This document provides key analytical applications to help laboratories address the pressing concerns of the changing global landscape. Specifically, Volume 10 includes applications for Energy & Industrial, Environmental, Food & Beverage, and Pharmaceuticals & Nutraceuticals.
CNIC Information System with Pakdata Cf In Pakistan
Spotlight on Analytical Applications e-Zine - Volume 10
1. CONTENTS
TABLE OF
SPOTLIGHT
ON APPLICATIONS.
FOR A BETTER
TOMORROW.
VOLUME 10
2. CONTENTS
TABLE OF
INTRODUCTION
PerkinElmer Spotlight on Applications e-Zine – Volume 10
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. CONTENTS
TABLE OF
CONTENTS
Consumer Products
• Analysis of Consumer Products by Headspace Trap GC/MS using the Clarus SQ 8
• Spectroscopic In Vitro Method for the Calculation of Sunscreen SPF Values
A
Energy Industrial
• ICP-OES Analysis of FeCr Alloys Prepared by Sodium Peroxide Fusion
• ifferential Scanning Calorimetry Performance Comparison
D
• he Determination of C1 to C5 Hydrocarbons in Gas Streams Using the
T
PerkinElmer Swafer Technology
• nalysis of Wear Metals and Additive Package Elements in New and Used Oil
A
Using the Optima 8300 ICP-OES with Flat Plate Plasma Technology
Environmental
• Driving Productivity and Increasing the Speed of Analysis
• etermination of As, Se and Hg in Waters by Hydride Generation/Cold Vapor
D
Atomic Absorption Spectroscopy
Food Beverage
• oxic Trace Metals in Edible Oils by Graphite Furnace Atomic Absorption Spectrophotometry
T
• he Qualitative Characterization of Fruit Juice Flavor using a TurboMatrix HS Trap and
T
a Clarus SQ 8 GC/MS
• nalysis of Pb, Cd and As in Tea Leaves Using Graphite Furnace Atomic Absorption
A
Spectrophotometry
• uantification of Essential Metals in Spice Mixtures for Regulatory Compliance
Q
Using the Flame Atomic Absorption Spectrophotometry
Pharmaceuticals Nutraceuticals
• nalysis of Ginsenosides in Ginseng Root with the PerkinElmer Flexar FX-15 System
A
Equipped with a PDA Detector
• nalysis of Drug Substances in Headache Medicines with the PerkinElmer
A
Flexar FX-15 System Equipped with a PDA Detector
PerkinElmer
4. CONTENTS
TABLE OF
a p p l i c at i o n n o t e
Gas Chromatography/
Mass Spectrometry
Author
Ruben Garnica
Andrew Tipler
PerkinElmer, Inc.
Shelton, CT 06484 USA
Analysis of Consumer Fragrant soaps and detergents are a
ubiquitous part of our modern society and
Products by Headspace add a certain romance to what would
otherwise be mundane household chores.
Trap GC/MS using Great care and expense is spent in
formulating the exact mixture of fragrant
the Clarus SQ 8 organic compounds to differentiate
“apple blossom” or “crisp apple” from
simple “apple” scent. At the other end
of the spectrum are “fragrance-free” products – products that contain no
fragrance producing organics, natural or otherwise. Unfortunately the term
“fragrance-free” is unregulated and the actual composition of these products is
left to the manufacturer’s discretion. For both situations a comprehensive analytical
technique is necessary to measure both composition and quality of any volatile
organic compounds present. In this application brief we describe a quick and
simple analytical technique using headspace trap gas chromatography/mass
spectrometry (GC/MS) to determine the volatile fragrance compounds contained
in various consumer products.
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5. CONTENTS
TABLE OF
CASE
Consumer Products
STUDY
A Spectroscopic
In Vitro Method Introduction
The sun produces ultraviolet (UV) A and ultraviolet B
Author
for the Calculation rays that reach the Earth, which are part of an elec-
tromagnetic spectrum. UVA ray wavelengths range
Jillian F. Dlugos
of Sunscreen SPF from 400 nanometers to 320 nanometers, while UVB
rays range from 320 nanometers to 290 nanometers.
Glenelg High School
Glenelg, MD USA
Values UVA can penetrate both the upper layer of skin, the
PerkinElmer, Inc.
epidermis, as well as the lower layer of skin, the
Shelton, CT USA
dermis. It is most often responsible for damaging
keratinocytes in the epidermis, where skin cancer is typically found. UVB, although it
does not penetrate the dermis, is more intense because of it’s shorter wavelengths.
However, both can be extremely harmful to humans, as they can cause sunburns,
skin cancer, and other skin damage. In order to prevent these problems from happening,
sunscreen use is recommended. Sunscreen protects skin by either absorbing or reflecting
the harmful ultraviolet rays, preventing them from reaching the skin. Using sunscreen
while exposed to the sun can greatly reduce the chances of damaging skin cells and
developing cancer. For this study the PerkinElmer® LAMBDA™ 1050 equipped with
a 150 mm integrating sphere will be use to collect scatter transmission data for
sunscreen placed on a tape substrate. Testing sunscreen on a tape model of human
skin to calculate the SPF value is more convenient and economical than testing on
human skin.
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6. CONTENTS
TABLE OF
a p p l i c at i o n n o t e
ICP-Optical Emission Spectroscopy
Author
Chady Stephan
PerkinElmer, Inc.
Woodbridge, Ontario, Canada
ICP-OES Analysis Introduction
Ferroalloys, alloys of iron with sufficient
of FeCr Alloys amounts of one or more other elements
present (V, Mo, Cr, etc.), are important as
Prepared by Sodium a source of various metallic elements in
the production of all types of steels. They
Peroxide Fusion usually have low melting points and can
be incorporated readily into molten steel
where they provide a certain chemical
composition with specified properties.1
The ferrochrome alloy is produced by electric arc melting of the mineral chromite
(FeCr2O4). It is largely used for the production of stainless steels. Increasing the
amount of chromium content in the steel allows for increased corrosion and
oxidation resistance. Other alloying elements, such as nickel (Ni) or molybdenum
(Mo), aid in making the steel more passive and increasing its stainless properties.2
The presence of unwanted impurities in the metal and slag may alter reaction
temperatures and cause undesirable reactions of their own.1 The chemical analysis
of the chromite ore and its final products are mandatory to assess the quality
of the chromite ore and to optimize the grade of stainless steel production.
Analysis of waste products is also needed to optimize recovery of chromium and
other additives.2
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7. CONTENTS
TABLE OF
a p p l i c at i o n n o t e
Thermal Analysis
Author
Justin Lang Ph.D.
PerkinElmer, Inc.
710 Bridgeport Avenue
Shelton, CT 06484
Differential Scanning Introduction
Differential scanning calorimetry (DSC) is a commonly used
Calorimetry technique for studying polymeric, pharmaceutical, and energetic
materials. When considering which type of DSC to use to per-
Performance form a specified measurement one typically chooses either a
Power Compensation, or Heat Flux design. These instruments
Comparison are often referred to as double and single furnace DSC respec-
tively. PerkinElmer is the only vendor to provide both designs to
customers, because we believe that both technologies provide
unique advantages and users can choose the best type of DSC to meet their specific need.
One of the more common questions is how do the instruments data compare when perform-
ing a standard measurement? To answer this question, a standard polystyrene (PS) and low-
density polyethylene (PE) sample are tested using the conventional heat-cool-reheat method.
DSC 8000/8500
• PerkinElmer’s new flagship DSC 8000 and DSC 8500 was developed for the user’s need
for greater sensitivity and accuracy. They can be used for many applications including QA/QC
applications, studying processes in plastics and pharmaceuticals.
• The DSC 8000 provides outstanding sensitivity and reproducibility. It features PerkinElmer’s
proprietary double-furnace technology, which directly measures the heat flow between
two independent furnaces. It provides the most precise energy measurements over the
whole temperature range of any DSC in order to meet the most demanding applications.
There is an optional 96-position autosampler available and the DSC 8000 can be upgraded
to a DSC 8500.
• The DSC 8500, while providing all of the features of the DSC 8000, also offers HyperDSC®
heating and cooling with extremely fast controlled scanning rates and in-situ ballistic cooling
important for applications such as isothermal crystallization, polymorph/amorphous-material
studies and high sensitivity measurements.
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8. CONTENTS
TABLE OF
a p p l i c at i o n n o t e
Gas Chromatography
Author:
A. Tipler
PerkinElmer, Inc.
Shelton, CT 06484 USA
The Determination of Introduction
C1 to C5 Hydrocarbons The determination of light hydrocarbons in refinery and
in Gas Streams Using other gases is typically performed through the use of packed
columns and mechanical rotary valves. For example ASTM®
the PerkinElmer Method D-2597 adopts this approach. A gas sampling valve
delivers a small metered quantity of the sample gas into
Swafer Technology a non-polar packed column. The C1 to C5 hydrocarbons
are allowed to elute from this column and into a second
packed column with a polar stationary phase. At that point
a rotary valve is actuated to reverse the flow of carrier gas through the precolumn and backflush any
residual sample in that column to a detector to determine the total C6+ content in the sample. In the
meantime, chromatography of the C1 to C5 content proceeds on the second column for separation,
identification and quantification. The whole analysis takes about 20 minutes and getting acceptable
chromatographic separation is often a challenge because of normal variations in the columns.
In this application note, a new method is described for this analysis that uses a Swafer™ backflushing
technology with capillary columns under isothermal conditions to both improve the chromatographic
separation and to reduce the analysis cycle time to just over 5 minutes.
Experimental
For this analysis, an S-Swafer is used to manage the backflushing operations on the precolumn rather
than a more conventional mechanical valve. The S-Swafer uses the Deans pressure balanced technique
to reverse gas pressures across a GC column to initiate the backflushing process. Such systems have
been widely used for 50 years – particularly for capillary columns where low thermal mass, inertness
and low dead volumes are critical.
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9. CONTENTS
TABLE OF
a p p l i c at i o n n o t e
ICP-Optical Emission Spectroscopy
Author
David Hilligoss
PerkinElmer, Inc.
Shelton, CT USA
Analysis of Wear Metals
and Additive Package Introduction
Elements in New and The analysis of new and used oil for concentration trends of
wear metals and for formulation or depletion of additive package
Used Oil Using the metals has been around for over 30 years. Wear metals such
as copper (Cu) and iron (Fe) may indicate wear in an engine
Optima 8300 ICP-OES or any oil-wetted compartment. Boron (B), silicon (Si) or sodium
(Na) may indicate contamination from dirt or antifreeze leading
with Flat Plate Plasma to a failure. Additive elements such as calcium (Ca), phosphorus
Technology (P) and zinc (Zn) are analyzed for depletion which contributes
to wear since these elements contribute to certain key lubri-
cation characteristics. A sound maintenance program, which
routinely measures metals in the lubricating oils, not only
reduces the expense of routinely dismantling the components for visual inspection, but
can indicate unexpected wear before component failure.
Atomic absorption spectrometers (AAS) were first used for these applications in the early-
to-mid 1960s. As the number of elements and samples grew over the years, inductively
coupled plasma-optical emission spectrometers (ICP-OES) were used for oil analysis.
Today, many oil analysis labs will handle between 500 to 2000 samples per day and
analyze from 15 to 24 elements per sample.
Many improvements to ICP technology have taken place over the years with the most
recent being the replacement of the helical load coil used to generate the plasma. The
Optima™ 8x00 ICP-OES series (Figure 1 – Page 2) utilizes the new Flat Plate™ plasma technology
that replaces the traditional helical coil design used since the inception of the inductively
coupled plasma. The Flat Plate plasma technology utilizes two flat induction plates
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10. CONTENTS
TABLE OF
Case
study Environmental
Driving Productivity
and Increasing the South West Water is
responsible for maintaining
Speed of Analysis and monitoring the quality
of drinking and bathing
waters and the sewage
system network in a region of England. They do this effectively through a
central analytical facility. In early 2010, as part of the rolling replacement
programme, the ICP-MS instrument was identified as due for renewal. The
analytical team were looking for an instrument that could be relied upon to
have minimum downtime and be a workhorse for high sample throughput;
but also offer flexibility to adapt to changing business requirements and
complete investigative work if required. After the evaluation of the top three
suppliers, the NexION® 300 ICP-MS from PerkinElmer was selected. The
flexibility offered by NexION having both a collision and dynamic reaction
cell ensures that the lab is future proofed. Being fully prepared to handle
any changes in sample matrices and still benefit from sensitive, reproducible
results day in day out.
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11. CONTENTS
TABLE OF
a p p l i c at i o n n o t e
Atomic Absorption
Author
Aaron Hineman
PerkinElmer, Inc.
Ontario, Canada
Determination of As, Introduction
Contamination of industrial and municipal water
Se and Hg in Waters by supplies with arsenic (As), selenium (Se), and mercury
(Hg) can occur from natural deposits, industrial
Hydride Generation/ discharge, runoff from mining, landfill and agricultural
operations. Consumption of contaminated water can
Cold Vapor Atomic cause skin damage (As), kidney and nervous system
damage (Hg) and numbness in the fingers and toes
Absorption Spectroscopy (Se).1 The U.S. Environmental Protection Agency
(EPA) and the Canadian Council of Ministers of the
Environment (CCME) have guidelines on the concen-
tration of As, Se and Hg for the protection of marine
and freshwater aquatic life and the protection of agriculture.1,2 Due to the low levels of
these guidelines for As, Se, and Hg, it is important to have analytical measurements that are
precise and accurate with low amounts of noise.
Hydride generation (HG) is a very effective analytical technique developed to separate
hydride forming metals, such as Se and As, from a range of matrices and varying acid
concentrations. The heated quartz tube atomizer is particularly useful for the determination
of arsenic and selenium because the absorption wavelengths for these elements are below
200 nm in an area subject to intense interference from flame radicals that can significantly
affect detection limits. Mercury can be easily reduced in solution to generate elemental
mercury, otherwise known as cold vapor (CV). This technique is also effective at separating
mercury from a range of matrices. These analytical techniques can improve detection limits
by a factor of approximately 3000 times that of flame detection limits and typically have less
interference than graphite furnace techniques.
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12. CONTENTS
TABLE OF
a p p l i c at i o n n o t e
Atomic Absorption
Authors
Surasak Manarattanasuwan
Senior Inorganic Product Specialist
PerkinElmer, Inc.
Thailand
Toxic Trace Metals Introduction
Graphite furnace atomic absorption spectropho-
in Edible Oils by tometry (GFAAS) has been widely applied to the
determination of trace elements in food due to
Graphite Furnace its selectivity, simplicity, high sensitivity, and its
capability for accurate determinations in a wide
Atomic Absorption variety of matrices. Edible oils are generally
low in trace element concentrations, however,
Spectrophotometry metals such as arsenic (As), lead (Pb), cadmium
(Cd), chromium (Cr), and selenium (Se) can be
found and are known for their toxicities which
affect the health of consumers. The determination
of toxic elements from naturally occurring or production-contamination sources
in oils can be determined by using GFAAS or inductively coupled plasma mass
spectrometry (ICP-MS). When only a few elements are being analyzed, GFAAS is
the preferred choice. It is easy to learn, faster in setting up, and simpler to use
than ICP-MS. GFAAS is also lower in initial capital investment and has a lower
operating and maintenance cost. Sample pretreatment procedures for edible
oils are normally required prior to instrumental analysis in order to eliminate the
organic matrix. Wet, dry or microwave digestion, dilution with organic solvent,
and extraction methods can be time consuming and require more operator training
than a direct analysis method.
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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 Qualitative Characterization
of Fruit Juice Flavor using a
TurboMatrix HS Trap and
a Clarus SQ 8 GC/MS
Introduction
The PerkinElmer® TurboMatrix™ Headspace Trap system coupled with a Clarus®
SQ 8 GC/MS is a very convenient means of identifying low concentration volatile
organic compounds (VOCs) in foodstuffs. In this application note, the VOCs in
various fruit juices were investigated. Sample preparation simply involved dispensing
a fixed volume of fruit juice into a sample vial and sealing it. The analysis was
fully automated.
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14. CONTENTS
TABLE OF
a p p l i c at i o n n o t e
Atomic Absorption
Author
Praveen Sarojam, Ph.D.
PerkinElmer, Inc.
Shelton, CT 06484 USA
Analysis of Pb, Cd and As in Introduction
Tea is drunk by about half of the world’s
Tea Leaves Using Graphite population. It is widely cultivated and
consumed in Southeast Asia. Tea is rich
Furnace Atomic Absorption in many trace inorganic elements.1,2
In addition to many essential elements
Spectrophotometry required for human health, some toxic
elements may also be present in tea
leaves. This could be due to polluted soil,
application of pesticides, fertilizers or industrial activities. There is often little information
available about the safety of tea leaves and finished tea products with respect to heavy
metal contamination. Due to the significant amount of tea consumed, it is important to
know the toxic metal contents.
The toxicity and effect of trace heavy metals on human health and the environment has
attracted considerable attention and concern in recent years. Among the heavy metals, lead
(Pb), cadmium (Cd) and arsenic (As) are especially toxic and are harmful to humans even
at low concentrations. They have an inherent toxicity with a tendency to accumulate in the
food chain and a particularly low removal rate through excretion.3 Exposure to heavy metals
above the permissible level can cause high blood pressure, fatigue, as well as kidney and
neurological disorders. Heavy metals are also known to cause harmful reproductive effects.4
A major challenge in the analysis of tea leaves is the extremely low analyte levels and the
very high matrix levels. For many years, graphite furnace atomic absorption spectrophotometry
(GFAAS) has been a reliable technique and the preferred method for this analysis. The use of
longitudinal Zeeman background correction and matrix modifiers help to achieve extremely
low detection limits in high matrix samples such as tea leaves, making GFAAS an indispensible
tool for carrying out such analyses.
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15. CONTENTS
TABLE OF
a p p l i c at i o n n o t e
Atomic Absorption
Author
Praveen Sarojam, Ph.D.
PerkinElmer, Inc.
Shelton, CT 06484 USA
Quantification of Introduction
Foods, together with water, provide the major proportion of
Essential Metals the total daily intake of trace elements by humans. Spices
and vegetables are some of the most common foods in the
in Spice Mixtures human diet around the world. Besides polluted soil and
water, foods can also be contaminated with trace metals by
for Regulatory the introduction of mechanized farming, the increasing use
of chemicals, food processing and packaging, etc. In order
Compliance Using to minimize adverse impact, it is important to measure and
continuously monitor the levels of trace elements in various
Flame Atomic kinds of food materials. Trace element food composition data
are also important for both consumers and health professionals.
Absorption In recent years, food labeling legislation has enforced this
Spectrophotometry requirement. Trace element determination in complex matrices,
such as food, often requires sample preparation prior to
determination by instrumental techniques.1
Cobalt (Co), copper (Cu), manganese (Mn), nickel (Ni) and zinc (Zn) are all essential elements,
not only for mammals, but also for plants. They play important roles in many biological processes
including carbohydrate and lipid metabolism.2 For example, a daily copper intake of 1.5 - 2.0 mg
is essential and copper at nearly 40 ng/mL is required for normal metabolism of many living organisms.3
However, copper at higher levels is toxic to the circulatory system and kidneys. The trace element
content of food items for all the essential elements mentioned above must be controlled on a daily basis.
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16. CONTENTS
TABLE OF
a p p l i c at i o n n o t e
UHPLC
Author
Njies Pedjie
PerkinElmer, Inc.
Shelton, CT 06484 USA
Analysis of Ginsenosides Introduction
The root of the panax genus plant (also
in Ginseng Root with the called Ginseng) has been used as an herbal
medicine in Asia for over two thousand
PerkinElmer Flexar FX-15 years for its purported various health
benefits, including (but not limited to),
System Equipped with a antioxidant, anticarcinogenic, anti-
inflammatory, antihypertensive and
PDA Detector anti-diabetic. The pharmacologically
active compounds behind the claims of
ginseng’s efficacy are ginsenosides; their
underlying mechanism of action although
not entirely elucidated appears to be similar to that of steroid hormones. There
are a number of ginseng species, and each has its own set of ginsenosides. In
fact, more than forty different ginsenosides have been identified. Ginsenosides
are a diverse group of steroidal saponins with a four ring-like steroid structure
with sugar moieties (Figure 1); they are found exclusively in ginseng plants and
are in higher concentration in their roots. There are two main groups of ginsen-
osides: the panaxadiol group or Rb1 group that includes Rb1, Rb2, Rc, Rd, Rg3,
Rh2, and Rh3; and the panaxatriol group or Rg1 group that includes Rg1, Re, Rf,
Rg2 and Rh1.
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17. CONTENTS
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a p p l i c at i o n n o t e
UHPLC
Author
Njies Pedjie
PerkinElmer, Inc.
Shelton, CT 06484 USA
Analysis of Drug Substances Introduction
Acetaminophen and aspirin are the drugs
in Headache Medicines of choice used to relieve the symptoms
of common headache. Acetaminophen,
with the PerkinElmer Flexar which is also called paracetamol, is widely
used as a pain reliever (analgesic) and
FX-15 System Equipped fever reducer (antipyretic). Because of
its fast onset (eleven minutes after intake),
with a PDA Detector acetaminophen is very effective. However,
every year its misuse (dose exceeding the
daily adult limit of four grams) can cause
fatal liver damage. In fact, acetaminophen
toxicity is the main cause of acute liver failure and accounts for most drug over-
doses in the United States. The other common active ingredient in headache
medicines is acetylsalicylic acid (aspirin), which is an analgesic, antipyretic and
anti-inflammatory drug. Despite its usefulness, aspirin has a harmful side effect.
For many people it can cause or exacerbate gastrointestinal ulcers by destroying
the mucosal lining. This is a major setback for a medicine that is otherwise very
inexpensive and can also be used for its antiplatelet effect to prevent heart
attack and stroke. In formulations specially designed to treat common headaches
(tension headache), acetaminophen and aspirin are often combined with caffeine.
In these formulations, caffeine not only increases the effectiveness of the two
drugs but it also stimulates the central nervous system and temporarily wards off
tiredness.
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