VOLUME 14

SPOTLIGHTON APPLICATIONS.FOR A BETTERTOMORROW.

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PerkinElmer

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INTRODUCTION

PerkinElmer Spotlight on Applications e-Zine – Volume 14

PerkinElmer knows that the right training, methods and application support are as integral to getting answers as the instrumentation. That’s why PerkinElmer has developed a novel approach to meet the challenges that today’s labs face, delivering you complete solutions for your application challenges.

We are pleased to share with you our Spotlight on Applications e-zine, which delivers a variety of topics that address the pressing issues and analytical challenges you may face in your application areas today.

Our Spotlight on Applications e-zine consists of a broad range of applications you’ll be able to access at your convenience. Each application in the table of contents includes an embedded link which takes you directly to the appropriate page within the e-zine.

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CONTENTS

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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

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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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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

a p p l i c a t i o n n o t e

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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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

a p p l i c a t i o n n o t e

Authors

Bruce Cassel

PerkinElmer, Inc. Shelton, CT USA

Jennifer McCurdy

Vineyard Haven, MA USA

Professor Charles Earnest

Dept. of Chemistry, Berry College Mount Berry, GA, USA

Porcelain Clay Analysis using the STA 8000 Simultaneous Thermal Analyzer

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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

a p p l i c a t i o n n o t e

Authors

Bruce Cassel

Kevin Menard

PerkinElmer, Inc. Shelton, CT USA

Professor Charles Earnest

Dept. of Chemistry Berry College Mt. Berry, GA USA

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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

a p p l i c a t i o n n o t e

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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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

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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

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TSTOF MS

Direct Sample analySiS

Easy to use

Fast accurate mass

Assures food safety

• ResidualthiabendazolewasconfirmedusingDSA/TOFwithhighmassaccuracy

• Analysisperformedin15secondswithnosamplepreparationandexternalcalibration

Food and Beverage: Fungicide on Apple Peel

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• Thiabendazoleisacommoningredientinthewaxesappliedtotheskinsofcitrusfruitsandisalsoafungicideusedtoprotectharvestyields.

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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

a p p l i c a t i o n n o t e

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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TSTOF MS

Direct Sample analySiS

Forensics: Nitroglycerin

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Results in seconds

No sample preparation

Non-destructive

• DSA/TOFanalysisonfabricidentifiedgunshotresiduebyconfirmationofnitroglyercinwithaccuratemass

• Analysiswasperformedin15secondswithnosamplepreparationandexternalcalibration• 2%Dichloromethyleneinmethanol(as

adopant)wasinfusedat10µL/mintoionizenitroglycerinasachlorideadduct

• Gunshotresidueanalysisonfabricisimportantforforensicanalysisofcrimescenes.Moderngunpowdersusenitrocelluloseandnitroglyercinasbasicingredients.

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TOF MS

Direct Sample analySiS

Results in seconds

No method development

Confirms product authenticity

• DSA/TOFanalysisofatabletdirectlydetectscomponentswithahighmassaccuracy

• Analysiswasperformedin15secondswithnosamplepreparationandexternalcalibration

• Paracetamolisawidelyusedoverthecounteranalgesicandantipyretic,commonlyusedforthereliefofminorachesandpains.

Pharmaceutical: Paracetamol Tablets

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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

a p p l i c a t i o n n o t e

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

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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. 010561_01

PerkinElmer, Inc. 940 Winter Street Waltham, MA 02451 USA P: (800) 762-4000 or (+1) 203-925-4602www.perkinelmer.com

TOF MS

DIrECt SAMPlE AnAlySIS

No method development

Fast accurate mass

Assures product safety

• TheactivecompoundwasmeasuredusingDSA/TOFwhichprovidedaccuratemassconfirmation

• Analysiswasperformedin15secondswithnosamplepreparationandexternalcalibration

• Albuterolsulfateinhalationaerosolisintendedfororalinhalationasatreatmentforbronchospasm.Itcontainsamicrocrystallinesuspensionofalbuterolsulfateinapropellant,andnootherexcipients.

Pharmaceutical: Aerosols/Inhalers

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Results in seconds

Complete component analysis

Confirms product authenticity

TOF MS

Direct Sample analySiS

• DSA/TOFanalysisofatabletdirectlydetectscomponentswithahighmassaccuracy

• Analysiswasperformedin15secondswithnosamplepreparationandexternalcalibration

For a complete listing of our global offices, visit www.perkinelmer.com/ContactUs

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. 010741_01

PerkinElmer, Inc. 940 Winter Street Waltham, ma 02451 USa p: (800) 762-4000 or (+1) 203-925-4602www.perkinelmer.com

• Panadol®SinusMaxisdesignedforfastandeffectivereliefofsinuscongestionandpressure.

Pharmaceutical: Components of Panadol® Sinus Max

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PerkinElmer, Inc.940 Winter StreetWaltham, MA 02451 USAP: (800) 762-4000 or(+1) 203-925-4602www.perkinelmer.com

For a complete listing of our global offices, visit www.perkinelmer.com/ContactUs

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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