Volume 37 – FAE • June, 2012 | Analytical Sciences and Laboratory Services

FOOD
AGRICULTURE
ENVIRONMENTAL

Harnessing the Power of FT-IR to

Guarantee Water Safety
Ben Perston PhD, Applications Scientist, Molecular Spectroscopy, PerkinElmer Chalfont Road, Seer Green, Beaconsfield HP9 2FX, UK

Aglobal risk to environmental and task and recycled water is one of the
human health largest contributors to offshore oil
pollution1, eventually causing surface
Pollution of water with oil and grease is contamination and smothering marine
a significant risk to human and life. Long term impacts, including acute
environmental health; therefore, toxic effects, can also be caused by
effective detection and measurement of specific chemical components of the oil2.
hydrocarbon contamination is essential. This potential for harm emphasises the
Infrared(IR) spectroscopy has long been a importance of rapid and accurate
standard method for measuring analytical methods that can be deployed
dispersed oil and grease in processwater in a variety of environmental testing
discharged from offshore oil operations, applications.
and has more recently gained application
to a widerrange of environmental Terrestrial sources of pollution are also
samples and matrices. Contamination responsible for a significant fraction of
incidents creating health hydrocarbon pollution in coastal waters
andenvironmental problems can range and sensitive environments like estuaries
from major oil spills to small scale and wetlands: river and urban runoff
domestic disposal. sources contribute 20% of petroleum
pollution within our oceans3.
Large amounts of water are extracted Accordingly, companies that discharge
during offshore oil operations, and this water into rivers or municipal drains are
must be separated from the oil prior to typically required to comply with Figure 1: Sample deposition for the HATR
being discharged back into the sea. discharge permits that specify limits of method, constraining the sample to the most
brightly illuminated portion of the crystal
However, the separation is not a simple potentially hazardous materials,
Fresh Volume 37 – FAE • June, 2012

a crystal through which the light passes

by total internal reflection. The
evanescent wave created just above the
surface of the crystal can be absorbed by
the sample, allowing a spectrum to be
measured. To apply this technique to
measuring oil in water, the sample is
extracted with a volatile hydrocarbon
solvent, such as hexane. An aliquot of
the extract is deposited on the ATR
crystal (Figure 1) and the solvent allowed
to evaporate, leaving the oil behind. The
IR spectrum is then measured, and the
including hydrocarbons, to ensure that spectroscopy for detecting and oil concentration calculated from the
long-term environmental damage is quantifying hydrocarbon contamination. intensity of the absorption
averted. Ideally, this testing can be The three methods discussed here are
Cyclohexane Transmission
carried out on-site, ensuring a rapid suitable for use across a variety of
The third method considered here
response to any problems encountered. different applications concerning
exploits a vibrational mode that is
hydrocarbon contamination.
Soil is an equally important part of the characteristic of hydrocarbons containing
–CH3 groups, and thus is not present in
environment, and is just as vulnerable to Halogenated solvent extraction
pollution. Petroleum pollution can render The first of these methods, ASTM the spectra of cycloalkanes such as
polluted areas not only unfit for D7066, still employs a halogenated cyclohexane. It thus combines the
development but also dangerous for solvent, but one that is less damaging to simplicity of a transmission measurement
nearby communities and ecosystems. the environment: a mixture of dimers with the use of a convenient
Hydrocarbons can easily pass into and trimers of chlorotrifluoroethylene. hydrocarbon solvent. This method allows
groundwater, making it unfit for use. If This method employs a traditional long- rapid measurement with a non-
land is to be reclaimed for other uses pathlength measurement of C–H halogenated solvent and can achieve
after decommissioning an oil or gas stretching absorptions that not only has useful sensitivity. The cyclohexane
facility, extensive testing must be carried the benefit of being standardised and method shows that it is possible with
out to ensure that the soil has not been trusted, but also affords excellent modern instrumentation, such as the
contaminated. In the event of a spill sensitivity, with detection limits well Spectrum Two instrument from
being discovered, a rapid, portable below 1 ppm readily obtained4. The PerkinElmer. In applications where sub-
analysis method can be used to make same methodology can be employed parts per million (ppm) detection is not
numerous measurements to accurately with tetrachloroethylene as the solvent necessary and it is desirable to avoid
delineate the extent of the spill. (this is also relatively environmentally halogenated solvents, this approach may
safe and widely used for dry cleaning be ideal.
IR testing of water and soil and metal degreasing, but has been
Although highly effective and well Although the use of FT-IR in the
classed as a probable carcinogen by the
established for the measurement of determination of oil in water is a classical
EPA5). A drawback of the method is the
hydrocarbons in water, historically analytical method, the environmental
expense involved in obtaining solvents
popular IR methods have raised issues concerning the use of CFCs
with the very low levels of hydrocarbon
environmental concerns themselves due associated with traditional IR analyses
residue required in order to avoid
to the use of ozone-depleting cannot be ignored, and alternative IR
interference with the analysis.
chlorofluorocarbon (CFC) solvents in the methods should be considered, bearing
sample extraction process. These Hexane extraction with IR in mind the real sensitivity requirements
environmental concerns have led to the measurements using attenuated of the analysis.
development of a number of alternative total reflection
approaches to IR analysis of oil pollution, Attenuated total reflection (ATR) For more detail applications of this
employing less harmful solvents. This measurement takes a different approach type please write to
[email protected]
note explores more environmentally- to transmission IR. Instead of passing
or log on to www.perkinelmer.com
friendly approaches to the use of IR light through the sample, it is placed on
Fresh Analytical Sciences and Laboratory Services

Accurate Determination of Lead in

Different Dairy Products
Milk is one of the basic food groups in
the human diet, both in its original form
and as various dairy products. The
Chinese contaminated baby formula
scandal in 2008 has increased public
awareness of contamination possibilities,
and has lead to tighter supervision of
dairy products as China is faced with
demands – both from home and abroad
– to improve 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 childrenand it has become a cause
and routinely used by technicians and by automated analysis using GFAAS. This
of major concern since the 1970s. As per
suitable for this determination. Sample method minimizes sample preparation,
World Health Organization (WHO)
preparation is an important part of an and also reduces potential contamination
standards, the permissible limit of lead in
analysis and yet can be time consuming. while still maintaining the speed of
drinking water is 10 μg/kg (parts per
analysis.
billion, ppb). Following an in-depth Generally, milk is an emulsion or colloid
review of the toxicological literature, the of butterfat globules within a water- A PerkinElmer® PinAAcle™ 900T flame
Chinese guideline for maximum levels of based fluid. The exact components of and longitudinal Zeeman atomic
lead content is set at 20 μg/kg (ppb wet raw milk vary by different animal species, absorption spectrometer can be usedfor
weight) in infant formula (use of milk as but it contains significant amounts of the GFAAS measurements of lead (Pb) in
a raw material measured by fluid milk lactose, fat, protein and minerals as well different milk samples. The PinAAcle
diluted from powder, referring to the as vitamins. Due to the relative 900T spectrometer’s transverselyheated
product ready-to-use) and at 50 μg/kg interference resulting from such a graphite atomizer (THGA) with
(ppb) in fresh milk, respectively. complex matrix, complete decomposition Longitudinal AC Zeeman background
of milk samples prior to instrumental correction provide a constant
Lead analysis has traditionally been one
measurement by microwave or heating uniformtemperature distribution across
of the major applications of graphite
block acid digestion is generally the entire length of the graphite tube.
furnace atomic absorption spectrometry
recommended. This approach, however, This allows a full implementation of
(GFAAS) worldwide. Currently, the
is more time-consuming and poses a theStabilized Temperature Platform
Chinese regulatory framework approved
more rigorous requirement on quality Furnace™ (STPF) technique in graphite
standard methods for lead analysis has
assurance than simple dilution when furnace analysis where we can analyze
set GFAAS as the technique for the
concentrations of lead are to be complex sample matrices using aqueous
compulsory arbitration in food testing.3
determined at μg/kg level in the final standard solutions as calibration for
In order to ensure protection of
solution which is extremely sensitive to suspended sample solutions to get
onsumers, analysis should be sensitive,
reagent blank contribution and accurate and precise results. Maximum
efficient, and cost-effective so that more
environmental contamination. To atomic signals can be obtained with
effective monitoring can be
overcome these issues, this work minimum memory effect and potential
accomplished. Because GFAAS is a
describes a simple and direct dilution interference.
mature technique, it is well-understood
method for sample preparation, followed
Fresh Volume 37 – FAE • June, 2012

For detail method and Comparison of lead levels in different

experimental conditions click on dairy-product samples obtained by two
this link. Or contact independent test methods:
[email protected] A) dried milk powder samples; B) liquid
milk samples.
For additional independent comparative
It is important to emphasize that there
data against GFAAS analysis using this
are no significant differences between
simple method, all collected dairy
the two independent testing methods,
products analyzed for lead by ICP-MS.
which further demonstrates the accuracy
Where it shows the concentrations of Pb
of the overall methods. However, the
found in each dairy product
Sample was matching with the results relative standard deviation (RSD) was
obtained with PinAAcle 900 Aas. generally higher for data obtained by
ICP-MS analysis after conventional
mineralization. This is most likely due to
the dilution introduced during the
digestion step used in the ICP-MS sample
preparation. Even though the ICP-MS
technique is more sensitive than GFAAS,
the dilution of the extremely low levels
of Pb present in the samples introduces
additional uncertainty. Based on the
results, it clearly appears that total
digestion of matrix components is
unnecessary with all these types of dairy-
PinAAcle 900 T Atomic absorption product samples, and it is more rapid
spectrometer with Zeeman furnace and economical to run the sampleswith
minimal preparation.

World Milk Day- 1st June 2012

Milk is a near perfect food source loaded the growth of the world economy since
with nine essential nutrients needed daily 1945.
to keep bodies healthy and strong.
In 1996, representatives from many
The Food and Agriculture Organization nations across the globe came together
(FAO) of the United Nations which is an at the first World Food Summit with the
intergovernmental organization goal to cut hunger in half by 2015. The
consisting of 191 Member Nations with work to achieve this goal propelled the
the mission to make sure people have creation of the UN Millennium
regular access to enough high-quality Development Goals in 2000. These eight
food to lead active, healthy lives started developmental goals relate to education,
celebrating the first World Milk Day on nutrition and environmental
June 1st, 2001. FAO has been working sustainability to ensure healthy foods to
to raise levels of nutrition, improve nourish every human being on the
agricultural productivity, better the lives planet.
of rural populations and contribute to
Fresh Analytical Sciences and Laboratory Services

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