VOLUME 12

SPOTLIGHTON APPLICATIONS.FOR A BETTERTOMORROW.

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PerkinElmer

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INTRODUCTION

PerkinElmer Spotlight on Applications e-Zine – Volume 12

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CONTENTS

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Consumer Products• Analysis of Broad Spectrum UVA and UVB Components in Sun Care Products for Compliance

with New FDA Regulations

• Thermal Analysis of Lipsticks using Differential Scanning Calorimetry

Energy & Industrial• Determination of Impurities in Organic Solvents used in the Semiconductor Industry with

the NexION ICP-MS

• Determination of Impurities in Semiconductor-Grade Sulfuric Acid with the NexION ICP-MS

• Determination of Impurities in Electronic-Grade Hydrochloric Acid with the NexION ICP-MS

• Determination of Impurities in Silica Wafers with the NexION ICP-MS

Environmental• Analysis of Drinking Waters by U.S. EPA Method 200.8 Using the NexION 300Q ICP-MS

in Standard Mode• Analysis of Drinking Waters by U.S. EPA Method 200.8 Using the NexION 300X ICP-MS

in Standard and Collision Modes• Analysis of Drinking Waters by U.S. EPA Method 200.8 Using the NexION 300D ICP-MS

in Standard, Collision and Reaction Modes• Method 8260C by Purge and Trap Gas Chromatography Mass Spectrometry using the Clarus SQ 8

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

• Characterization of Fats in Cookies Using Power Compensation DSC

Pharmaceuticals & Nutraceuticals• High Resolution Characterization of Pharmaceutical Polymorphs Using Power Compensation DSC

• StepScan DSC for Obscured Transitions

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Introduction

The FDA has made changes to how products containing sunscreen are labeled in the U.S. to ensure they meet the new regulations set forth for safety and effectiveness. The new regulations will require companies that want to use the ‘Broad Spectrum’ label to test for both 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.

Liquid Chromatography

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Author

Nonie Danna

PerkinElmer, Inc. Waltham, MA USA

Analysis of ‘Broad Spectrum’ UVA and UVB Components in Sun Care Products for Compliance with New FDA Regulations

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Introduction

Thermal analysis is very useful when applied to the development and analysis of cosmetics. Lipsticks are a complex mixture of compounds that are designed to spread easily and yet wear well. 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 of performance. As lipstick is applied on the body and worn at room temperature, melting normally occurs slightly above room temperature.

Differential Scanning Calorimetry

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

Thermal Analysis of Lipsticks Utilizing DSC

DSC 4000

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Introduction

Two of the most commonly used organic solvents in the semiconductor industry are isopropyl alcohol (IPA) and propylene glycol methyl ether acetate (PGMEA). While IPA is used frequently to clean silicon wafers, PGMEA is used as a thinner or stripper of photoresist. Both must be analyzed to check for trace metal contamination where the presence of contaminants would have detrimental 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.

Determination of Impurities in Organic Solvents used in the Semiconductor Industry with the NexION 300S ICP-MS

ICP-Mass Spectrometry

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

Author

Kenneth Ong

PerkinElmer, Inc. Singapore

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Introduction

The making of a semiconductor device comprises of forming a sacrificial layer on a substrate. Usually, a patterned resist layer forms the sacrificial layer so that ion implantation to the substrate can be 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 40Ca+, 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.

ICP-Mass Spectrometry

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Author

Kenneth Ong

PerkinElmer, Inc. Singapore

Determination of Impurities in Semiconductor-Grade Sulfuric Acid with the NexION 300S ICP-MS

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Introduction

In the production of semiconductor devices, the wafers are subjected to a so-called “Standard Clean 2” step, commonly referred to as an “SC2” step. The SC2 step is thought to desorb atomic 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 (ICP-MS) has been used for determination of ultra-trace impurity levels in various process chemicals. Nevertheless, under conventional plasma conditions, argon ions combine with matrix components to generate polyatomic interferences. Examples of chloride-based interferences observed during the analysis of HCl are listed in Table 1.

Determination of Impurities in Electronic-Grade Hydrochloric Acid with the NexION 300S ICP-MS

Table 1. Chloride interferences observed during HCl analysis.

Interference Analyte37Cl1H2 39K35Cl16O 51V35C16O1H 52Cr37Cl16O 53Cr37Cl16O16O 69Ga40Ar35Cl 75As40Ar37Cl 77Se

ICP-Mass Spectrometry

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

Author

Kenneth Ong

PerkinElmer, Inc. Singapore

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Introduction

The control of impurity levels in silicon-based semiconductor devices is critical because even ultratrace amounts of impurities, including alkali and alkali-earth elements and transition metals, can cause defects, such as voltage 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.

ICP-Mass Spectrometry

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

Author

Kenneth Ong

PerkinElmer, Inc. Singapore

Determination of Impurities in Silica Wafers with the NexION 300S ICP-MS

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Introduction

Method 200.8 is a well-established method promulgated by the U.S. Environmental Protection Agency (EPA) for the analysis of ground waters, surface waters, drinking waters, and wastewaters by inductively coupled plasma mass spectrometry (ICP-MS). 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.

ICP-Mass Spectrometry

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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 Waters by U.S. EPA Method 200.8 Using the NexION 300Q ICP-MS in Standard Mode

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Introduction

Method 200.8 is a well-established method promulgated by the U.S. Environmental Protection Agency (EPA) for the analysis of ground waters, surface waters, drinking waters, and wastewaters by inductively coupled plasma mass spectrometry (ICP-MS). 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.

ICP-Mass Spectrometry

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

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 Waters by U.S. EPA Method 200.8 Using the NexION 300X ICP-MS in Standard and Collision Modes

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Introduction

Method 200.8 is a well-established method promulgated by the U.S. Environmental Protection Agency (EPA) for the analysis of ground waters, surface waters, drinking waters, and wastewaters by inductively coupled plasma mass spectrometry (ICP-MS). 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.

ICP-Mass Spectrometry

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

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 Waters by U.S. EPA Method 200.8 Using the NexION 300D ICP-MS in Standard, Collision and Reaction Modes

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Introduction

U.S. EPA Method 8260C – Volatile Organic Compounds (VOCs) by Gas Chromatography Mass Spectrometry (GC/MS) is one of the most common environmental applications for GC/MS. This method outlines the analysis of volatile organic compounds in a variety 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.

Gas Chromatography/ Mass Spectrometry

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Authors

Ruben Garnica

Dawn May

PerkinElmer, Inc. Shelton, CT USA

Method 8260C by Purge and Trap Gas Chromatography Mass Spectrometry using the Clarus SQ 8

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Introduction

Starch is one of the primary sources of energy in the human diet, and is also used in a wide range of industrial processes, including brewing, bioethanol 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

Dynamic Mechanical Analysis

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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 Hydrothermal Behavior of Starch with Dynamic Mechanical Analysis

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Introduction

Differential scanning calorimetry (DSC) is a useful technique for the characterization of food products, including:

• thegelatinizationandstaling(retrogradation)behaviorofstarches

• polymorphismoffatssuchascocoabuttersandchocolate

• effectsofmoisturecontentorabsorbedmoisture

• agingeffects

• proteindenaturation

• determinationoffatcontentorsolidfatindex(SFI)

Theprocessingandhandlingbehavioroffoodfatshasbeenfoundtodependupon the solid-to-liquid fat ratio in the food sample. Many rheological or flow properties,andtheirresultanteffectonthetextureofthefinalproduct,stemfromthisfatratioindex.

Thestudyofthefatcontentandthenatureofthefatsoffoodsisbecomingincreasingly more important due to health considerations, especially with regards tothelevelofsolidfats,saturatedfatsandtransfatsinfoodproducts.Thereisavarietyoffatswithdifferentlevelsofsolidfatsavailableinfoodproducts.AnexampleofthisistheOreo®CookiewherethereistheregularOreo® and the reducedfatversion.TherearealsoOreo®-like cookies with no solid, hydrogenated fats present.

Thermal Analysis

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Characterization of Fats in Cookies Using Power Compensation DSC

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Introduction

Many pharmaceutical materials exhibit polymorphism, which means that, depending upon the given processing conditions, the crystalline form may exist in two or more states. The crystalline states or forms exhibit different levels of thermodynamic stabilities and an unstable form can melt at a temperature significantly less than the melting point of the thermodynamically stable form. Depending upon the conditions used to generate the crystalline form(s), the drug may exhibit one or more unstable, polymorphic crystalline states. In addition, as one state undergoes melting, it may be followed by 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:

• Theuptakeoftheactivedrugintothebloodstreamonceingested

• Theshelflifeofthedrug.

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 formulation.

Thermal Analysis

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High Resolution Characterization of Pharmaceutical Polymorphs Using Power Compensation DSC

DSC 8500

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

Thermal Analysis

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StepScan DSC for Obscured Transitions

Author

Kevin MenardPerkinElmer Thermal Laboratory College of Materials Science and Engineering University of North Texas Texas, USA

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