restekapp07 - page 217

Restek Corporation
(800) 356-1688, ext. 4
Environmental
ExtractionofPCBsusingResprep
-C18-47SPEdisks
andResprep
-6D
note
A
pplications
cat.# 59564
For more information
call technical service:
(800) 356-1688,
ext. 4
SampleAddition
Pour the sample into theDiskcover
-47
reservoir, adding it directly to the filmof
methanol left on thedisk from the
conditioning step. Adjust thevacuum to
approximately25 in.Hg.
DiskDrying
After theentire samplehasbeen
processed, draw air through thedisk
under vacuum to remove any residual
water from thedisk.
AnalyteElution
Release systemvacuum. Insert the
collection rackandvessels into theglass
chamber,making sure to label each
vesselwith thecorresponding
Diskcover
-47.Reassemble the
Resprep
-6D.Add 5mLmethylene
chloridedirectly to thesamplebottle,
andgently swirl to rinseall inner
surfacesof thebottle.Transfer the
methlyenechloride to thediskusinga
glasspipetteand rinse the reservoir
sides in theprocess. Let the solvent
stand for threeminutes.Draw the
solvent through thedisk at 5 in.Hg.
Repeat thebottle rinseanddiskelution
oncemorewith a fresh aliquot of
methlyenechloride, combiningall
eluates in thecollection tube.
FinalAnalysis
Removewater from sample eluateby
passing through anhydrous sodium
sulfate.Concentrate to1mL, and
analyze.
SamplePretreatment
Allow1 liter of deionizedwater to
equilibrate to room temperature.Adjust
sample pH to less than2with6NHCl.
Add5mLofmethanol andmix
thoroughly. ForQA/QC samples, spike
with1mLof a5ug/mL solution for a
final concentration in thewater of 5ppb.
ApparatusAssembly
Assemble theDiskcover
-47mmwith
reservoir,making sure theTeflon
®
o-
ring is inplace. Alsobe sure toplace
theC18disk in theDiskcover
-47
wrinkled sideup.Assemble the
Resprep
-6D as detailed in the
instruction sheet, alongwith thevacuum
pump, vacuum line, andvacuum trap.
DiskPrecleaning
Add10mLofmethylene chloride to the
disk’s top surfaceand immediatelydraw
throughunder vacuum at 15 in. Hg.
Continue to draw vacuum at 15 in. Hg
for5minutes, removingall solvent.
DiskConditioning
Add10mLofmethanol to thedisk’s top
surface and let stand for a fewminutes.
Draw themethanol through thedisk
until themethanol’s top surface is just
above the disk.Donot allow any air to
pass through thediskor reach the top
surfaceof thedisk.Note: It ispreferable
to leaveextra liquidabove thedisk
rather than allow any air to contact the
disksurface.
UseResprep
-C18-47SPEdisksandResprep
-6D toextractpolychlorinatedbiphenyls (PCBs)
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