Spotlight on Analytical Applicatons e-Zine - Volume 12

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SPOTLIGHT
ON APPLICATIONS.
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VOLUME 12

CONTENTS
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INTRODUCTION
PerkinElmer Spotlight on Applications e-Zine – Volume 12
PerkinElmer knows that the right training, methods and application support are
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We are pleased to share with you our Spotlight on Applications e-zine, which
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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
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CONTENTS
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CONTENTS

Consumer Products
• nalysis of Broad Spectrum UVA and UVB Components in Sun Care Products for Compliance
A
with New FDA Regulations
• Thermal Analysis of Lipsticks using Differential Scanning Calorimetry

Energy Industrial
• etermination of Impurities in Organic Solvents used in the Semiconductor Industry with
D
the NexION ICP-MS
• etermination of Impurities in Semiconductor-Grade Sulfuric Acid with the NexION ICP-MS
D
• etermination of Impurities in Electronic-Grade Hydrochloric Acid with the NexION ICP-MS
D
• etermination of Impurities in Silica Wafers with the NexION ICP-MS
D

Environmental
• nalysis of Drinking Waters by U.S. EPA Method 200.8 Using the NexION 300Q ICP-MS
A
in Standard Mode
• nalysis of Drinking Waters by U.S. EPA Method 200.8 Using the NexION 300X ICP-MS
A
in Standard and Collision Modes
• nalysis of Drinking Waters by U.S. EPA Method 200.8 Using the NexION 300D ICP-MS
A
in Standard, Collision and Reaction Modes
• ethod 8260C by Purge and Trap Gas Chromatography Mass Spectrometry using the Clarus SQ 8
M

Food Beverage
• Characterizing the Hydrothermal Behavior of Starch with Dynamic Mechanical Analysis

• Characterization of Fats in Cookies Using Power Compensation DSC

Pharmaceuticals Nutraceuticals
• igh Resolution Characterization of Pharmaceutical Polymorphs Using Power Compensation DSC
H
• StepScan DSC for Obscured Transitions

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

Liquid Chromatography

Author
Nonie Danna
PerkinElmer, Inc.
Waltham, MA USA

Analysis of ‘Broad Spectrum’ Introduction
The FDA has made changes to how
UVA and UVB Components products containing sunscreen are labeled
in the U.S. to ensure they meet the
in Sun Care Products for new regulations set forth for safety and
effectiveness. The new regulations will
Compliance with New require companies that want to use the
‘Broad Spectrum’ label to test for both
FDA Regulations UVA and UVB protection. The FDA’s
standardized test for broad spectrum
enables consumers to determine the
level of UVA protection a sunscreen provides in addition to its ultraviolet B
(UVB) radiation protection. Previous rules only dealt with preventing sunburn
which is primarily due to UVB radiation but did not address UVA which
protects against early aging and skin cancer. These new testing and labeling
requirements are necessary to educate consumers and provide information
for consumers to make knowledgeable choices. All products that claim to
provide Broad Spectrum SPF protection are regulated as sunscreen products.
Therefore, the regulations the FDA has developed for Over The Counter (OTC)
sunscreen products apply to cosmetics, moisturizers, lip balms, and shampoos
labeled with SPF values.

Download Entire Application Note

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Differential Scanning
Calorimetry

Thermal Analysis Introduction
Thermal analysis is very useful when applied to the development
of Lipsticks and analysis of cosmetics. Lipsticks are a complex mixture of
compounds that are designed to spread easily and yet wear well.
Utilizing DSC Often they are studied by Dynamic Mechanical Analysis, where
the frequency response can be correlated with the spreading of
the material. However, DSC is often used as a QC tool because
it is faster to run than DMA. This application note describes DSC
evaluation of lipstick qualities based on the melting of the fats and
oils which are the main content of lipsticks.

Methods
Using DSC to analyze lipstick involves a technique called fingerprinting.
The peaks are not assigned to specific transitions but the overall
shape, size, and temperature of the peaks are used as an indicator
DSC 4000 of performance. As lipstick is applied on the body and worn at
room temperature, melting normally occurs slightly above room
temperature.


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ICP-Mass Spectrometry

Author
Kenneth Ong
PerkinElmer, Inc.
Singapore

Determination of Impurities Introduction
Two of the most commonly used organic solvents in the
in Organic Solvents used semiconductor industry are isopropyl alcohol (IPA) and
propylene glycol methyl ether acetate (PGMEA). While
in the Semiconductor IPA is used frequently to clean silicon wafers, PGMEA is
used as a thinner or stripper of photoresist. Both must be
Industry with the NexION analyzed to check for trace metal contamination where
the presence of contaminants would have detrimental
300S ICP-MS effects on the reliability of memory devices. SEMI Standard
C41-0705 specifies limits for high purity IPA Grade 4 with
contamination limits of less than 100 ppt for each element.

With its ability to determine analytes rapidly at the ultratrace (ng/L or parts-per-trillion) level in various process
chemicals, inductively coupled plasma mass spectrometry (ICP-MS) has become an indispensable analytical tool
for quality control. However, it is extremely important to address certain potentially problematic areas when
analyzing organic solvents directly, including: viscosity and volatility, compatibility of the sample introduction
device, deposition of carbon on the interface cones, matrix-derived polyatomic interferences, as well as matrix
suppression effects due to carbon content. A cooled spray chamber might help to reduce the vapor pressure
with an optimized sample uptake rate for volatile organic solvents. Carbon deposited on the tip of the
interface cones can be avoided by adding a small amount of oxygen into the injector gas flow between the
spray chamber and the torch.

Although cool plasma has been shown to be effective in reducing argon-based interferences, it is even more
prone to matrix suppression than hot plasma. Additionally, the low plasma energy may result in preferential
formation of other polyatomic interferences, which are not seen under hot plasma conditions. Collision cells
using multipoles and nonreactive gases have proven useful in reducing polyatomic interferences. However, kinetic
energy discrimination results in the loss of sensitivity, which is an issue when analyzing ng/L levels. Reaction mode
is another technique which uses a reactive gas, such as NH3, to selectively react with the polyatomic interference,
and a quadrupole mass filter to create dynamic bandpass to prevent undesirable formation of by-product ions,
thereby removing the polyatomic interference effectively without suppressing the analytes’ signal.


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Author
Kenneth Ong
PerkinElmer, Inc.
Singapore

Determination of
Impurities in Introduction
Semiconductor-Grade The making of a semiconductor device comprises
of forming a sacrificial layer on a substrate. Usually,
Sulfuric Acid with the a patterned resist layer forms the sacrificial layer
so that ion implantation to the substrate can be
NexION 300S ICP-MS performed, after which a wet etching solution is
used to remove the patterned photoresist layer.
Typically, an etching solution comprises of sulfuric acid (H2SO4) and peroxide (H2O2), known
as piranha or ozonated sulfuric acid. As with other chemicals used, any metal impurities
present would have detrimental effect on the reliability of an IC device and thus need to be
of high purity and quality. SEMI Standard C44-0708 specifies the maximum concentration of
metal contaminants by element and tier for sulfuric acid.

Inductively coupled plasma mass spectrometry (ICP-MS) is an indispensable analytical tool for
quality control because of its superior capability to detect at the ultratrace (ng/L or parts-per-
trillion) level. Nevertheless, under the conventional plasma conditions, argon ions combine
with matrix components to generate polyatomic interferences. Some of the interferences in
sulfuric acid are 32S15N+ on 47Ti+, 32S16O2+ on 64Zn+, ArS+ on 70-74Ge+, 38Ar1H+ on 39K+, 40Ar+ on
40
Ca+, 40Ar16O+ on 56Fe+.

The Dynamic Reaction Cell (DRC™), which uses a quadrupole mass filter to create Dynamic
Bandpass Tuning (DBT), is a powerful correction technique to remove interferences on
analytes of interest. Collision cells, using nonreactive gases, have proven to be another
simple method in reducing specific polyatomic interferences. Both of these techniques
are available in PerkinElmer’s NexION® 300 ICP-MS through its unique Universal Cell
Technology™, which allows the use of all three modes (Standard, Collision and Reaction)
within one analytical method.


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Author
Kenneth Ong
PerkinElmer, Inc.
Singapore

Determination of
Impurities in Electronic- Introduction
In the production of semiconductor
Grade Hydrochloric Acid devices, the wafers are subjected to
a so-called “Standard Clean 2” step,
with the NexION 300S commonly referred to as an “SC2” step.
The SC2 step is thought to desorb atomic
ICP-MS and ionic contaminants from the wafers.
In particular, the SC2 step is intended
to remove metals deposited on the
wafer surface. In a typical SC2 step, the wafers are submerged in a solution
of H2O:HCl:H2O2. Thus, it is important to analyze for the presence of metal
contaminants in electronic-grade hydrochloric acid (HCl). SEMI Standard C27-
0708 specifies the maximum concentration of metal contaminants by element
and tier for hydrochloric acid.

Inductively coupled plasma mass spectrometry Table 1. Chloride interferences
(ICP-MS) has been used for determination of observed during HCl analysis.
ultra-trace impurity levels in various process Interference Analyte
chemicals. Nevertheless, under conventional 37
Cl1H2 39
K
plasma conditions, argon ions combine with 35
Cl O
16 51
V
matrix components to generate polyatomic
interferences. Examples of chloride-based
35
C16O1H 52
Cr
interferences observed during the analysis of 37
Cl O
16 53
Cr
HCl are listed in Table 1. 37
Cl16O16O 69
Ga
40
Ar Cl
35 75
As
40
Ar37Cl 77
Se


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Author
Kenneth Ong
PerkinElmer, Inc.
Singapore

Determination of Introduction
The control of impurity levels in silicon-based
Impurities in Silica semiconductor devices is critical because even
ultratrace amounts of impurities, including
Wafers with the alkali and alkali-earth elements and transition
metals, can cause defects, such as voltage
NexION 300S ICP-MS breakdown or high dark current.

For quality control purposes, there are two types of silicon that are routinely analyzed: bulk
silicon and the surface of silicon wafers. Bulk silicon analysis can be performed by totally
digesting the silicon using a very aggressive acid, such as hydrofluoric acid (HF). Vapor phase
decomposition is the most common method used for the surface analysis of silicon wafers
and involves collecting impurities on the wafer surface using a very small amount of acid
(typically HF) deposited on the surface as a droplet. This results in a typical sample volume
of around 200 μL. For bulk silicon analysis, sample volume is not an issue; however, small
sample volumes are desirable in order to minimize time-consuming sample preparation. As
such, both types of silicon analyses require the ability to handle small sample volumes and
high silicon matrices, as well as an HF-resistant sample introduction system. Since a typical
analysis may take 2-3 minutes per sample, low-flow nebulizers with sample uptake rates
from 20-100 μL/min are routinely used.


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Authors
Ewa Pruszkowski, Ph.D.
Senior ICP-MS Application Scientist
Cynthia P. Bosnak
Senior Product Specialist
PerkinElmer, Inc.
Shelton, CT USA

The Analysis of Drinking Introduction
Method 200.8 is a well-established method
Waters by U.S. EPA Method promulgated by the U.S. Environmental

200.8 Using the NexION Protection Agency (EPA) for the analysis of
ground waters, surface waters, drinking
300Q ICP-MS in Standard waters, and wastewaters by inductively
coupled plasma mass spectrometry (ICP-MS).
Mode The method was first published in 1990
to support the National Primary Drinking
Water Regulations (NPDWR), which specified
maximum contaminant levels (MCL) for 12 primary elemental contaminants in
public water systems as part of the Safe Drinking Water Act (SDWA) of 1986.
There have been many iterations of Method 200.8, including the addition of 9
secondary contaminants under the National Secondary Drinking Water Regulations
(NSDWR). These 21 elements, along with suggested analytical masses, are shown
in Table 1. The version in use today is Revision 5.4 of the Method, which was
approved for drinking water in 1994 and became effective in January, 1995.3
In addition, Method 200.8 was also recommended in 1992 for the monitoring
of wastewaters under the National Pollutant Discharge Elimination System
(NPDES) permit program to control the discharge of pollutants into navigable
water systems, as part of the amended Clean Water Act (CWA) of 1977.4
It was approved on a nation-wide basis for this matrix in 2007.


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Authors
Cynthia P. Bosnak
PerkinElmer, Inc.
Shelton, CT USA


200.8 Using the NexION 300X Protection Agency (EPA) for the analysis of
ICP-MS in Standard and waters, and wastewaters by inductively
Collision Modes The method was first published in 1990
There have been many iterations of Method 200.8, including the addition
of 9 secondary contaminants under the National Secondary Drinking Water
Regulations (NSDWR). These 21 elements, along with suggested analytical
masses, are shown in Table 1. The version in use today is Revision 5.4 of the
Method, which was approved for drinking water in 1994 and became effective
in January, 1995.3 In addition, Method 200.8 was also recommended in 1992
for the monitoring of wastewaters under the National Pollutant Discharge
Elimination System (NPDES) permit program to control the discharge of pollutants
into navigable water systems, as part of the amended Clean Water Act (CWA)
of 1977.4 It was approved on a nation-wide basis for this matrix in 2007.


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Authors
Cynthia P. Bosnak
PerkinElmer, Inc.
Shelton, CT USA


200.8 Using the NexION 300D Protection Agency (EPA) for the analysis of
ICP-MS in Standard, Collision waters, and wastewaters by inductively
and Reaction Modes The method was first published in 1990
There have been many iterations of Method 200.8, including the addition of
9 secondary contaminants under the National Secondary Drinking Water Regulations
(NSDWR). These 21 elements, along with suggested analytical masses, are shown
in Table 1. The version in use today is Revision 5.4 of the Method, which was
approved for drinking water in 1994 and became effective in January, 1995.3 In
addition, Method 200.8 was also recommended in 1992 for the monitoring of
wastewaters under the National Pollutant Discharge Elimination System (NPDES)
permit program to control the discharge of pollutants into navigable water
systems, as part of the amended Clean Water Act (CWA) of 1977.4 It was
approved on a nation-wide basis for this matrix in 2007.


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Gas Chromatography/
Mass Spectrometry

Authors
Ruben Garnica
Dawn May
PerkinElmer, Inc.
Shelton, CT USA

Method 8260C by Introduction
U.S. EPA Method 8260C – Volatile
Purge and Trap Gas Organic Compounds (VOCs) by Gas
Chromatography Mass Spectrometry
Chromatography (GC/MS) is one of the most common
environmental applications for GC/MS.
Mass Spectrometry This method outlines the analysis of
volatile organic compounds in a variety
using the Clarus SQ 8 of solid waste matrices including vari-
ous air sampling trapping media, ground
and surface water, soils, and sediments
among others. The method requires not
only demonstration of laboratory sample preparation and handling competence
but instrument performance as well. The study presented here demonstrates
the PerkinElmer® Clarus® SQ 8 GC/MS with purge and trap sample introduction
both meets and exceeds the performance criteria set out in method 8260C and
describes the analytical results and instrumental methodology.

Experimental
The PerkinElmer Clarus SQ 8C GC/MS operating in electron ionization mode
with an Atomx purge and trap sample introduction system (Teledyne Tekmar,
Mason, OH) was used to perform these experiments. The purge and trap
conditions are presented in Table 1 and represent standard conditions for
the analysis of method of VOCs by EPA Method 8260C.


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Dynamic Mechanical Analysis

Authors
Dr. Frederick J. Warren
Dr. Paul G. Royall
Dr. Peter R. Ellis
Dr. Peter J. Butterworth
King’s College London
London, UK
Dr. Ben Perston
PerkinElmer, Inc.
Shelton, CT USA

Characterizing the
Introduction
Hydrothermal Behavior Starch is one of the primary sources of energy in

of Starch with Dynamic the human diet, and is also used in a wide range of
industrial processes, including brewing, bioethanol

Mechanical Analysis production, paper manufacture and in the production
of biodegradable plastics.1

Starch exists in plants in a granular form, the granules being between 1 and
100 μm in diameter, and has a complex semi-crystalline structure. Starch consists
of two polymeric components: amylose, which is an essentially linear α (1→4)
linked glucose chain, and amylopectin, which is a branched polymer of α (1→4)
linked glucose chains interspersed with α (1→6) branch points. The relative
proportions of amorphous and crystalline material in the starch granule, and
the arrangement of structure in the granule, have a significant bearing on the
behavior of the starch and its response to hydrothermal treatments.2

One of the most important modifications of starch structure that occurs
during processing of starch, for both food usage and industrial applications,
is gelatinization. When heated in excess water, starch goes through a thermal
transition, termed gelatinization, at temperatures between 50 and 70 ˚C. Starch
gelatinization is an endothermic transition associated with rapid swelling of
the granule and melting of crystalline regions. In the absence of water, starch
crystallites go through a melting transition at much higher temperatures


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Thermal Analysis

Characterization Introduction
Differential scanning calorimetry (DSC) is a useful technique for the characterization
of Fats in Cookies of food products, including:

Using Power • the gelatinization and staling (retrogradation) behavior of starches
• polymorphism of fats such as cocoa butters and chocolate
Compensation DSC • effects of moisture content or absorbed moisture
• aging effects
• protein denaturation
• determination of fat content or solid fat index (SFI)

The processing and handling behavior of food fats has been found to depend
upon the solid-to-liquid fat ratio in the food sample. Many rheological or flow
properties, and their resultant effect on the texture of the final product, stem
from this fat ratio index.

The study of the fat content and the nature of the fats of foods is becoming
increasingly more important due to health considerations, especially with regards
to the level of solid fats, saturated fats and trans fats in food products. There is
a variety of fats with different levels of solid fats available in food products. An
example of this is the Oreo® Cookie where there is the regular Oreo® and the
reduced fat version. There are also Oreo®-like cookies with no solid, hydrogenated
fats present.


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Thermal Analysis

High Resolution Introduction
Many pharmaceutical materials exhibit polymorphism, which means
Characterization that, depending upon the given processing conditions, the crystalline
form may exist in two or more states. The crystalline states or forms
of Pharmaceutical exhibit different levels of thermodynamic stabilities and an unstable
form can melt at a temperature significantly less than the melting
Polymorphs Using point of the thermodynamically stable form. Depending upon the
conditions used to generate the crystalline form(s), the drug may
Power Compensation exhibit one or more unstable, polymorphic crystalline states. In
addition, as one state undergoes melting, it may be followed by
DSC crystallization and then melting at increasingly higher temperatures,
due to the formation of a more stable state. The existence of these
polymorphic crystalline states is important for many pharmaceutical
materials, as they can have a major effect upon:

• The uptake of the active drug into the bloodstream once ingested

• The shelf life of the drug.

One polymorphic form of a given drug may be more easily dissolvable
or ingestible than another form and the time release of the material
can sometimes by controlled by the given type and level of a particular
polymorphic form. Additionally, one crystalline form may exhibit a
longer shelf life than another form. It is also possible that an easily
dissolvable crystalline form can convert, over time, to a less dissolvable
form thus changing the pharmaceutically active properties of the drug
DSC 8500 formulation.


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Thermal Analysis

Author
Kevin Menard
PerkinElmer Thermal Laboratory
College of Materials Science and Engineering
University of North Texas
Texas, USA

StepScan DSC for StepScan DSC is a temperature modulated
DSC technique that operates in conjunction

Obscured Transitions with the Power Compensation Diamond
DSC from PerkinElmer. The approach
applies a series of short interval heating
and isothermal hold steps to cover the temperature range of interest. With the
StepScan™ DSC approach, two signals are obtained: the Thermodynamic Cp
signal represents the thermodynamic aspects of the material, while the Iso K
signal reflects the kinetic nature of the sample during heating. The following
basic equation mathematically describes the StepScan DSC approach:

Heat Flow = Cp(dT/dt) + f(T,t)

In this equation, Cp is the sample’s heat capacity, dT/dt is the applied heating
rate and f(T,t) is the kinetic response. The first Cp term represents the thermo-
dynamic aspects of the sample and, while the Power Compensation DSC applies
a purely linear heating ramp for the best results rather than a sine wave where
the heating rate is continuously varying. When the sample is held under iso-
thermal conditions, as does take place with the Power Compensation DSC and
the StepScan DSC approach, the heating rate becomes 0 and the sample’s heat
flow is purely described by the kinetic term. Because the sample is either linearly
heated or held isothermally (true isothermal), the StepScan DSC approach is
straightforward and provides the purest approach to TMDSC measurements.


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USEFUL LINKS
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• Volume 3 • Volume 6 • Volume 9 • Archives

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By Technology:
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• Infrared Spectroscopy (FT-IR IR)
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• Mass Spectrometry
• Raman Spectroscopy
• Thermal Analysis
• UV/Vis UV/Vis/NIR

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