Lab Report 18 - 12 - 2023

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Lab report 18/12/2023

Raman spectroscopy and micro plastic extraction


By: Wessel Du Plessis

Aim:
The objective of the microplastics extraction process was to isolate plastic particles from
beach sand and concentrate them onto filter paper for further analysis to determine their
types and abundance. This was achieved using density separation and a Raman
spectrometer.

Method:
Density separation method:
1. Transfer 100 ml of KCOOH solution and 100 ml of pure water to clean beakers
(washed with Isopropyl alcohol).
2. Measure the weight of an empty pycnometer, fill with deionized water
3. Subtract the weight of the vessel from the total leaving only the weight of the water.
The beaker weighed 72.704g. After water was added the total weight was 128.995g.
128.995g - 72.704g = 56.251g at 21.5 c°. The density is thus 0.997882.
4. Add potassium sorbate to the pycnometer. Then weigh, the total weight is 142.123g.
142.123g - 72.704g = 69.419g at 21.5 c°, the density is thus 1.232.
5. Measure a 100g of sediment and mix it with 100g of KCOOH solution. Using a
magnetic stirrer, stir for 5 min. It should then be rested for at least 30 min.
6. Transfer the supernatant to a clean beaker, by slowly pouring the liquid out trying not
to disturb the sediment.
7. Set up a vacuum filter. Filter the supernatant being careful not to add too much liquid
as microplastics can stick to the surface of glass.
8. The residue left on the filter will be a mixture of sand particles and plastics as plastics
tend to have a lower density than sand and would thus have drifted to the top of the
denser solution.

Raman spectroscopy:
1. Turn on the spectrometer and the computer.
2. Place the filter with the extracted micro plastics on the stage. Then look for plastics to
analyse. Once an interesting piece has been found, activate the laser.
3. It is important to note that plastics have a low melting point so it's best to use the
laser at a lower power setting as it can burn a hole in the sample.
4. Once the laser is activated you will receive a graph on the computer in it will be
information about the Raman shift. The amount of shift and where the peaks are
located will indicate the type of plastics that are found.
5. The more pieces that are investigated the more accurate the measurement will be,
thus it is best to map the sample by letting the laser scan as many points as possible.
This can be done by setting the laser to mapping and letting it run for an hour or two.
Results:
The analysis revealed the presence of microplastics. These microplastics were further
characterised using a Raman spectrometer, which yielded two distinct peaks: green peaks
corresponding to polystyrene and red peaks corresponding to polypropylene.

Image 1: Two lines red(likely polypropylene) and green(likely polystyrene). These were the
two analyses done by the Raman spectrometer. The reason that the word likely is used is
because it may be hard to determine the exact composition of the plastic as it decays and
further analysis will be necessary.
Image 2: Contains a picture of microplastics in their various forms. And a scale that indicates
the size of the pieces, namely, fibres (a, b), fragments (c, d), films (e, f), and pellets (g, h).
Microplastic pollution in urban green-belt soil in Shihezi City, China - Scientific Figure on
ResearchGate. Available from:
https://www.researchgate.net/figure/Images-of-microplastics-obtained-using-stereomicrosco
pe-namely-fibers-a-b-fragments_fig3_359772257 [accessed 26 Dec, 2023]

Discussion:
The detection of microplastics in the sample was unsurprising, given their ubiquity in the
environment. The separation method employed can be tailored to selectively capture
different types of plastic, as these materials exhibit a wide range of properties. This
adaptability is crucial for comprehensive microplastics analyses. For instance, high-density
plastics may not be effectively separated using potassium formate, a commonly used
separation solution. The preference for potassium formate stems from its relatively benign
environmental impact compared to alternative methods.

Conclusion:
A comprehensive assessment of microplastic distribution and types in Baltic Sea sand
necessitates a more exhaustive mapping of the sand samples. By contributing to this
database, this experiment will facilitate future research efforts in identifying the types of
plastics present in Baltic Sea sediments.

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