shimadzu | - pau winterplasma 2019...shimadzu edx-720 element analysis: edx-rf sample preparation:...
TRANSCRIPT
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Collaboration:
Pau Winterplasma 2019
Project: Short Description
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Introduction: Problem
Plastic production is all time high: 335 MT worldwide 2016 (Plastic Europe
2017)
Thermoplastics are a
versatile material. Tailor
made for application.
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Momentary Risk Assesment
Plastic waste in the environment is also all time high, estimated release in
oceans yearly 8 Million Ton (Lambeck et al. 2015).
Momentary risk assesment environmental plastic is mainly based on
studies of pristine or virgin pellets. But complexity grows during producing
tailor made consumer products: additives, like colorants, are added.
Reference materials for PLASTOX.
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Restricted metalls in the environment
Shore river Rhein XantenCd: 4152 ppm
Beached TexelCd: 3692 ppm
Eaten FulmarCd: 2171 ppm
Eaten FulmarPb: 130 ppm
Inhertance of the past in the environement.
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Classification: 14 groups
Collecting the right sample
Goal: preparation of a more correct environmental
sample for further analysis: PTX001.
Composition of PTX001 is based on a beach clean up,
Texel (Van Franeker, 2005).
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Collecting the right sample, composition
WMR prepared 5 batches of 1 kg
Each batch contained 351 samples
of plastic.
Identification of 351 samples with FTIR-ATR.
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Sample preparation of 14 groups is reduced to 4 and fragmentated with
cryogenic (LN) ultra centrifugal milling:
- Ropes and nets
- Sheets
- Foam
- Rest
Homogenized
(w/w) to PTX001
Preparation of the right sample
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EDX-RF:
Shimadzu EDX-720
Element analysis: EDX-RF
Sample preparation: none, prepared samples can be used.
Callibration: restricted on 7 elements, more information: see paper.
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Results: EDX-RF
Limitations EDX-RF:
- Sample matrix (crystallinity varies)
- Sensitivity Na, Mg, Al and P low
- Callibration (solid): labour intensive and expensive
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ICP-OES:
Shimadzu ICPE-9000
Sample preparation:
microwave digestion (CEM
Mars 5) in HNO3 (65%).
(More information: see paper.)
Callibrated: 34 elements, more information: see paper.
Element analysis: ICP-OES
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Results: ICP-OES
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ICP-MS: measurements done by SINTEF (Norway)
Agilent 8800 Triple Quadrople
Sample preparation: microwave digestion (Milestone Ethos) in HNO3 and
HF. (More information: see paper.)
Callibrated: 13 elements, more information: see paper.
Element analysis: ICP-MS
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Results: ICP-MS
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Main results are comparable.
Comparision results
Samples ICP-OES, ICP-MS
and EDX-RF are from different
batches.
These first results show that an environment sample for laboratory
studies can be prepared.
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Some remarkeble results
Al: Colorant and barrier
Br: flame retardant?
Sb: catalyst PET
Cd: colorant and stabiliser
To describe
elements in
plastic and their
possible effects:
further research
is necessary
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Preparation of environmental relevant samples isn‘t easy.
Beaches are flooded with the legacy of the past.
Some thoughts….
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Questions?
Thank you for your attention