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Functionalized glass fiber filters for the simultaneous sampling of vapour and particle phase PCDD/Fs and dl-PCBs

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Functionalised filber filters were used for the sampling of PCDD/Fs and dl-PCBs, and their performances were compared to normal filters. Results show that these devices can efficiently retain PCDD/Fs and PCBs without using an adsorbent cartridge, thus avoiding all disadvantages previously discussed (blank artefacts, costs, encumbarance). As a further development, these devices might be easily used in automated samplers, as well as in personal samplers for occupational hygiene applications.
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Functionalized glass fiber filters for the
simultaneous sampling of vapour and
particle phase PCDD/Fs and dl-PCBs
Valerio Paolini1,2, Ettore Guerriero1, Paolo Benedetti1,
Silvia Mosca1, Marina Cerasa1, Mauro Rotatori1, Alessandro Bacaloni2
1 National Research Council of Italy , Institue of Atmospheric Pollution Research (CNR IIA)
2 Sapiernza University of Rome, Chemistry Department
36th International Symposium on Halogenated Persistent Organic Pollutants
Florence, August 28th - September 2nd 2016
PCDD/Fs and dl-PCBs air sampling
2
Filters do not retain the total amount of analytes:
Vapour/particle partitioning
Desorption (and ab/adsorption) phenomena
Filter/adsorbent sampling:
PUF (polyurethane foam), XAD (microporous styrene/divinylbenzene) etc
Does the adsorbent/filter ratio gives the atmospheric vapour/particle partitioning?
PCDD/Fs and dl-PCBs air sampling
3
Other adsorbent problems:
Reuse or not: higher sampling costs or higher sampling blanks?
Size problems with personal/automated samplers
Accelerated (pressurised) solvent extraction vs Soxhlet
Simultaneous filtering and adsorbing device
Simultaneous filtering and adsorbing devices
ENVITM (Sigma Aldrich/Supelco) adsorbent microspheres
deposited on a fiber filter (loss of microspheres with sampled
analyte); medium impedance
EMPORETM (3M) adsorbent microspheres incorporated on a
teflon filters with inglobed; high impedance
In order to reduce the impedance, we developed a FILTER
MADE OF FUNCTIONALIZED FIBERS, without adsorbent
microspheres (very low impedance)
ATLANTICTM (Horizon) adsorbent microspheres beetween two
fiber filters (sandwich); very high impedance
We looked for a simultaneous filtering and adsorbent device, trying to use in
air devices commonly used for water samples, but all these devices could not
be used in air because of their high impedance:
4
Functionalisation of filters
5
Whatman GF/D glass microfiber filtre (47 mm and
100 mm diametre)
Pretreatments
Dehydration (anhydrous acetone and toluene)
Functionalisation (PTES in toluene)
Pretreatment
Increase in weight
No
pretreatment (0.7 ± 0.1) %
HCl
0.5 M for 24 hours (1.2 ± 0.1) %
NaOH
0.5 M for 24 hours (6.2 ± 0.1) %
NaOH
0.5 M for 24 hours,
then
HCl
0.5 M for 24 hours (2.8 ± 0.1) %
NaOH
0.1 M for 24 hours (5.1 ± 0.1) %
NaOH
0.2 M for 24 hours (6.2 ± 0.1) %
NaOH
0.5 M for 24 hours (6.3 ± 0.1) %
NaOH
1 M for 24 hours (6.3 ± 0.1) %
NaOH
0.2 M for 12 hours (5.9 ± 0.1) %
NaOH
0.2 M for 48 hours (6.4 ± 0.1) %
Reaction
time Reaction
temperature Increase in
weight
12 h 25 °C (2.9 ± 0.1) %
24 h 25 °C (4.1± 0.1) %
48 h 25 °C (4.2± 0.1) %
12 h 80 °C (5.8 ± 0.1) %
24 h 80 °C (6.2 ± 0.1) %
48 h 80 °C (6.3 ± 0.1) %
Characterisation of filters
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DSC/TGA (air, 5 °C/min)
Oxidation of phenyls
Hygroscopicity
Functionalised fiber filters: air sampling
7
PAH sampling efficiency
8
Paolini et al., Aerosol and Air Quality Research, 16: 175183, 2016
PAH sampling efficiency
9
Paolini et al., Aerosol and Air Quality Research, 16: 175183, 2016
PAH extraction and purification recovery
10
Comparison with other SPE disks not possible
PCDD/Fs and dl-PCB sampling
Tecora EcoPUF samplers
Filters 110 mm diameter
Filters followed by a PUF cartridge
PUF: density 0,022 g cm-1, 5 cm diameter per 5 cm length; Tisch Environmental.
200 L min-1 flow rate
48 h sampling time
Parallel sampling using normal and functionalized filters was performed.
Filters and PUF separately extracted and analysed
11
PCDD/Fs sampling efficiency
12
PCBs sampling efficiency
13
Remarks and open questions
14
Normal filter/PUF efficiency: 15-95%
Functionalised filter sampling >80% (including all carcinogenic PAHs)
Is filter/PUF partitioning a useful information?
Industrial emission samplig:
improved efficiencybut not enough!
oxidation is the predominant phenomenon for PAHs
Water samples?
15
Thank you for your kind attention
v.paolini@iia.cnr.it
www.iia.cnr.it
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