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MICROWAVE ASSISTED
SOLVENT EXTRACTION
OF POLYVINYL CHLORIDE (PVC)OF POLYVINYL CHLORIDE (PVC)
FOR ANALYSIS OF PLASTICIZERS
BY GAS CHROMATOGRAPHY
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Objective
To demonstrate the application of MicrowaveAssisted Solvent Extraction (MASE™) for theAssisted Solvent Extraction (MASE™) for theanalysis of Plasticizers in Poly Vinyl Chloride
(PVC) wire wrap by GC/FID
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Equipment Used
• MARS-X™ Microwave Sample PreparationSystem, equipped with fiberoptic temperaturecontrol, and safety features for use of organicsolvents
• GreenChem™ Extraction Vessels• GreenChem™ Extraction Vessels
• VAF-100™ Vacuum Filtration Apparatus
• N-EVAP™ Nitrogen Evaporation Device
• Varian STAR 3400 Cx GC/FID
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MARSX (Accelerated Extraction)
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MARS-X Safety Features
• Solvent detector which monitors and reacts tosolvent vapor levels in the microwave cavity
• Exhaust fan which exchanges air through themicrowave cavity
•• Air flow switch which assures constant airexchange
• Vessel design incorporating over pressurizationventing mechanism
• Reinforced microwave door
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MARS-X Cavity, Vessels and Exhaust System
MicrowaveCavity
ExhaustFan
Solvent
ExtractionVessel
SolventDetector
Air FlowSwitch
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• Innovative Frame Design
• Glass or Teflon™ innerliner with reinforcedsleeve
• Fourteen positionturntable for high sample
GreenChem Extraction Vessels
Screw
Temperature Probe
DiscCover
turntable for high samplethroughput
• Autovent style sealingmechanism
• 200 ºC operatingtemperature
• 200 psi operating pressureControl VesselControl Vessel Standard VesselStandard Vessel
SupportModule
Liner
Sleeve
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Sample Matrix
Wire Wrap cut into small pieces
NextNextSlide
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Sample Matrix
• PVC wire wrap received as athree part completed wire
•• Outer wrap was seperatedfrom internal wires
• Outer wrap was cut intosmall pieces
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Analytes
Diisodecyl Phthalate (DIDP)
Ditridecyl Phthalate (DTDP)
Triisononyl Trimellitate (TINTM)
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Traditional Soxhlet Procedure
Weigh 0.5 grams of PVC into a Soxhlet thimble
Add 150 mL solvent* and assemble Soxhlet apparatus
Run for 16 hours
*solvent = di-Ethyl Ether
Analyze by GC/FID
Allow to cool
Take extract to dryness
Weigh Dry Residue
Re-dissolve residue in THF
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Microwave Extraction MethodDevelopment
20
25
30
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tab
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(Gra
vim
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ic)
0
5
10
15
%E
xtr
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(Gra
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MASE95 ºC
MASE115 ºC
MASE135 ºC
Soxhlet
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Parameters for MicrowaveExtraction of Poly Vinyl Chloride
Wire Wrap
• Sample Size 0.5g• Sample Size 0.5g
• Solvent di-Ethyl Ether
• Extraction Temp. 135 ºC
• Extraction Time 30 min.
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Microwave Extraction Procedure
Weigh 0.5 grams of PVC into a GreenChem glass liner
Add 40 mL solvent* and assemble the vessel
Extract in the MARS-X for 30 min. @ 135 oC
*solvent = di-Ethyl Ether
Analyze by GC/FID
Allow to cool and filter
Take extract to dryness
Weigh dry residue
Re-dissolve residue in THF
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PVC Wire Wrap ResultsGravimetric Analysis
AverageTechnique % Extractables* %RSD
* N=6
Soxhlet 26.14 4.64
Microwave 25.23 2.87
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GC OperatingConditions
• 1/8” Stainless Steel PackedColumn 3% SP-2100 on100/120 Suplecoport ™
• Flame Ionization Detector
• Injector Temp 330 ºC• Injector Temp 330 ºC
• Detector Temp 335 ºC
Heating Profile
Initial: 70 ºC Hold 2 min.
Ramp: 30 ºC/min 300 ºC
Ramp: 5 ºC/min 320 ºC
Hold: 20 min.
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PVC Wire Wrap ResultsGC/FID Analysis
Soxhlet Soxhlet Microwave MicrowaveAnalyte Avg. (%)* (% RSD) Avg.(%)* (%RSD)
DIDP 18.68 0.0117 18.90 0.0167
*N=6
DIDP 18.68 0.0117 18.90 0.0167DTDP 2.08 0.0299 2.21 0.0214
TINTM 2.52 0.0349 2.82 0.0205
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Conclusions
• MASE is a fast, safe, economical technique toprepare PVC samples for plasticizer analysis bygravimetric and GC/FID methods.
• MASE yields acceptable results when compared tothe standard Soxhlet method.the standard Soxhlet method.
• MASE provides extraction with 1/3 the amount ofsolvent required for the traditional method.
• MASE requires 1/10 the time of the Soxhletmethod.