Spotlight on Analytical Applications e-Zine - Volume 9

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SPOTLIGHT
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VOLUME 9

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INTRODUCTION
PerkinElmer Spotlight on Applications e-Zine – Volume 9
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CONTENTS

Energy & 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 Spectroscopy

Environmental
• Organic Elemental Analysis of Soils — Understanding the Carbon-Nitrogen Ratio
• Determination of Hydrocarbons in Environmental Samples with Spectrum Two

Food 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/MS

Forensics Toxicology
• enzoylecgonine in Urine by SAMHSA GC/MS
B
• ympathomimetic Amines in Urine by SAMHSA GC/MS
S

Pharmaceuticals Nutraceuticals
• yphenated DSC-Raman, a new Powerful Research Tool
H
• Study of Aged Carbon Nanotubes by Thermogravimetric Analysis
A

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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.

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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.

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.1


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Atomic Absorption

Author
Stan Smith
PerkinElmer, Inc.

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.


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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.


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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.


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

FT-IR Spectroscopy

Authors
Ben Perston
Aniruddha Pisal
PerkinElmer, Inc.

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.


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Gas Chromatography/
Mass Spectrometry

Authors
Lee Marotta
Sr. Field Application Scientist
Andrew Tipler
Senior Scientist
PerkinElmer, Inc.

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.


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Atomic Absorption

Authors
Jijun Yao
Renkang Yang
Jianmin Chen

PerkinElmer, Inc.

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.


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Atomic Absorption

Authors
David Bass
Senior Product Specialist
Cynthia P. Bosnak
Senior Product Specialist
PerkinElmer, Inc.

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.


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Gas Chromatography/
Mass Spectrometry

Author
A. Tipler, Senior Scientist
PerkinElmer, Inc.

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.


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Gas Chromatography/
Mass Spectrometry

Author
Timothy D. Ruppel
PerkinElmer, Inc.

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.


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Gas Chromatography/
Mass Spectrometry

Author
Timothy D. Ruppel
PerkinElmer, Inc.

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).


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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.

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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.

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.


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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

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