Spotlight on Analytical Applications e-Zine - Volume 9

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This document provides key analytical applications to help laboratories address the pressing concerns of the changing global landscape. Specifically, Volume 9 includes applications for Energy & Industrial, Environmental, Food & Beverage, and Pharmaceuticals & Nutraceuticals and Forensics & Toxicology.

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Spotlight on Analytical Applications e-Zine - Volume 9

  1. 1. CONTENTS TABLE OF SPOTLIGHT ON APPLICATIONS. FOR A BETTER TOMORROW.VOLUME 9
  2. 2. CONTENTSTABLE OF INTRODUCTION PerkinElmer Spotlight on Applications e-Zine – Volume 9 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 that take you directly to the appropriate page within the e-zine. We invite you to explore, enjoy and learn! Be sure to receive future issues by subscribing here. PerkinElmer
  3. 3. CONTENTS TABLE OFCONTENTSEnergy & Industrial• Analysis of Bioethanol Impurities with the Spectrum Two FT-IR Spectrometer• nstrumental Requirements for Accurate Analysis of Optical Components: A comparison of the I PerkinElmer 983 Dispersive Spectrometer and the Frontier Optica FT-IR Spectrometer• nalysis of Vanadium, Nickel, Sodium, and Iron in Fuel Oils using Flame Atomic Absorption A• etermination of Oil Content in Membranes Used in Compressed Air Sampling by D Infrared SpectroscopyEnvironmental• Organic Elemental Analysis of Soils — Understanding the Carbon-Nitrogen Ratio• Determination of Hydrocarbons in Environmental Samples with Spectrum TwoFood Beverage• Monitoring VOCs in Beer Production Using the Clarus SQ 8 GC/MS and TurboMatrix Headspace Trap • ccurate Determination of Lead in Dairy Products by Graphite Furnace Atomic Absorption A• he Determination of Toxic, Trace, and Essential Elements in Food Matrices using THGA T Coupled with Longitudinal Zeeman Background Correction• he Determination of Low Levels of Benzene, Toluene, Ethylbenzene, Xylenes and Styrene T in Olive Oil Using a TurboMatrix HS and a Clarus SQ 8 GC/MSForensics Toxicology• enzoylecgonine in Urine by SAMHSA GC/MS B• ympathomimetic Amines in Urine by SAMHSA GC/MS SPharmaceuticals Nutraceuticals• yphenated DSC-Raman, a new Powerful Research Tool H• Study of Aged Carbon Nanotubes by Thermogravimetric Analysis A PerkinElmer
  4. 4. CONTENTSTABLE OF a p p l i c at i o n n o t E FT-IR Spectroscopy Authors Ben Perston Joe Baldwin PerkinElmer, Inc. Shelton, CT 06484 USA Analysis of Bioethanol Introduction The intensifying global emphasis on developing sustainable Impurities with the fuel supplies has led to increasing use of fuels derived from biological sources. The most important of these are biodiesel Spectrum Two FT-IR (produced by transesterification of plant and animal oils and fats) and bioethanol, which is produced by fermentation of Spectrometer sugars, starches and, increasingly, cellulose from a range of crops including corn, sugarcane, wheat and sugarbeet. The fermentation produces a complex mixture of ethanol and byproducts, from which the ethanol is isolated by distillation. The performance of the ethanol as a fuel is dependent on its purity, and international standards such as ASTM® D4806 and EN 15376 limit the allowable concentrations of impurities in fuel ethanol and specify the test methods to be used. At present, the specified tests are time-consuming chromatographic and titrimetric methods, so a rapid spectroscopic method such as FT-IR could provide an attractive alternative. Figure 1. The Spectrum Two FT-IR Spectrometer. In this note we show that the Spectrum Two™ FT-IR spectrometer (Figure 1) can be used to develop a quantitative method with sufficient sensitivity to meet the required detection limits for methanol, water, C3–C5 alcohols and gasoline denaturant, while requiring less than two minutes of analysis time per sample. Download Entire Application Note
  5. 5. CONTENTS TABLE OF a p p l i c at i o n n o t e FT-IR Spectroscopy Authors Dean H. Brown Richard Spragg PerkinElmer, Inc. Shelton, CT 06484 USA Instrumental Requirements for Accurate Analysis of Optical Abstract Components: A comparison of In the development of the Frontier™ the PerkinElmer 983 Dispersive Optica™, PerkinElmer has addressed the well known sources of error in the Spectrometer and the Frontier measurement of challenging optical materials with standard FT-IR instruments. Optica FT-IR Spectrometer The resulting improved performance over the previous standard of the optical industry is demonstrated by both the verification carried out internally, and also by that carried out by an external test laboratory. Introduction Measurements of optical components are some of the most challenging that can be made with an IR spectrometer (Figure 1). Since optical sensing systems can contain over 100 components, individual measurements require very high accuracy to minimize cumulative errors. The samples themselves present particular problems. Optical filters may themselves have 40 to 70 coating layers on a substrate with high refractive index. This affects the measurement by distorting the beam. They are often highly reflective, maximizing the potential errors from unwanted reflections. For years the PerkinElmer® 983 double-beam dispersive IR spectrometer has been the standard for this industry. However dispersive instruments take longer to acquire a spectrum and do not benefit from the other advantages of FT-IR.1Download Entire Application Note
  6. 6. CONTENTSTABLE OF a p p l i c at i o n n o t e Atomic Absorption Author Stan Smith PerkinElmer, Inc. Shelton, CT 06484 USA Analysis of Vanadium, Introduction Elemental analysis of fuel oil is an important Nickel, Sodium, and Iron step in quantifying its quality. Combustion of fuels containing metals can lead to the in Fuel Oils using formation of low melting-point compounds that are corrosive to metal parts. The pres- Flame Atomic Absorption ence of certain metals, even at trace levels, can deactivate or foul catalysts used during Spectrophotometry the processing of the oil. ASTM® International publishes numerous test methods for the analysis of petroleum products, including fuel oils. ASTM® D5863-00a (2005), “Standard Test Methods for Determination of Nickel, Vanadium, Iron, and Sodium in Crude Oils and Residual Fuels by Flame Atomic Absorption Spectrometry”, is an industry-standard method for the analysis of fuel oils. Due to its multi-element capabilities, inductively coupled plasma optical emission spectroscopy (ICP-OES) may be the preferred technique for petroleum analyses requiring many elements, however, flame atomic absorption spectrophotometry (FAAS) methods are still quite effective and rapid for smaller numbers of elements such as those required for fuel oil analyses. In addition, flame AA instrumentation is significantly more compact than ICP-OES instruments, costs a fraction of the price, and requires less operator training. Download Entire Application Note
  7. 7. CONTENTS TABLE OF a p p l i c at i o n n o t e FT-IR Spectroscopy Author Avdhut L. Maldikar, Ph.D. Perkin Elmer, Pvt. Ltd. Kasarvadavali, Thane (West) India Determination of Oil Introduction Compressed air sampling is very essential Content in Membranes from an environmental point of view, wherein it is required to know all the Used in Compressed Air environmental parameters such as SOx and NOx. These parameters are very Sampling by Infrared important to determine the air quality. Membranes used in compressor should be Spectroscopy oil free. Hence quantitative estimation of oil trapped in the membranes being used in air compressor is very important. FT-IR studies can be very effective in calculating the oil content in membranes to a very low level as well. This type of work is being carried out using FT-IR in the envi- ronmental segment using such tools as the Environmental Hydrocarbons FT-IR Analysis System (http://www.perkinelmer.com/Catalog/Product/ID/L160000S), which includes the Spectrum Two instrument and Spectrum Touch software with an application for oil in water measurement. This note describes the test method for the quantitative analysis of aerosol oil and liquid oil typically present in the air discharged from compressors and com- pressed air systems. The method is rapid, sensitive and cost effective and shows the FT-IR can be an effective tool for the monitoring of oil content. The meth- odology followed for the analysis by FT-IR is reported in BIS (Bureau of Indian Standard)1 and we have also tested for its ruggedness, spike recovery, linearity and detection limits.Download Entire Application Note
  8. 8. CONTENTSTABLE OF a p p l i c at i o n n o t e Elemental Analysis Organic Elemental Introduction Analysis of Soils – Understanding the health of the soil in which crops grow is fundamental in ensuring healthy yields. Two elements that are Understanding the essential to this are Carbon and Nitrogen, especially in their proportion to each other. This relationship is called the Carbon- Carbon-Nitrogen Ratio Nitrogen or CN ratio. This ratio is relatively simple to understand. If soil is made up of 30% Carbon and 2% Nitrogen then the CN ratio is 15 to 1. Carbon is important because of it’s energy content in the form of species such as carbohydrates, whereas Nitrogen is essential for growth. Average CN ratios vary from country to country depending on the predominant soil type, but a value between 8 and 17 is typical.1 Fertilizers, which are added to soils to regulate the CN ratio, should also be consid- ered. When organic matter is added to soil the breakdown of the content by bacteria and fungi causes changes in the CN ratio. It is important that any fertilizer added has sufficient nitrogen levels or the addition will have a negative effect. The addition of composted manure, which typically has a CN ratio of about 20:1, is desirable however the addition of sawdust, which has a high CN ratio of 400:1, could be disastrous.2 The microorganisms that break down the organic matter will very quickly run out of Nitrogen and therefore will start to consume the Nitrogen in the soil. This reduces the amount available to the plants and therefore depresses crop yield. In addition to these, both Carbon and Nitrogen can be further broken down into organic and inorganic subsections. Carbon in particular is often quoted as TOC, total organic Carbon, and TIC, total inorganic Carbon. TOC takes into account all the Carbon from such sources as decaying vegetation or bacterial growth. TIC includes all Carbon remaining so Carbon in the form of carbonates and bicarbonates, for example. Download Entire Application Note
  9. 9. CONTENTS TABLE OF a p p l i c at i o n n o t E FT-IR Spectroscopy Authors Ben Perston Aniruddha Pisal PerkinElmer, Inc. Shelton, CT 06484 USA Determination of Introduction The concentration of dispersed oil and grease in water is an important Hydrocarbons in parameter for human and environmental health. Infrared spectroscopy has long been a standard method for detecting and quantifying hydrocarbon Environmental contamination, particularly in water discharged during offshore oil operations.1 Samples with Recently, this analytical technique has enjoyed renewed interest and application to a wider range of environmental samples and matrices, from Spectrum Two cooling water, to soil in land reclamation, to drinking water; at the same time, concern over the environmental impact of chlorofluorocarbon solvents has led to the development of a number of alternative approaches using less harmful solvents. This application note presents an overview of three methods and a comparison of their performance: 1. Halogenated solvent extraction and transmission measurement (C–H stretch modes), e.g. ASTM® D7066. This is the traditional approach, but requires the use of relatively expensive solvents that may be harmful. 2. Hexane extraction and ATR measurement allows the use of an inexpensive hydrocarbon solvent, but does not permit the measurement of volatile contaminants. 3. Cyclohexane extraction and transmission measurement (1377 cm-1) exploits a deformation mode that is not present in the spectra of cycloalkanes (see Figure 1), and combines the simplicity of a transmission measurement with a hydrocarbon solvent.2 All three of these methods are supported by the Spectrum Two Environmental Hydrocarbons Analysis System (Figure 2), with the appropriate sampling accessory. This note evaluates the three methods and discusses their relative advantages.Download Entire Application Note
  10. 10. CONTENTSTABLE OF a p p l i c at i o n n o t e Gas Chromatography/ Mass Spectrometry Authors Lee Marotta Sr. Field Application Scientist Andrew Tipler Senior Scientist PerkinElmer, Inc. Shelton, CT 06484 USA Monitoring Volatile Introduction Beer is a popular beverage produced by the fermentation Organic Compounds of hopped malt extracted from barley and other grains. Although simple in concept, beer is a highly in Beer Production Using complex mixture of many compounds including the Clarus SQ 8 GC/MS sugars, proteins, alcohols, esters, acids, ketones, acids and terpenes. Flavor is an important quality of any and TurboMatrix Headspace beer and the chemical content of the beer is obviously responsible for that flavor. Aroma is an extremely Trap Systems important part of the flavor and so there is a strong interest by brewers in the volatile organic compounds (VOCs) in beer that affect its aroma. Some VOCs have a positive effect on aroma (attributes) and some have a negative effect (defects). The ability to characterize these in beer products before, during and after fermentation would be an important tool in process control, quality assurance and product development. This application note describes a system comprising a headspace trap sampler to extract and concentrate VOCs from a beer sample and deliver them to a gas chromatograph/ mass spectrometer (GC/MS) for separation, identification and quantification. The purpose of our experiments is to demonstrate that attributes and defects can all be monitored using one detector and from a single injection with mass spectrometry (MS). The associated benefits include a quicker return on investment, enhanced productivity, more information from a single analysis, and less bench space requirements. Download Entire Application Note
  11. 11. CONTENTS TABLE OF a p p l i c at i o n n o t e Atomic Absorption Authors Jijun Yao Renkang Yang Jianmin Chen PerkinElmer, Inc. Shelton, CT 06484 USA Accurate Determination Introduction Milk is one of the basic food groups in the human of Lead in Different diet, both in its original form and as various dairy products. The Chinese contaminated baby formula Dairy Products by scandal in 2008 has increased public awareness of contamination possibilities, and has lead to tighter Graphite Furnace Atomic supervision of dairy products as China is faced with demands – both from home and abroad – to improve Absorption Spectrometry its food safety record. It is well-known that lead (Pb) is toxic and causes damage to the nervous system; it has a particularly detrimental effect on young chil- dren1 and it has become a cause of major concern since the 1970s. As per World Health Organization (WHO) standards, the permissible limit of lead in drinking water is 10 µg/kg (parts per billion, ppb). Following an in-depth review of the toxicological literature, the Chinese guideline for maximum levels of lead content is set at 20 µg/kg (ppb wet weight) in infant formula (use of milk as a raw material measured by fluid milk diluted from powder, referring to the product ready-to-use) and at 50 µg/kg (ppb) in fresh milk, respectively.2 Lead analysis has traditionally been one of the major applications of graphite furnace atomic absorption spectrometry (GFAAS) worldwide. Currently, the Chinese regulatory framework approved standard methods for lead analysis has set GFAAS as the technique for the compulsory arbitration in food testing.3 In order to ensure protection of consumers, analysis should be sensitive, efficient, and cost-effective so that more effective monitoring can be accomplished. Because GFAAS is a mature technique, it is well-understood and routinely used by technicians and suitable for this determination. Sample preparation is an important part of an analysis and yet can be time consuming.Download Entire Application Note
  12. 12. CONTENTSTABLE OF a p p l i c at i o n n o t e Atomic Absorption Authors David Bass Senior Product Specialist Cynthia P. Bosnak Senior Product Specialist PerkinElmer, Inc. Shelton, CT 06484 USA The Determination of Toxic, Introduction Ingestion of trace elements from food Trace, and Essential Elements in can be linked to nutrition, disease, and physiological development. Whether they Food Matrices using THGA are needed for proper nutritional value or contain toxic elements, the presence of Coupled with Longitudinal major and minor elements in food needs to be verified to help determine health Zeeman Background Correction effects for the consumer. Contamination of food products may result from metals present during cultivation and/or processing. Acute or chronic exposure to heavy metals can lead to damaged nervous system function and have detrimental effects on vital organs. Food safety laboratories performing these analyses are often high-throughput facilities and require a detection tool that is efficient and cost effective. Unlike flame atomic absorption spectrophotometry (FAAS) where the ground state atoms quickly diffuse into surrounding air, graphite furnace atomic absorption spectrophotometry (GFAAS), being a total consumption technique, offers the ability to dry and atomize the entire pipetted sample in a more controlled environment within the graphite tube. This significantly increases sensitivity and provides superior detection limits with microliter (μL) sample volumes. Only ICP-MS can provide the same level of detection as GFAAS, however GFAAS is more cost efficient, simpler to operate and has fewer laboratory facility requirements. Download Entire Application Note
  13. 13. CONTENTS TABLE OF a p p l i c at i o n n o t e Gas Chromatography/ Mass Spectrometry Author A. Tipler, Senior Scientist PerkinElmer, Inc. Shelton, CT 06484 USA The Determination of Low Levels of Benzene, Toluene, Ethylbenzene, Xylenes and Styrene in Olive Oil Using a TurboMatrix HS and a Clarus SQ 8 GC/MS Introduction Levels of benzene, toluene, ethylbenzene, xylenes and styrene (BTEXS) are a concern in olive oil. These compounds find their way into olive trees and hence into the olives and olive oil mainly as a result of emissions from vehicles, bonfires, and paints into ambient air near the orchards. Various methods have been developed to detect and quantify these compounds down to levels of 5 ng/g (5 ppb w/w). This application note describes an easy to perform method using PerkinElmer® Clarus® SQ 8 GC/MS with a TurboMatrix™ 110 headspace sampler to achieve detection limits below 0.5 ng/g.Download Entire Application Note
  14. 14. CONTENTSTABLE OF a p p l i c at i o n n o t e Gas Chromatography/ Mass Spectrometry Author Timothy D. Ruppel PerkinElmer, Inc. Shelton, CT 06484 USA Benzoylecgonine in Introduction The United States Department of Health Urine by SAMHSA and Human Services (DHHS), Substance Abuse and Mental Health Services GC/MS Administration (SAMHSA) regulates urine drug testing programs in the Mandatory Guidelines for the Federal Workplace Drug Testing Program. These Mandatory Guidelines require a laboratory to conduct two analytical tests before a urine specimen can be reported positive for a drug, the initial drug test and the confirmatory drug test. The initial drug test is performed by immunoassay screening for the five drug classes (i.e., amphetamines, cocaine, opiates, phencyclidine and marijuana). Examples of immunoassay screening would include radioimmunoassay (RIA), enzyme immunoassay (EIA, EMIT) or others. Samples found positive to the immunoassay screening are subjected to a second confirmatory test by chromatographic separation and identification by mass spectrometry. SAMHSA defines the Method Quantification Cutoff Level as 100 ng/mL for benzoylecgonine, the major metabolite of cocaine. Download Entire Application Note
  15. 15. CONTENTS TABLE OF a p p l i c at i o n n o t e Gas Chromatography/ Mass Spectrometry Author Timothy D. Ruppel PerkinElmer, Inc. Shelton, CT 06484 USA Sympathomimetic Introduction The United States Department of Health Amines in Urine by and Human Services (DHHS), Substance Abuse and Mental Health Services SAMHSA GC/MS Administration (SAMHSA) regulates urine drug testing programs in the Mandatory Guidelines for the Federal Workplace Drug Testing Program. These Mandatory Guidelines require a laboratory to conduct two analytical tests before a urine specimen can be reported positive for a drug, the initial drug test and the confirmatory drug test. The initial drug test is performed by immunoassay screening for the five drug classes (i.e., amphetamines, cocaine, opiates, phencyclidine, and marijuana). Examples of immunoassay screening would include radioimmunoassay (RIA), enzyme immunoassay (EIA, EMIT) or others. Samples found positive to the immunoassay screening are subjected to a second confirmatory test by chromatographic separation and identification by mass spectrometry. SAMHSA defines the Method Quantification Cutoff Level as 250 ng/mL for each of 5 amines (AMP, MAMP, MDA, MDMA, MDEA).Download Entire Application Note
  16. 16. CONTENTSTABLE OF Case Pharmaceutical study Hyphenated “The DSC-Raman offers the advantage of collecting important DSC-Raman, data with one simple experiment which is not possible with any other instrument. It’s a powerful and exciting tool for material a new Powerful characterization in the early stage of drug development and can take us to the next level of analysis. It also has the potential to Research Tool. provide in-depth understanding of pharmaceutical systems.” – Research Investigator (a major U.S. pharmaceutical company) Differential Scanning Calorimetry (DSC) and Raman spectroscopy are comple- mentary analytical techniques. DSC measures thermal behaviors of samples like glass transition temperature (Tg), melting temperature and melting enthalphy, crystallization. While Raman gives insight into the chemical/physical structure of the sample, they are often used to address the same material characterization problem. Simultaneous DSC and Raman measurement offers more information about the material which may be missed by each technique separately. Spectra recorded continuously during the temperature scan can generate curves repre- senting the changes in the Raman spectra for direct comparison with the DSC heat flow curve. Download Entire Case Study
  17. 17. CONTENTS TABLE OF a p p l i c at i o n n o t e Thermogravimetric Analysis Authors E. Sahle-Demessie A. Zhao U.S. EPA, Office of Research and Development National Risk Management Research Laboratory Cincinnati, OH 45268 A. W. Salamon PerkinElmer, Inc. Shelton, CT 06484 USA A Study of Aged Carbon Nanotubes by Introduction Thermogravimetric Increased use of carbon nanotubes in consumer and industrial products have scientists asking about the implications of CNTs in Analysis our environment. Many end product applications include polymer composites, drug delivery systems, coatings and films, military applications, electronics, cosmetics, healthcare, among others. CNTs are desirable for many applications because of their high surface area to weight ratio. They are lightweight and highly elastic compared to carbon fibers, and deliver higher surface area for increased chemical interaction in its specific application. Thermogravimetry a simple analytical technique that is frequently used to characterize carbon nanotubes.1 The Pyris™ 1 TGA delivers accurate results quickly because of its low mass furnace. The Pyris 1 TGA low mass furnace has accurate temperature control and fast cooling for higher sample throughput.Download Entire Application Note
  18. 18. CONTENTSTABLE OF USEFUL LINKS View previous issues of our Spotlight on Applications e-Zine • Volume 1 • Volume 4 • Volume 7 • Volume 2 • Volume 5 • Volume 8 • Volume 3 • Volume 6 • Archives Access our application archives By Industry: • Consumer Products • Energy • Environmental • Food, Beverage Nutraceuticals • Forensics • Lubricants • Pharmaceutical Development Manufacturing • Polymers/Plastics NEW Clarus® SQ 8 GC/MS • Semiconductor Electronics Most sensitive solution for accurate food and environmental analysis By Technology: • Atomic Absorption (AA) • Elemental Analysis • Gas Chromatography (GC) • GC Mass Spectrometry (GC/MS) • Hyphenated Technology • ICP Mass Spectrometry (ICP-MS) Supra-Clean™ and Supra-Poly™ • Inductively Coupled Plasma (ICP-OES ICP-AES) • Infrared Spectroscopy (FT-IR IR) SPE Solutions • LIMS Data Handling • Liquid Chromatography (HPLC UHPLC) Finally, reproducibility comes to SPE • Mass Spectrometry • Raman Spectroscopy • Thermal Analysis • UV/Vis UV/Vis/NIR PerkinElmer, Inc. 940 Winter Street Waltham, MA 02451 USA P: (800) 762-4000 or (+1) 203-925-4602 www.perkinelmer.com For a complete listing of our global offices, visit www.perkinelmer.com/ContactUs Copyright ©2011, PerkinElmer, Inc. All rights reserved. PerkinElmer® is a registered trademark of PerkinElmer, Inc. All other trademarks are the property of their respective owners. 009855_01

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