Spotlight on Analytical Applications e-Zine - Volume 13

VOLUME 13

SPOTLIGHTON APPLICATIONS.FOR A BETTERTOMORROW.

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PerkinElmer

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INTRODUCTION

PerkinElmer Spotlight on Applications e-Zine – Volume 13

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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Consumer Products• Analysis of Plastics for Toxic Metals by Laser Ablation-ICP-MS in Collision Mode

• A Robust Method for the Analysis of Commonly Used Sunscreen Compounds for Compliance with New FDA Regulations

Energy & Industrial• Biodiesel Analysis for Inorganic Contaminants Using the Optima 8000 ICP-OES with Flat Plate

Plasma Technology

• Curing of an Optical Adhesive by UV Irradiation in the DSC 8000

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

• Determination of Impurities in Semiconductor-Grade TMAH with the NexION 300S ICP-MS

Environmental• Mercury Speciation in Biological Tissue and Sediments by GC/ICP-MS • Benefits of NexION 300 ICP-MS Technology for the Analysis of Power Plant Flue Gas

Desulfurization Wastewaters • Analysis of Pharmaceuticals and Personal Care Products in River Water Samples by UHPLC-TOF • Methane, Ethylene, and Ethane in Water by Headspace-Gas Chromatography (HS-GC)

with Flame Ionization Detection (FID)

Pharmaceuticals & Nutraceuticals• Analysis of Cyclic Antidepressant Drugs in Human Plasma by UHPLCAPCI Single Quadrupole

Mass Spectrometry

• Benefits of the NexION 300X ICP-MS Coupled with the prepFAST In-line Auto-dilution/calibration System for the Implementation of the New USP Chapters on Elemental Impurities

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Analysis of Plastics for Toxic Metals by Laser Ablation-ICP-MS in Collision Mode

A P P L I C A T I O N B R I E F

ICP-Mass Spectrometry

Introduction

Owing to growing international concern, governments around the world are setting in place regulatory guidelines to restrict the migration of certain toxic substances from manufactured materials into the environment. Elements of particular concern include chromium (Cr), arsenic (As), cadmium (Cd), mercury (Hg) and lead (Pb). The European Union (EU) and the United States (US) have defined regulations to protect their citizens from pathways for migration of these elements into biological systems. Two typical pathways that are of concern to health officials are:

(a) The migration of toxic elements in the human body from plastic parenteral nutrition products (IV bags, catheters, tubing and product containers) which are in direct contact with the human blood stream;

(b) The transfer of trace elements into the local ecosystem from consumer plastics (computer hardware and peripherals, product packaging, etc.), incinerated or deposited into landfills.

Traditionally, polymeric materials are digested using mineral acids to dissolve them. However, such acid digestion procedures can be complex, time consuming and carry the risk of contamination or elemental losses. Laser ablation solid sampling is a micro-destructive technique that reduces sample preparation times dramatically, enabling high sample throughput. The data presented in this work describe a unique laser ablation solid sampling method that displays real promise as a viable technique capable of accurate multi-element quantitative analysis

Experimental

An NWR213 laser ablation system (ESI, Fremont, CA U.S.) was coupled to a NexION® 300D quadrupole ICP-MS system equipped with a reaction/collision cell (PerkinElmer, Shelton, CT U.S.). The system was run in both Standard mode (no collision cell gas) and Collision mode (He collision cell gas) to compare and contrast the analytical capabilities of both modes. A large area scan over the surface of the samples was used to provide a bulk analysis. The main operating parameters are listed in Table 1.

Authors

Fadi Abou-Shakra

PerkinElmer, Inc.

Dr. Rob Hutchinson

ESI

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Introduction

Over time, exposure to ultra violet (UV) radiation from the sun or tanning beds can damage the skin’s cellular DNA, resulting in mutations that cause 3.5 million cases of skin cancers and about 11,500 deaths in the U.S. each year, for a total cost of nearly $2 billion. There are three types of UV: UVC, UVB, and UVA. Of the three, UVC has the shortest wavelengths and is the most dangerous; fortunately it is completely absorbed by

the ozone layer in the atmosphere. UVB has short wavelengths that penetrate the outer layer of the skin causing sunburn. UVA has longer wavelengths that penetrate deeper into the skin, causing wrinkling and premature aging.

There are two types of skin cancers: one type develops in melanocytes and is called melanoma (melanocytes are the cells producing the skin coloring pigments called melanin); the other type develops elsewhere in the skin cells and is called non-melanoma. Though it is the least common form of skin cancer, melanoma is the most deadly. Melanoma caused the death of about 9000 people every year in the U.S., which is about 75% of the deaths attributed to skin cancers, although it accounts for only 2% of all the cases diagnosed.

UHPLC

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Author

Njies Pedjie

PerkinElmer, Inc. Shelton, CT USA

A Robust Method for the Analysis of Commonly Used Sunscreen Compounds for Compliance with New FDA Regulations

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Introduction

In the Unites States, the production of biofuels is primarily driven by the use of corn for ethanol and soy beans for biodiesel. Unfortunately, the competition for these raw materials has had an adverse effect on the price of food stuffs produced from these crops. The search for alternative and more efficient sources of raw materials for biodiesel production is ongoing. Biodiesel can be made from any

plant or vegetable material that contains oils as well as from animal fat. Common sources include soybeans, palm, rapeseed, and tallow. However, many other sources have been used, such as peanuts, coconuts, corn, switchgrass, and algae.

ASTM® International publishes both standard test methods and specifications for pure, neat biodiesel which is also known as B100. The European Union is also involved with publishing standards for biodiesel.1 ASTM® D6751 Standard Specification for Biodiesel Fuel Blend Stock (B100) for Middle Distillate Fuels describes the requirements for the use of biodiesel as a blend component with middle distillate fuels (e.g., diesel fuel).2 The specification contains detailed requirements for biodiesel properties, chemical constituents, and contaminants. Biodiesel must meet these specifications prior to being blended with petroleum diesel fuel or being used directly in combustion engines. There are specific maximum limits for certain elemental contaminants which may be present as a result of the biodiesel reaction catalysts (sodium and potassium), constituents

ICP-Optical Emission Spectroscopy

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

Author

Stan Smith

PerkinElmer, Inc. Shelton, CT USA

Biodiesel Analysis for Inorganic Contaminants Using the Optima 8000 ICP-OES with Flat Plate Plasma Technology

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Introduction

Optical adhesives are used in many industries where solvents are undesirable. Semiconductors and chip manufacturers for example can not afford solvents depositing on components. Photo-DSC allows fast analysis of the curing profile and measurement of the energy of

the curing reactions. Because photo-initiated reactions are fast and energetic, good temperature control and responsiveness are needed to get good data. Power compensated instruments are the best choice for these applications

Experimental

A specialized DSC pan with a quartz cover can be used although an open pan often is acceptable. The sample is heated or cooled to the isothermal temperature and allowed to equilibrate. Pyris™ software allows triggering the shutter of the light source to open and close for irradiation of the sample. Data can be collected at various intensities and times to develop the best cure cycle for the material.

Differential Scanning Calorimetry

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

Author

Tiffany Kang

PerkinElmer, Inc. Shelton, CT USA

Curing of an Optical Adhesive by UV Irradiation in the DSC 8000

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Introduction

Semiconductor devices are currently being designed with smaller line widths and are more susceptible to low-level impurities. Nitric acid (HNO3) is widely used as a mixture with hydrofluoric

acid (HF) to alter between diffusion-limited or rate-limited etching in the semiconductor industry. The mixture is commonly used to etch and expose the critical layer in the front-end processing. In this stage, the actual devices, including transistors and resistors, are created. A typical front-end process includes the following: preparation of the wafer surface, growth of silicon dioxide (SiO2), patterning and subsequent implantation or diffusion of dopants to obtain the desired electrical properties, growth or deposition of a gate dielectric and via etching. Any metal impurities present would have detrimental effects on the reliability of an IC device. Nitric acid is also commonly used in semiconductor laboratories to carry out analysis of other semiconductor materials, and thus needs to be of high purity and quality. SEMI Standard C35-0708 specifies the maximum concentration of metal contaminants by element and tier for nitric acid.

Determination of Impurities in Semiconductor-Grade Nitric Acid 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

Tetramethylammonium hydroxide (TMAH) is widely used as a basic solvent in the development of acidic photoresist in the semiconductor photolithography process and in liquid crystal display (LCD) manufacturing. Its wide usage in these demanding applications has made the analysis of impurities in TMAH more and more critical. SEMI Standard C46-03061 specifies limits for 25% TMAH with

contamination limits to less than 10 ppb for each element. TMAH, however, is not commonly used in its concentrated form; in fact, most applications would have the concentration between 1 and 3%.

With its ability to determine analytes rapidly at the ultra trace (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. It is, however, extremely important to address the significant matrix-derived polyatomic interferences, as well as matrix suppression effects, due to carbon content. These issues are especially prominent when analyzing organic solvents directly. 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

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 Semiconductor-Grade TMAH with the NexION 300S ICP-MS

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Introduction

The chemical determination of mercury (Hg) species in the environment is gaining increasing interest both for improved understanding of their reactional pathways and also to meet regulation limits in both Europe and the U.S. Mercury species play an important role in environmental pollution because they can result from anthropogenic activities, as well as natural biomethylation processes.1

Inorganic mercury (Hg2+) is the main form present in water and sediment samples, while methylmercury (MMHg) compounds are considered more toxic than inorganic mercury and can be accumulated in biological tissues. Fish tend to concentrate MMHg by a factor of 105-107; hence, fish consumption is the major contributor to Hg risk in humans and wildlife.2 The European Union (EU) added Hg and its compounds in the list of priority pollutants (Decision 2455/2001/EC amending the Water Framework Directive 2000/60/EC).3 In addition, the EU established 0.5 µg/g (wet weight) as maximum level of Hg in different foodstuffs (Commission Regulation EC-78/2005 amending regulation CE-466/2001).3 The U.S. Food and Drug Administration (FDA) set an advisory standard of 1 µg/g wet weight in fish flesh.2 In 2003, the Joint FAO/WHO Expert Committee on Food Additives (JECFA) established a Provisional Tolerable Weekly Intake (PTWI) of 1.6 µg MMHg/kg body weight (bw) and 5 µg THg/kg bw.4 In 2010, the PTWI for total Hg was withdrawn by the Committee and replaced by a PTWI for inorganic mercury (Hg2+) of 4 µg/kg bw.4

GC/ICP-MS

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Authors

Joaudimir Castro

Emmanuel Tessier

Olivier F.X. Donard

Institut des Sciences Analytiques et de Physico-chimie pour l’Environnement et les Matériaux (IPREM)Laboratoire de Chimie Analytique Bio-inorganique et Environnement (LCABIE) UMR 5254 CNRSUniversité de Pau et des Pays de l’Adour Hélioparc, France

Kenneth Neubauer

PerkinElmer, Inc. Shelton, CT USA

Mercury Speciation in Biological Tissue and Sediments by GC/ICP-MS

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Introduction

One of the most widely used technologies for removing pollutants, such as sulfur dioxide, from flue gas emissions produced by coal-fired power plants, is the limestone-forced oxidation scrubbing system. More commonly known as flue gas desulfurization (FGD), this process employs gas scrubbers to spray limestone

slurry over the flue gas to convert gaseous sulfur dioxide to calcium sulfate.1 Unfortunately, many of the contaminants from the coal, limestone and make-up water are concentrated in the circulating water of the scrubbing system. So in order to maintain appropriate plant operating conditions, a constant purge stream of water containing these contaminants has to be discharged from the scrubbers while fresh limestone slurry is fed in. This purge stream is extremely acidic and saturated with high concentrations of gypsum, heavy metals, alkali earth metals, chlorides and dissolved organic compounds. A schematic of a typical FGD process is shown in Figure 1.

Benefits of NexION 300 ICP-MS Technology for the Analysis of Power Plant Flue Gas Desulfurization Wastewaters

Figure 1. The flue gas desulfurization (FGD) process.

slurry sprayers

wastewater

various treatment procedures

treated effluent to discharge

gypsum cake

dewatering vacuum belt

flue gas exhaust

slurry purge

flue gas inlet

limestone slurry inlet

air injection

ICP-Mass Spectrometry

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

Authors

Stan Smith

Ewa Pruszkowski, Ph.D.

PerkinElmer, Inc. Shelton, CT USA

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Introduction

Identifying the presence of emerging pollutants in surface water samples is a growing area of concern in the environ-mental field.1,2 Many of these pollutants are introduced into the surface waters anthropogenically through municipal waste water. Among the emerging pollutants, pharmaceuticals and personal care products (PPCPs) have been detected at parts per million and parts per trillion concentrations in surface waters. The presence of PPCPs suggests inefficient removal of these compounds by current sewage treatment processes.

We present a study of PPCPs in river water samples from the northeastern United States using UHPLC-TOF-MS for both targeted and non-targeted analytes. Unlike a triple quadrupole, which is operated in multiple reaction monitoring mode for screening only predefined targeted analytes, the time-of-flight (TOF) mass spectrometer provides full spectrum accurate mass data that can be used to analyze and identify an unlimited number of compounds, without prior knowledge of target analytes or when reference standards are not available. In this study we show how high mass accuracy information provided by the PerkinElmer AxION 2® TOF along with the priopriatory AxION EC ID software can be used to identify unknown analytes in surface river waters.

Liquid Chromatography/Mass Spectrometry

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Author

Sharanya Reddy

PerkinElmer, Inc. Shelton, CT USA

Analysis of Pharmaceuticals and Personal Care Products in River Water Samples by UHPLC-TOF

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Introduction

The rapid development of natural gas from unconventional sources in North America has created an energy “gold rush” not seen in contemporary times. The advent of horizontal drilling technologies and hydraulic fracturing has made this production economical and presents an energy source of sufficient magnitude that could last 100 years.

The technology presents a number of environmental challenges as the wells are drilled vertically through aquifers on their way to the deep shale deposits thousands of feet under the surface, and then turned horizontally and drilled another several thousand feet through the shale deposit. Herein lies the challenge: in the process of drilling the wells and preparing them for production (including “fracking” to optimize production), opportunities arise for contamination of the clean drinking water aquifers with methane and other low molecular weight organics (e.g., propane and ethane). Correctly drilled and cemented well bores should not be an issue, but any errors in engineering could result in contamination.

It is also possible that methane already exists at a low concentration in the aquifer from diffusion of the gas occurring naturally. There is a need (by property owner and lease holder) to confirm the level of gas in the aquifer before and during drilling, and also after the well is placed into production.

Methane, Ethylene, and Ethane in Water by Headspace-Gas Chromatography (HS-GC) with Flame Ionization Detection (FID)

Gas Chromatography

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

Authors

Lee Marotta

Dennis Yates

PerkinElmer, Inc. Shelton, CT USA

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Introduction

Antidepressants are important drugs in the treatment of mental health problems. As such, they are characterized for absorption, distribution, metabolism and excretion (ADME), and monitored for abuse, toxicology and efficacy. Tricyclic and tetracyclic antidepressants have been approved by the U.S. Food and Drug Administration (U.S. FDA) to treat depression and brain disorders other than depression.

These may include anxiety disorders, attention deficit hyperactivity, neuralgia and insomnia. Cyclic antidepressants manage depression symptoms by affecting molecular signaling pathways in the brain. The proposed mechanism for the drugs’ action involves modulating reactivity of specific chemicals (neurotransmitters). Antidepressants function to enhance serotonergic and/or noradrenergic neurotransmission by antagonistic action preventing neurotransmitter reuptake at their target receptors. This therapeutic effect is achieved through binding to the respective neurotransmitter molecules, specifically inhibiting interactions at the human 5-hydroxytryptamine receptor 3A (5-HT3A).

This application note demonstrates a fast, simple, and highly-effective method to quantify cyclic antidepressants in human plasma by combining a simple and robust sample preparation method with ultra-high pressure liquid chromatography separation and atmospheric pressure chemical ionization mass spectrometry (APCI LC/MS) analysis. This procedure has the potential to improve sample analysis throughput in clinical research and pharmacokinetic studies.

Liquid Chromatography/ Mass Spectrometry

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

Authors

Eugene Davidov

Adam J. Patkin

PerkinElmer, Inc. Shelton, CT USA

Analysis of Cyclic Antidepressant Drugs in Human Plasma by UHPLC-APCI Single Quadrupole Mass Spectrometry

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ICP-Mass Spectrometry

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

Authors

Lee Davidowski

Ewa Pruszkowski

PerkinElmer, Inc. Shelton, CT USA

Introduction

In April of 2012, the United States Pharmacopoeia (USP) came out with a brand new ICP-OES/ICP-MS method to determine a group of metallic contaminants in pharmaceutical products. The method, which has been summarized in General Chapters <232> and <233> entitled

“Elemental Impurities – Limits and Procedures”,1,2 replaces Chapter <231>, a heavy metals test based on precipitation of the metal sulfide in a sample, and comparing the intensity to a lead standard.3 Even though this test has been used for over a hundred years, it is well-accepted that it is prone to error and requires a skilled analyst to interpret the color correctly.

This study will focus on the practical benefits of the NexION® 300X ICP-MS coupled to the prepFAST in-line, auto-dilution and auto-calibration sample delivery system to determine a group of toxicologically-relevant elements in various pharmaceutical products. It will give an overview of the USP methodology, with particular emphasis on the impurity levels and the recommended analytical procedure. It will analyze some common pharmaceutical products covering the major drug delivery systems – oral, intravenous and inhalational – and present performance figures of merit for the system, based on the USP validation protocol for the method.

Benefits of the NexION 300X ICP-MS Coupled with the prepFAST In-line Auto-dilution/calibration System for the Implementation of the New USP Chapters on Elemental Impurities

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

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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.

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By Industry:

• Consumer Products• Energy• Environmental• Food, Beverage & Nutraceuticals• Forensics• Lubricants• Pharmaceutical Development & Manufacturing• Polymers/Plastics• Semiconductor & Electronics

By Technology:

• Atomic Absorption (AA)• Elemental Analysis• Gas Chromatography (GC)• GC Mass Spectrometry (GC/MS)• Hyphenated Technology• ICP Mass Spectrometry (ICP-MS)• Inductively Coupled Plasma (ICP-OES & ICP-AES)• Infrared Spectroscopy (FT-IR & IR)• LIMS & Data Handling• Liquid Chromatography (HPLC & UHPLC)• Mass Spectrometry

• Thermal Analysis• UV/Vis & UV/Vis/NIR

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