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DAIKIN Advanced(DAAnIaKlIyNsAiAsMM)ethodfor C6/C8
1. Introduction `This analysis method is designed for simple and accurate determinationofwhethear fabricis treated with C6 or C8 PEC product. Traditionally, a difficult extraction/LC-mass analysis method has been used as C6/C8 identification method. This traditional method, however, is most useful to quantify impurities (PFOA etc.) in PFC products before and after application to final products like fabric, and is not well suited to simple confirmationofwhether articles have been treated with C6 or C8 product. `This new method can be applied, not only to distinguish C6/C8, but also to determine C4, or fluoro-chains longer than C8.
2. Apparatus and Materials Head Space Vial (5mi) (PTFE/Silicone septum, Aluminum cap) GeMSorGe (Note; There is the possibility that C8 or longer fluoro-chain cannot be detected by GC only (FID) due to its detection limit. GCMS is recommended for correct analysis. Headspace Autosampler (Perkin-Elmer and Agilent are available) or Gas-Tight Syringe and Oven (100- 200C) Standard Reagent Available from Sigma-Aldrich. > C6: Perfluorohexylethanol (CASH 647-42-7) CFACF:CF:CF:CF,CFy-CH:CHz-OH > C8: Perfluorooctylethanol (CASH 678-39-7) CF3CF2CFZCF2CF2CF,CF:CF2-CH:CHOzH-
DAIKIN Patent pending.
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3. Method description The method is based on 1) significantly degrading fluorotelomer monomers and polymers to alcohol by severing the ester-bond with heat, and 2) measuring the resulting alcohol.
<sample preparation> 1) Prepare a 100 mg fabric sample, or in any case one larger than 3cm x cm. 2) Place the fabric sample into headspace vial. 3) Seal the headspace vial with septum and cap. <Headspace GC analysis> 1) Heat the headspace vial at 200C for 30min in oven. (Use of an autosampler is
preferred.) 2) Take 2mlofgaseous phase sample from headspace vial and inject into GC. <GC conditions> See 5. Actual Results below. The conditions are not limited to our conditions.
4. Dataanalysis
The signal for identification C6/C8 is detected as Perfluorohexylethanol (C6)/
Perfluorooctylethanol (CB).
<In caseofmass available>
> C6: CFSCF,CF:CF,CF,CF2-CH.CHa-OH
MW 364
> C8: CFaCFACFACFACF:CFaCRaCFy-CHCHOy-H MW 464
<In case of mass unavailable>
Compare the retention time with a standard reagent.
5. Actual Result
<Equipment>
GC/MS: Perkin-Elmer GC Auto System XL + Turbomass
Column: DB624 60m x0.32mm, 1.8mm (Agilent Technologies)
Initial SOC for Smin, 10C/min to 250C (hold for Smin)
IN:
250C
`Transfer line Temp.: 250C
Carrier: He, 1.4ml/min constant flow
Sprit: 14:20
Sample quantity: 2m
Tonization: Electron impact (EI)
Ionization Voltage: 70V.
'DAIKIN Patent pending.
DAIKIN AAM "Type of experiment: Scan
ScanRang: 10~600
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6. TestReport Report "Positive" or "Negative that are chosen from complying with following requirement
7. MeOH Washing Method `This method is the pre-treatment for verification when C8and/orC8 related compound is detected and reportedas "Inconclusive".
3) Place the vessel inside an ultrasonic bath for 10min 5) Repeat 2) - 4) 6) Put the fabric sample in vacuum dryer
8. Safety
eTT TnaSr erepimers `Above 280 C, hydrogenfluorideand othertoxicgasmaybe produced.
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