications of HyperDSC in a Pharmaceutical Laboratory
• Analysis of Aerosols/Inhalers Using DSA TOF
• Components of Panadol®
Sinus Max Using DSA TOF

Download Entire Application Note
TABLEOF
CONTENTS
Introduction
While determining the composition of alloys has traditionally
been the domain of differential scanning calorimeters or
differential thermal analyzers,1
the STA 8000 has shown itself
to be capable of this type of demanding analysis as well. The
requirements for melt analysis are accurate temperature and
melt energy measurement and the ability to exclude oxygen –
or if necessary, nitrogen – during the analysis. This note shows
examples of two high temperature melting systems, including
iron-nickel alloys which require oxygen exclusion.
Experimental
The STA 8000 (Figure 1) provides the analysis of sample sizes typically in
the 10 to 200 milligram range with the samples heated by a small furnace
(~20 cc volume) capable of operating from 15 to 1600 degrees Celsius.2
The STA sensor is a double pan differential temperature sensor which is
calibrated to generate data for heat flow to the sample with an accuracy
of 5% or better. The weight sensor is located remotely below the furnace
where it is isolated from sample decomposition products by inert purge
through a narrow channel. This provides microgram-level weight change
detectability of sample loss or oxidative gain. Unless otherwise noted the
purge gas used for this note was nitrogen at a flow rate of 100 cc/min. The
use of argon instead of nitrogen is supported in the Pyris™
software which
controls the flow rate of gas through the furnace chamber and provides for
gas switching and flow rate changes.
Simultaneous Thermal Analysis
a p p l i c a t i o n n o t e
Authors
Bruce Cassel
Kevin P. Menard
PerkinElmer, Inc.
Shelton, CT USA
Professor Charles Earnest
Berry College
Department of Chemistry
Mount Berry, GA USA
Use of the STA 8000
Simultaneous Thermal
Analyzer for Melt
Analysis of Alloys
Figure 1. STA 8000 Simultaneous
Thermal Analyzer.

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CONTENTS
Introduction
There are more than a thousand products claiming to
contain Engineered Nanoparticles (ENP) in products
ranging from clothing, cosmetics, and electronics, to
biomedical, chemical, energy, environmental, food,
materials and optical products. The effects of ENP on
environmental and human health are strongly related to
their large surface-to-mass ratio and surface properties.
Although the influence of natural colloids on the
environment is well documented, we have limited
understanding of the fate, transport, toxicity and
pollutant interactions of ENP. The tools to study these
interactions are being developed.
Pollutants-colloid interaction
Many nanoparticles suspended in natural water come in contact with pollutants and proteinaceous
materials. The unique properties and behaviors of ENP are strongly influenced by their physical-
chemical characteristics, including their high surface area relative to their volume, high interface
energy and high surface-to-charge ratio density.
The partitioning and phase distribution of hazardous organic compounds (HOC) can influence
the fate and bioavailability of the contaminants in aquatic systems and aquatic microorganisms
significantly. There are a wide range of organic and inorganic pollutants that become associated
with partitioning of HOC to the particles. This partitioning has been shown to be inversely
proportional to log solubility of HOC and the log of particle concentration. Dynamics of nanoparticle-
water partitioning can significantly influence the speciation, and hence, understanding the fate,
transport and toxicological impact of POPs such as PAHs, PCBs is critical. The fate of organic
pollutants in aquatic environment depends largely on their partitioning behavior to nanoparticles
and colloids.
TGA-GC-MS
Authors
E. Sahle-Demessie
Amy Zhao
U.S. Environmental Protection Agency
Cincinnati, OH USA
Andrew W. Salamon
PerkinElmer, Inc.
Shelton, CT USA
Characterizing Interaction of
Nanoparticles with Organic
Pollutants Using Coupling
Thermal Analysis with
Spectroscopic Techniques

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CONTENTS
Introduction
In a process known for millennia, clay
is heated to yellow heat where the
components are transformed in a series of
processes, as the “mud” is transformed
into a useful vessel, or a beautiful piece of
art. Whether a porcelain clay formulation
is being used in the production of
a commercial product, or an artistic
creation, the ceramicist needs to ensure the quality of the finished product, and
this depends in part upon the chemical and physical behavior of the formulation
during the firing process. For example, in the firing of a porcelain clay object,
such as shown above,1
the physical and chemical properties of the clay
formulation determines whether the structure slumps as it is fired, whether there
is cracking around sharp edges, and whether the final product is bright and
translucent. So what can thermal analysis in general, and Simultaneous Thermal
Analysis (STA) specifically, tell us about such a clay formulation and about the
firing process?2,3,4
Simultaneous Thermal Analysis
Authors
Bruce Cassel
PerkinElmer, Inc.
Shelton, CT USA
Jennifer McCurdy
Vineyard Haven, MA USA
Dept. of Chemistry, Berry College
Mount Berry, GA, USA
Porcelain Clay Analysis
using the STA 8000
Simultaneous Thermal
Analyzer

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CONTENTS
Abstract
The STA 8000 Simultaneous Thermal
Analyzer (STA) is able to analyze coal and
coke to obtain Proximate Analysis data
– volatiles, fixed carbon and ash – using
10 to 100 milligram samples. This paper
demonstrates this utility using standard
coal and coke samples.
Introduction
Proximate analysis has long been used to determine the rank of coals by
separating volatile components, fixed carbon and inert components. Because
of the wide ranging quality of coal products and the commercial value of
ranking these products the need for good methods is obvious. To meet these
needs there are ASTM®
tests to perform these separations separately using
specialized industrial equipment.1
When using the ASTM®
methods, these
tests are carried out with gram sized samples to reduce the effort required to
get a representative, smaller sample. Round robin testing using homogenized
sample materials and multiple laboratories identified and documented many
of the considerations for performing this coal-ranking separation reliably.
Because of the wide range of volatile and pyrolytic components this is an
empirical separation with an arbitrary aspect to it. Therefore, standard samples
are used to allow testers to fine-tune their conditions to get the standardized
analysis.2
These standard samples are available in a -60 mesh (250 micron
Proximate Analysis of
Coal and Coke using the
STA 8000 Simultaneous
Thermal Analyzer
Thermal Analysis
Authors
Bruce Cassel
Kevin Menard
PerkinElmer, Inc.
Shelton, CT USA
Dept. of Chemistry
Berry College
Mt. Berry, GA USA

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CONTENTS
Introduction
Hops are crucial in beer brewing. They are added after the malting
of the grains and provide beers with their recognizable bitter taste
and aroma. The widespread use of hops in beer dates back to the
sixteenth century. However, as early as in the eleventh century it
was used as a natural preservative in central Europe (today Germany); the outcome was not only a
well preserved beer, but a beer with a distinctive smell and taste.
Hops come from a cone-like plant called Humulus lupulus with luplin gland that contains resin
and oils. The resins contain a number of α-acids that impart the bitter taste to most beers; the oils
in large part give beers their aroma.
One essential aspect of the quality control in beer brewing is making sure that the type and
amount of α-acids are the same from batch to batch, and that their transformation into the bitter
iso-α-acids during the brewing process gives individual brand its recognizable taste consistently
(Figure 1). To that end, in breweries around the world, α-acids in hops and beers are constantly
monitored. This application note presents a straightforward method to determine the type and
amount of α-acids in pellets from five hops varieties. An American IPA beer is analyzed to confirm
the presence of isomerized α-acids.
UHPLC
Authors
Njies Pedjie
PerkinElmer, Inc.
Shelton, CT USA
Determination
of α-acids in Hops
and Beers
Figure 1. Isomerization of hop α-acids to iso-α-acids during brewing.

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CONTENTS
Pomegranate Juice
Adulteration
Introduction
Pomegranate juice’s popularity has skyrocketed in the last
10 years. This has been due to a combination of the perceived
health benefits of consuming the juice’s various antioxidant
compounds (punicalagin, anthocyanins and ellagic acid) and
its increased mainstream availability through Western pomegranate producers. This increase
is highlighted by the rise in the consumption of 8-ounce servings of pomegranate juice in the
U.S., which went from 75M servings in 2004 to 450M servings by 2008.1
Interestingly, this
data indicates that in 2004, there was 50:50 pure-to-blended pomegranate juice consumption,
whereas in 2008, 100% pomegranate juice made up 75% of that consumed.1
Popular juice
blends, such as apple and grape, are less bitter and can make the overall juice taste more
pleasant to those new to pomegranate. These blends have an additional advantage of being
cheaper than pure pomegranate juice. Whereas a gallon of pomegranate juice concentrate costs
$30-60, a gallon of apple or grape juice is between $5-7. This means if a pomegranate juice
product is labeled as a blend with apple and grape juice, the consumer can expect to pay less
than the cost of pure pomegranate juice.
Case
study
Food Fraud
Download Entire Case Study

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CONTENTS
Milk Authenticity –
Organic vs Non-organic
With increasing concerns over contaminants in milk,
both intentionally and unintentionally added, a growing
number of people are switching to organic milk
(sales of whole organic milk were up 17% between January and October of 2011 in the
U.S. with reduced fat organic milk up 15%).1
This surge in popularity, coupled with high
food and fuel prices, has caused shortages in the supply of organic milk.2
With demand
therefore outstripping supply, and a gallon of organic milk costing anywhere from 25%
to 100% more than conventional milk, the selling of conventional milk as organic is an
attractive proposition to fraudsters. In the U.S. and E.U., the labelling of organic products
has meant stricter policing of farming practices but this is not the case with all countries.
Furthermore, with the growing export of organic milk powders, these fake organic milk
powders can find their way into the West through distributors or through processed
foods, such as chocolates, which will also command a higher price if claiming to be
organic. While these substitutions invariably do not cause health problems it is still fraud,
with consumers not getting what they paid for and hardworking organic farmers losing
business and having profit margins eroded.
Case
study
Food Fraud
Download Entire Case Study

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CONTENTS
TOF MS
Direct Sample analySiS
Easy to use
Fast accurate mass
Assures food safety
• Residual thiabendazole was
confirmed using DSA/TOF with
high mass accuracy
• Analysis performed in 15 seconds
with no sample preparation and
external calibration
Food and Beverage: Fungicide on Apple Peel
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p: (800) 762-4000 or
(+1) 203-925-4602
www.perkinelmer.com
• Thiabendazole is a common
ingredient in the waxes applied
to the skins of citrus fruits and is
also a fungicide used to protect
harvest yields.
Download Application Brief

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CONTENTS
Synthetic cathinones are gaining popularity
as drugs of abuse and are often sold in bath
salts. Currently, there is no standard method
to quickly screen and confirm cathinones
in bath salts. To address this issue, use of
the AxION®
Direct Sample Analysis™
(DSA™
)
integrated with the AxION 2 time-of-flight
mass spectrometer (TOF) (PerkinElmer, Waltham,
MA) was implemented. Cathinone standards and bath salt samples were rapidly
screened and confirmed in seconds by accurate mass and isotopic distribution of
parent and fragment ions using DSA/TOF and AxION Solo™
software.
Introduction
Cathinone is a beta-ketone amphetamine analogue that is found naturally
in the Catha edulis plant. Derivatives of cathinone have been synthesized
and are grouped together as cathinones.1
Synthetic cathinones have gained
popularity in the U.S. over the last few years as drugs of abuse, and are often
sold as bath salts in head shops. The synthetic stimulants are used as legal
substitutes for other illicit drugs, such as cocaine and methamphetamine. Bath
salt components continually change as street chemists alter existing compounds
to avoid detection. This in turn makes law enforcement surrounding bath salts
and cathinones difficult. To date, the Drug Enforcement Agency (DEA) has only
been successful in permanently banning two cathionones: mephedrone and
methylenedioxypyrovalerone (MDPV).2
Mass Spectrometry
Authors
Noelle M. Elliott
Avinash Dalmia
Carl Schwarz
PerkinElmer, Inc.
Shelton, CT USA
Amanda M. Leffler
Frank Dorman
Pennsylvania State University
University Park, PA USA
Analysis of Cathinones
in Bath Salts by Direct
Sample Analysis TOF MS

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CONTENTS
TOF MS
Forensics: Nitroglycerin
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940 Winter Street
p: (800) 762-4000 or
(+1) 203-925-4602
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Results in seconds
No sample preparation
Non-destructive
• DSA/TOF analysis on fabric identified
gunshot residue by confirmation of
nitroglyercin with accurate mass
• Analysis was performed in 15 seconds
external calibration• 2% Dichloromethylene in methanol (as
a dopant) was infused at 10 µL/min to
ionize nitroglycerin as a chloride adduct
• Gunshot residue analysis on fabric is
important for forensic analysis of crime
scenes. Modern gun powders use
nitrocellulose and nitroglyercin as basic
ingredients.

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CONTENTS
TOF MS
Results in seconds
No method development
Confirms product
authenticity
• DSA/TOF analysis of a tablet directly
detects components with a high mass
accuracy
• Paracetamol is a widely used over
the counter analgesic and antipyretic,
commonly used for the relief of minor
aches and pains.
Pharmaceutical: Paracetamol Tablets
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940 Winter Street
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(+1) 203-925-4602
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CONTENTS
HyperDSC™
(or High Speed DSC), a
thermal technique that complements
conventional calorimetry, has
found applications in the fields
of pharmaceutical, polymers and
compounds.
This technique features measurements taken at high heating (or cooling)
rates, from 100 to 500 °C/min. It is an approach that makes it easier to detect
such events as glass transition or the melting of a compound when they
are concealed by kinetic phenomena like, for example, water vaporization,
crystallization or chemical degradation.
Furthermore, HyperDSC offers greatly enhanced analysis
sensitivity due to the concentration of the energy phenomena
measured into a very brief space of time. Calorimetric
analyses on samples of very low mass (below 10 µg) are
thus made possible. The detection limits permitted by this
technique can be lowered considerably as compared with
conventional DSC, down to values 1% when quantifying
physical forms (amorphous or crystalline). HyperDSC analyses
can be carried out on the power compensation DSC 8500
from PerkinElmer shown in Figure 1. Figure 1. DSC 8500.
Differential Scanning Calorimetry
Authors
Svenja Goth
PerkinElmer, Inc.
Rodgau, Germany
Didier Clénet
Sanofi-Aventis
Analytical Sciences Department
Physical Characterization Laboratory
Vitry-sur-Seine, France
Practical Applications
of HyperDSC in a
Pharmaceutical
Laboratory

TABLEOF
CONTENTS
Copyright ©2012, PerkinElmer, Inc. All rights reserved. PerkinElmer®
is a registered trademark of PerkinElmer, Inc. All other trademarks are the property of their respective owners.
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940 Winter Street
Waltham, MA 02451 USA
P: (800) 762-4000 or
(+1) 203-925-4602
www.perkinelmer.com
TOF MS
DIrECt SAMPlE AnAlySIS
No method development
Fast accurate mass
Assures product safety
• The active compound was measured
using DSA/TOF which provided
accurate mass confirmation
• Analysis was performed in
15 seconds with no sample preparation
and external calibration
• Albuterol sulfate inhalation aerosol
is intended for oral inhalation as
a treatment for bronchospasm. It
contains a microcrystalline suspension
of albuterol sulfate in a propellant, and
no other excipients.
Pharmaceutical: Aerosols/Inhalers

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CONTENTS
Results in seconds
Complete component
analysis
Confirms product
authenticity
TOF MS
• DSA/TOF analysis of a tablet directly
detects components with a high mass
accuracy
010741_01
PerkinElmer, Inc.
940 Winter Street
p: (800) 762-4000 or
(+1) 203-925-4602
www.perkinelmer.com
• Panadol®
Sinus Max is designed
for fast and effective relief of
sinus congestion and pressure.
Pharmaceutical: Components of Panadol®
Sinus Max

TABLEOF
CONTENTS
PerkinElmer, Inc.
940 Winter Street
Waltham, MA 02451 USA
P: (800) 762-4000 or
(+1) 203-925-4602
www.perkinelmer.com
Copyright ©2013, PerkinElmer, Inc.All rights reserved. PerkinElmer® is a registered trademark of PerkinElmer, Inc.All other trademarks are the property of their respective owners.
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