STANDARDOPERATINGPROCEDURES

revisedJuly2006

SOLVENTSTILLS.........................................................................................................2
ROTARYEVAPORATOR.............................................................................................6
INERTATMOSPHEREGLOVEBOX..........................................................................8
FUMEHOODS.............................................................................................................12
UltraSonicator..............................................................................................................13
SlowSpeedCentrifuge..................................................................................................14
HighSpeedCentrifuge..................................................................................................15
SOLVENTCABINET...................................................................................................15
REFRIGERATOR/FREEZER.......................................................................................16
GAS/VACUUMMANIFOLD......................................................................................17
BASEBATHS...............................................................................................................20
WASTEDISPOSAL.....................................................................................................21
SAFETYPROTOCOLFORHANDLINGOFCARCINOGENS................................22

SOLVENT STILLS
1.Process
Refluxandsubsequentdistillationoforganicsolventsoverdryingmaterialsand
undernitrogenorargon.Theequipmentconsistsofagascylinder,gasregulator,anoil
bubbler,andforeachsolventthereisastillpot(2Lroundbottomflask),astillhead,and
acondenser.
2.HazardousChemicals
a)Solvents(benzene,toluene,hexane,heptane,ethanol,ether,THF,chloroform,
methylenechloride,etc.).Someoftheseareflammableandsomearecarcinogenic.
b) Drying agents (sodium, benzophenone, magnesium, iodine, phosphorus
pentoxide,calciumhydrideetc).Manyofthesearehygroscopicandflammableandreact
violently withwater.Byproductsincludehydrogengas,metalhydroxides,phosphoric
acidandorganicwastes.
3.PersonalProtectiveEquipment
Eyeprotection:Gogglesorfaceshieldmustbeused.
Handprotection:Dryglovesarerequiredwhenhandlingdryingagentsand
somesolvents.Whilealmostanywaterproofgloveswillprotectyoufromthe
dryingagents,thechoiceofglovesshouldbedictatedbythenatureofthe
solvent.Achartofsolventpermeabilityofseveralglovesisshowninthelast
fewpagesoftheFishercatalogue.
4.Engineering/VentilationControls
a)Fumehoodisrequiredfordistillationofcarcinogenicsolvents,toxicsolvents
orpyridine.
b)Allofthesestillsmustbeoperatedunderanatmosphereofargonornitrogen
gas,whichissuppliedviarubbertubingandcontainedwithintheglassware.
5.HandlingProcedures
Equipment
Eachstillconsistsofaheatingmantle,heatingmantlecontroller,2litreround
bottomflask(24/40femalejoint),stillhead,condenser,andnitrogen/argonadapter.The
stillheadreturnsthecondensedliquidbacktotheroundbottomflaskunlessavalveis
closed,inwhichcasethesolventcollectsinthe1Lchamberwhichformsthecenterof
thestillhead.Asolventoverflowpathallowsthesolventtoflowbackintotheround
bottomflaskiftoomuchsolvent(>1000mL)iscollected.Aflowmonitormeasuresthe
flowofwatercomingoutofthecondensers.
Preparation
Thereareseveralchoicesofdryingagent.

Sodium/benzophenone (foralkanes,toluene,benzene,tetrahydrofuran):Reflux
thesolventwith4goffinesodiumparticles(perlitreofsolvent)foroneworkingday(8
h). Add 5 g of benzophenone and reflux for a second day. The level of dryness is
indicatedbythecolour.Purple(best)>blue>green>yellow(terrible).Foralkanes,itis
difficulttogetbetterthangreen.Ifthesolutionisyellowandremainsyellowevenafter
continuedreflux,thenthebenzophenoneisusedupandthesodiummayalsobeusedup.
Inthissituation,dooneofthefollowing:
a)
deactivatethestill(seeWasteDisposal)iftherearealotofsolidson
thebottomoftheflask,
b)
addmoresodiumifthereisnosodiumleftinside(feelwithalong
spatula),refluxfor4h,cool,andaddmorebenzophenone,or
c)
chopuptheremainingsodiumifthereissomesodiumleftinside(chop
itupwithalongspatula),refluxfor4h,cool,andaddmorebenzophenone.

Sodium/potassium alloy (for low boiling alkanes and ether): Fill three neck
distillation flask with the solvent. Add equal amounts of freshly cut sodium and
potassiummetals.Refluxthesolventwithstirringfor>8h.Ifalloysolidifiesaddmore
potassiummetal.
Stilldeactivation:
Magnesium/iodine(foralcohols):Startwithonly200mLofalcohol.Add23g
ofmagnesiumturningsand12crystalsofiodine.Letstirover56hours.Donotheat.
Waituntilthebrowncolordisappears.Thenaddmorealcoholandheatituptorefluxfor
8h.
CalciumHydride(acetonitrileandmethylenechloride):Addmethylenechloride
or acetonitrile to a roundbottom flask which contains 1020g of CaH2 per litre of
solution.Refluxfor>4h.
Phosphoruspentoxide(formethylenechloride):Treatmethylenechloridewith
potassiumpermanganate(afewgramsperlitre).Shakeitandletitsituntilnomore
reactionoccurs,andthenforhalfanhourlonger.Pouritintoaroundbottomflaskwhich
contains1020gofP2O5perlitreofsolution.Refluxfor8h.
DistillationProcedure
Selectthethreeneckflaskwhichcontainstheappropriatesolvent/dryingagent
combinationfromtheflammablestoragecabinet,placeitonthecoldheatingmantleand
assembleitwiththedryinghead,andwiththenitrogensupply.StarttheN2flowataslow
rate(~1bubblepersecond)andconfirmthatthetubingconnectionbetweenthestilland
theargonflowisnotobstructed(ie.checkforbends,constrictions,orclosedstopcocks
andopenthem).Startthewaterflowataflowratestrongenoughthattheflowfillsthe
exittubebutnotsostrongthattheflowisturbulentorexcessivepressurebuildsup.
Checktheflowratenowandafter10minutes.Closethestopcockwhichisattachedto
thesidearmoftheupperchamber.Alsoclosetheteflonstopcockwhichleadstothe
collectionportbelowtheupperchamber.Opentheteflonstopcockwhichallowssolvent

intheupperchambertoflowdowntothelowerchamberorstillpot.Confirmthatthere
arenoforeignobjectsbetweentheheatingmantleandtheflask.Turnontheheating
mantletoasettingappropriateforthesolvent(ie.higherboilingsolventsrequireahigher
setting,seeTable).Adjustlaterifnecessary.
Checkthewaterflowrate.
Afterrefluxhasbeenachieved,waitanhouroruntilthecolorofthesolution
showsthatthesolventisdry,whicheverislater,andthenclosetheteflonstopcockwhich
allowssolventintheupperchambertoflowdowntothelowerchamberorstillpot.After
thedesiredvolumeofsolventhasaccumulatedintheupperchamber,turnofftheheating
mantle. At this point, watch for suckback of bubbler oil into the argon lines and if
necessaryincreasetherateofflowoftheargongastopreventthis.
Removethecollectedsolventbyeitherofthefollowingtwomethods:
a)Byusingasyringe(flushedtwicewithargon)withalongneedle,passingthe
needlethroughaseptumandthenthestopcockwhichisattachedtothesidearmofthe
upperchamber,or
b)byattaching asolventstorageflasktothecollection portbelow theupper
chamber.Themalejointofthedistillationheadhastobepurgedwithnitrogenfroma
separatehosebeforethereceiver flaskisconnected. Opentheteflonstopcockinthe
collectionporttotransferthesolvent,thenclosetheteflonstopcockatthedistillation
head,andclosethereceiverflaskwithaglassstopperwhilepurgingwithnitrogen.
Opentheteflonstopcockwhichallowssolventintheupperchambertoflow
downtothelowerchamberorstillpot.
Afterthestillpotiscooltothetouch,stoptheargonandcoolingwaterflow.
Solvent

b.p.C

suggested
appropriate
inappropriate
controller
glovesc
gloves
setting
b
Benzene
80
5
SSbest,Vok
B,N,R
Diethylethera
34.5
4
SS
V,B,N,R
Hexane
69
5
SS,V,N
B,R
Methanol
65
5
N,R
Methylenechloride
40
4.5
SSbest,Vok
B,N,R
Pentane
36
4.5
SS,V,N
B,R
Pyridineb
116
6
SS
B,N,R
Tetrahydrofuran
67
5
SS
V,B,N,R
Toluene
111
6
SS,V
B,N,R
a
Boilingpointissolowthatvaporsmaytravelthroughcondensersandcontaminatelines
andotherstills.Useprecooledwater(coldtapwaterisnotcoldenough).
b
Needstobedistilledinafumehood.
c
SS=SilverShield,V=Viton,B=Butyl,N=NitrileLatex,R=naturalrubber
DeactivationofStills
Collectmostbutnotallofthesolventintheupperchamber.Usethiscollected
solventtostartyournewstillpot.Atleast50mLshouldremaininthelowerflask.The

remnantsofsolvent,dryingagentandjunkintheoldstillpotmustbetransferredtoa
vacuum/gasmanifoldinafumehood,flushedwithargonorN2 anddeactivatedbythe
followingprocedureswhilestillunderargonorN2:
Sodium/benzophenonemixtures:Injectisopropylalcohol(afewdrops,thenafter
10minutesafewmL)throughthestopcockusingasyringewhileN2gasisflowing.Then
breakupallchunksofsodiumandsodiumsaltsusingaverylargespatula(youwillhave
toflushwithN2againafterthat).Repeatuntilnofurtherreactionoccurs.Treatsimilarly
withethanol.Breakupallchunks.Repeatuntilnofurtherreactionoccurs.Treatsimilarly
withwater.Breakupallchunks.Repeatuntilnofurtherreactionoccurs.Beabsolutely
surethereisnomoresodium.Add500mLmorewater,thenseparatetheorganicand
aqueouslayers,ifpossible.Theaqueouslayerwillcontainlessthan24%alcoholand
thereforecanbepoureddownthedrain.Theorganiclayerisnowwasteandshouldbe
putintoaproperlylabeledorganichazardouswastecontainer.Ifthelayerscannotbe
separated,thentheentiremixtureshouldbeputintoaproperlylabeledorganichazardous
wastecontainer.
Magnesium/iodine:Treatwithdilute(1M)hydrochloricacidslowly,untilthere
isnofurtherreactionandnomagnesiumisvisible.Neutralizetheaqueousphasewith
sodiumbicarbonate(ifnecessary).Theaqueousphaseisnownonhazardousandcanbe
poured down the drain. The organic fraction should be put into a properly labelled
organichazardouswastecontainer.
Calciumhydride:Treatwithethanolwatermixture(1:1byvolume)untilthe
hydrogengasevolutionhasstopped.Dilutewithwaterandpourtheaqueoussolution
downthedrain.
Phosphoruspentoxide(forthismixturetheargonatmosphereisnotnecessary):
Add water slowly, until there is no further reaction. After the reaction is complete,
neutralizewithsodiumbicarbonateandthenpourtheaqueousportiondownthedrain.
The organic waste should be put into a properly labelled organic hazardous waste
container.
6.AccidentProcedures
Incaseoffireorpotentialfireatthestills,cutthepoweratthecircuitbreakers
(nearthefridge),notattheheatingmantles.Theheatingmantlepowerswitchesandwall
socketsaretooclosetothemantlesandthereforewouldbeinadangerzoneifthestills
weretocatchfireorexplode.
Ifthereisasignificantspillofflammablematerial,keepallsparksources
away.Keeplabdoorsandwindowsclosed;thefumehoodwillexhausttheroomandkeep
itatnegativepressurewithrespecttothehallandotherrooms.Call911toreportthe
incident. The Hazardous Materials Emergency Response Team will supervise the
cleanup.
Afullyloadedstillonfireistoolargeafire,orcouldrapidlybecometoolargea
fire.Insuchacase,evacuatethelab,closethedoor,andcall911,orpullthefirealarm.
Anyfirefightingefforts,bylaboratorystafforfirefightingpersonnelshouldbeaimedat
puttingoutthesolventfire.

 In case of a fire during deactivation of the sodium, potassium, or calcium

hydride,immediatelyclosethehood.Ifthefireissmall,letitburnoutbyitself.DOnot
addwater toextinguish the fire!Subsequent cleanup shouldbeperformed extremely
carefullybecauseofthepossibilitythatunreactedsodiumandflammablesolventvapors
remain.

7.ApprovalRequired
Useofthesolventstillsisrestrictedtothoseresearcherswhohavebeentrainedin
their use by the PI or by an experienced user with the specific approval of the PI.
PermissionfromthePIisrequiredbeforeanyofthefollowingsolventstillsmaybe
prepared:benzene,carbontetrachloride,anyothercarcinogenicsolvent,oranysolvent
withaboilingpointhigherthan130C.Potassiumorpotassium/mercuryamalgammay
notbeusedinasolventstillwithoutthespecificpermissionofthePI.
8.Decontamination
Seewastedisposal
9.Preventivemeasures
DeactivationofthestillsmustbeperformedunderargonorN 2,notair,andby
thespecialproceduredescribedbelow.
Neveraddfreshsolvent,dryingagentorindicatorwhenthestillishot.Donot
dismantletheequipmentwhilethestillishot.
Neverleavetheapparatusunattendedwhilecollectingdistilledsolvent.Thestill
potcouldoverheatorrundryandresultinanexplosion.
10.Maintenance:
Everysixmonths,checktomakesurethatallwaterlinesareadequatelywired
or clamped and are not cracked or weakened. Check whether the mantles are in
reasonablecondition(cables andfabricarenotfrayed,mantleisnotcontaminatedor
dirty).
Donotallowsolidmaterialtoaccumulateintheroundbottomflasks.Deactivate
thestillsaccordingtotheproceduregiveninthewastedisposalsection.

ROTARY EVAPORATOR

1.Process
Evaporationofsolventundernormalorreducedpressure.Theequipmentconsists
oftherotaryevaporator,andaheatedwaterbath.
2.HazardousChemicals
a) Solvents (acetonitrile, benzene, toluene, hexane, ethanol, ether, THF,
chloroform, methylene chloride, etc.). Some of these are flammable and some are
carcinogenic.
3.PersonalProtectiveEquipment
Gogglesmustbeused,especiallywithreducedpressureevaporation.RotaryEvaporator
hastobeshieldedbyplexiglassshield.
4.Engineering/VentilationControls
a)Fumehoodisrequiredfordistillationofcarcinogenicsolvents,toxicsolvents
orpyridine.
5.HandlingProcedures
Equipment
Ensurethatcoolingwateristurnedonandthatpressurerelievevalveontopof
condenserisopen.Chargeevaporatorflaskwithsolution(infumehood)andconnectto
condenserwhilemotorisinelevatedposition.Secureflaskwithscrewandturnonmotor
onslowestsetting.Adjustrotatingspeed,andimmerseflaskinwaterbathusingthelift.
Donotapplyvacuumwhenlowboilingsolvents(Bp<60degCelcius)areevaporated,
becausethesesolventswillnotcondenseunderreducedpressure.Whenfinished,first
openpressurerelievevalve(afterworkunderreducedpressure),liftflaskoutofwater
bath, reduce rotational speed and turn of motor, then disconnect flask with residue.
Disposeorganicsolventdistillateinappropriatewastecontainer.Turnoffwater.Clean
spillsintothecondenser.Cleancondenser,whenwaterorcarcinogenicsolventshave
beenevaporated.
SomeBoilingpointsofcommonorganicsolvents.
Solvent

b.p.C

Benzeneb
Diethylethera
Hexane
Methanol
Methylenechloride
Pentane
Pyridineb
Tetrahydrofuran
Toluene

80
34.5
69
65
40
36
116
67
111

suggested
controller
setting
5
4
5
5
4.5
4.5
6
5
6
7

appropriate
glovesc

inappropriate
gloves

SSbest,Vok
SS
SS,V,N
N,R
SSbest,Vok
SS,V,N
SS
SS
SS,V

B,N,R
V,B,N,R
B,R
B,N,R
B,R
B,N,R
V,B,N,R
B,N,R

 Boilingpointissolowthatvapoursmaytravelthroughcondensersandcontaminate
linesandotherstills.bNeedtobedistilledinafumehood.
c
SS=SilverShield,V=Viton,B=Butyl,N=NitrileLatex,R=naturalrubber
a

6.AccidentProcedures
Incaseoffireorpotentialfireatthestills,cutthepoweratthecircuitbreakers
(nearthefridge),notattherotaryevaporator.
Fire fighting efforts should only be attempted for small fires. A fully loaded
evaporatorflaskcouldrapidlybecometoolargeafire.Insuchacase,evacuatethe
lab,closethedoor,andcall911,orpullthefirealarm.Anyfirefightingefforts,by
laboratorystafforfirefightingpersonnelshouldbeaimedatputtingoutthesolvent
fire.
Ifthereisasignificantspillofflammablematerial,keepallsparksourcesaway.Keep
lab doors and windows closed; the fumehood will exhaust the room and keep it at
negativepressurewithrespecttothehallandotherrooms.Call911toreporttheincident.
TheHazardousMaterialsEmergencyResponseTeamwillsupervisethecleanup.
Cleanupofthemessafteranaccidentshouldbeperformedcarefully.
7.Decontamination
Seewastedisposal
8.Preventivemeasures
Neverleavetheapparatusunattendedwhileinoperation.
9.Maintenance:
Check whether the seals are in reasonable condition and tight. Check for
squeakingnoises.Ifnecessary,disassembleglasswareandcleanit.

INERT ATMOSPHERE GLOVE BOX

Useofthegloveboxisrestrictedtothoseresearcherswhohavebeentrainedinits
usebythePIorbyanexperienceduserandwiththeapprovalofthePI.
ForfirsthandinformationconsulttheM.Braunreferencemanual.

0.Generalremarks
Never attempt to wash the plexiglass windows with organic solvents. The
windowswillgoblind,andyouwillhavetowatchyourexperimentsthroughahazeuntil
youfinishthegraduateprogram.Instead,cleanthewindowsfrominsidewithadrypaper
towel(Kimwipe),andfromtheoutsidewithwaterwithsomedishwashingagent.

Neveropenbothantechamberdoorssimultaneously.Airwillleakin,andyour
andyourcolleagueschemicalswilldecompose.
Neverrushoutoftheglovessoquickly,thatsubatmosphericpressureisapplied
to the glove box. Air will come in through microscopic leaks, with mentioned
consequences.
Neveropentheinnerdooroftheantechamberwhenyouarenotabsolutelysure
thattheantechamberisunderacleannitrogenatmosphere.Ifyouhavedoubtaboutthe
stateoftheantechamber,applythreeevacuation/nitrogenpurgecycles.Whennotinuse,
keeptheantechambersundervacuum.
Never releaseanychemicalsintothegloveboxatmosphere.Mostchemicals
reactwiththecatalystandsignificantlyreduceitslifetime.Moreimportantly,vaporsof
harmful solvents/chemicals can penetrate the butyl rubber gloves and damage your
health.Keepinmind,thatthegloveboxisaclosedsystem,andthateverythingyou
releaseintotheatmospheremayatsomelaterpointinterferewitheitheryouoryour
experiments. Accordingly, donotcarryoutstronglyexothermic reactions inthe box,
whichmayresultinchemicalspills.Becausewecannotuserefluxcondenserinthebox,
neverheatanychemicaltoabove50deg.Celciusinthebox.
1.Process
Thegloveboxisusedforstorageorhandlingofair/moisturesensitivechemicals
(i.e.chemicalswhichareeitherdangerousorrendereduselesswhenexposedtoairor
water).Thegloveboxisfurtherusedforcarrying outsmall scale(<20mL solvent)
reactionsthatinvolveairandmoisturesensitivecompounds.Exceptionsfromthisrule
requirethepermissionofthePI.
2.HazardousChemicals
Allchemicalsaretobestoredinclosedvesselswithinthegloveboxand
this is especially important for hazardous and pyrophoric chemicals. Most chemicals
reactwiththecatalystandsignificantlyreduceitslifetime.Moreimportantly,vaporsof
harmful solvents/chemicals can penetrate the butyl rubber gloves and damage your
health.Keepinmind,thatthegloveboxisaclosedsystem,andthateverythingyou
releaseintotheatmospheremayatsomelaterpointinterfereswitheitheryouoryour
experiments.
Otherhazardsofthegloveboxincludeoverpressurizationandventingofnoxious
materials.Thegaspurificationcatalystconsistsofmetalsandtheiroxideswhichmay
reactviolentlywithairorwater.Theoperatinggasisnitrogenandtheregenerationgasis
afewpercenthydrogeninargon.Thesegasesarenottoxicbutwillnotsupportlife.
3.PersonalProtectiveEquipment
Operatorsshouldwearcottonglovesontheirhandsandputbabypowderonthe
gloves.Theseprecautionshelppreventthebuildupofsweat,whichrenderstheskinmore
permeabletochemicals.Ifcarcinogenssuchaschloroformorbenzenearehandledinside
theglovebox,wearapairofSilverShieldorVitonglovesinsidetheboxandoverthe

main gloves. The main gloves themselves are either butyl rubber or neoprene and
thereforewillnotprotectyoufromsuchchemicals.

4.HandlingProcedures
Refertothegloveboxreferencemanualforproperoperatingprocedure.
Somegeneraladvice:
Afteranantechamberhasbeenevacuatedandfilledwithargon/nitrogen3times,switch
thesigntoIN.
Ifyouopentheoutsidedoortotheantechamber,changethesigntoOUT.
Ifyoutakethingsout,changethesigntoOUT.
Iftheantechamberhasntbeenusedforafewdays,changethesigntoOUT.
Neveropenbothdoorstoanantechamberatthesametime.
Alwaysusethesmallantechamberunlessyouabsolutelyhavetousethebigone.
Alwaystakeallvisiblerubbishoutwithyouevenifitisnotyourrubbish.
Putrubbishintothedustbininsidethebox,especiallysharps.
Ifyoubreakglass,pickupallthepieces(withtweezers,notgloves)rightaway.
Keepflaskscoverediftheycontainliquids.
Thefollowingchemicalsarenotpermittedinsidetheglovebox:H2,H2O,CO,air,O2,
N2O,HF,HCl,HBr,HI,HCN,HCO2H,NH3.
Avoid using chromatography columns in the box unless absolutely necessary. The
silica/alumina powders plug up the oxygen monitor. Clean up powders as soon as
possible,avoidingdispersingtheminthebox.
Vacuumapplications
Installafreshlycleanedcoldtrapbetweenthevacuumpumpbeforestartingtouse
thevacuum.Ensurethatevacuatedflasksaresecuredagainstfall.
Whatkindofobjectscanbebroughtthroughtheantechambersintotheglovebox:
Ifpossible,objectshavetobedriedoverseveralhoursinthedryingoven.
a)Solidobjectssuchasglassware,metalimplements,openboxesofKimwipes,etc.may
bebroughtinaslongastheyarenotcapableoftrappingair.
b)Reagentswhichareintheiroriginalunopenedbottlesandwerepackagedunderargon
maybebroughtintothegloveboxwithoutfurtherpreparation.Theunopenedbottleisall
thecontainmentthatisrequired.
c)Driedanddistilledsolventsfromthestillsmustbetransferredintoasolventflask
whichhasbeenevacuatedtoaminimumpossiblepressurewhichdependsonthesolvent.
Stopcocks have to be secured with clamps, and rubber bands, and must be at room
temperature.Flasksmustbecontainedinsecondarycontainers,whichpreventsolvent
fromleakingintothevacuumpumps.
d)Otherliquidsshouldbedegassed.Theliquidsshouldbeatroomtemperaturewhen
theygothroughtheantechamber.
e)Bottlesorjarsofairstablesolidsshouldbeopened,andafoldedKimwipeshouldbe
placedoverthejarandhelddownwithrubberbandstoprotectpowdersfromspillingout

10

intoantechamberandvacuumpump.Theoriginalcapshouldgointothegloveboxalong
withtheKimwipecoveredjar.
Procedureforbringinganobjectintothegloveboxviathesmallantechamber.
Ensure that inside door, vacuum valve and the N2 valve are closed, and that the
antechamber pressure is 1 atm. Further ensure, that the vacuum valve of the big
antechamberisclosed.Opentheoutsidedoor,placeobjectinsidetheantechamber,close
the outside door, and open vacuum valve. Evacuate antechamber until vacuum is
attained,butatleastfor1minute.Closevacuumvalve,openrefillvalveuntilpressure
reaches atmospheric, close refill valve, repeat vacuum/refill cycle twice more. Open
insidedoor,extractobject,closeinsidedoor.ChangesigntoIN.Forstandbyleave
antechamberundervacuum.
BringinganobjectintothegloveboxviatheKF40port(nexttofridge).Ensure
thattheboxpressureisatleast0.8units,andthatnosubatmosphericpressurecanresult
from sudden movements of a person working in the box. Open the outside port by
unscrewingthescrew,placeobjectinsidetheantechamber,andclosetheportagainby
lockingthescrews.Duringtheprocedure,avoidsuddenmovementsthatmaycauseair
circulations.Reducetheglovepressuretoworkingpressure.Onlyobjectswithsmooth
sufaces(nmrtubes,UV/Viscells,screwcapbottles,vials)shouldbebroughtintothebox
throughtheKF40port.
Bringinganobjectintothegloveboxviathelargeantechamber.
Usebigantechamberonly,whenobjecttobigforsmallantechamber.Procedureisthe
sameasforsmallantechamber,exceptthatduetolargersize,evacuationtimetakesat
least20minsforeachcycle.
Procedureforbringinganobjectoutofthegloveboxviaeitherantechamber.
EnsurethattheoutsidedoorisclosedandthesignsaysIN(ifthesignsaysOUTthen
youhavetogothroughthebringinginprocedureasdescribedabove,beforetryingto
bringanythingout).Opentheinsidedoor,placeobjectinsidetheantechamber.Closethe
insidedoor.Openoutsidedoor,extractobject,closeoutsidedoor.ChangesigntoOUT.
5.AccidentProcedures
Ifforsomereasonthepressureclimbstoohighsothattheglovesstarttoballoon,
closethemainvalveonthecylindersupplyingtheinertgas.Iftheglovesburst,closethe
mainvalveonthecylindersupplyingtheinertgasandputtheportcoverinplacetoblock
offtheburstglove.Thiswillpreventthesmellofthegloveboxfromspreadingintothe
roomandwillalsominimizethecontaminationofthegloveboxwithair.
Incaseofafireoroverheatingofthedryingcatalystduringregeneration,close
themainvalveonthecylinderwhichissupplyingtheregenerationgas(H 2/Argon)tothe
glovebox.
Ifinertgashasbeenorisbeingreleasedandthereisnodangeroffire,closethe
valvetotheinertgassupply.

11

Ifaglovebreaks,ripsorispunctured,usethathandtopullthegloveportcover
overtheglovehole.Thegloveportcoverisstoredjustbelowtheceilingoftheglove
box.Readtheoperatingmanualtofindouthowtoreplacethedamagedglove.(Note:
duringtheprocedureforflushingthenewglove,donotevacuatethenewglovesomuch
thattheknobonthegloveportcoverbecomestoodifficulttoturn.)Iftheotherthree
glovesareundamagedandtheO2andH2Olevelsareacceptable(lessthan10ppm),then
thegloveboxcanbeusedevenwhilethedamagedgloveremainsunreplaced.
PowerOutage
Iftheoxygenlevelrisesabove200ppm,stoptherecirculation,solvetheleak,thenpurge
withN2orargonuntiltheO2levelfallsto200ppmandthenstarttherecirculationagain
untilthelevelfallstobelow10ppm.Iftheoxygenlevelrisesslowlyorfailstocome
downafteraleakdespitecontinuedrecirculation,regeneratethedrytrainasdescribedin
themanual.
IftheoxygenlevelishighanddoesnotrespondtopurgingwithfreshN 2,orifthe
measuredoxygenleveldoesnotseemtocorrespondtothetrueoxygenlevel,thenthe
circulationmaybeturnedoff.
Thetrueoxygenlevelcanbecheckedindependentlybythefollowingprocure:a)remove
theupperhalfoftheglassfromanormal60wattlightbulbusingaglassblowingtorch,b)
bringthislightbulbintotheglovebox,c)putitintoalampsocketclampontoastand,
andd)turningonthelamp.Ifthelightbulbglowsformorethanaminute,thenthe
oxygenlevelisverylow(probablylessthan10ppm).
6.WasteDisposal
Chemicalwastehastoberemovedfromthegloveboxinsuitablecontainers,e.g.
sealedplasticbagsforusedkimwipes,orflasksforbothliquidandsolidchemicals.The
latterhavetotreatedaccordingtowastedisposalregulations.Usedpumpoilshouldbe
putintoaproperlylabeledhazardouswastecontainer.
7.Decontamination
All materials exposed to hazardous chemicals in the glove box have to be
decontaminatedinafumehood.
8.Preventivemeasures
Thefollowingmaterialsarebannedfrombeingintroducedintotheglove
box: mercury, air, oxygen, nitrogen oxides, sulfur oxides, sulfuric acid, nitric acid,
hydrochloricacid,aqueoussolutions,water,halogens,andanyotherchemicalsrelatedto
anyoftheabove.Alcoholsmaybeintroducedbutpreferablyinonlysmallquantities.
9.Maintenance:
Every2months,checkthattheoilinthevacuumpumpisclearandnearly
colorlessandofsufficientvolume(asindicatedbythemarkingsontheviewwindow).

12

Every2months,cleanthecondenserfinsontheDriColdrefrigerator.Checkthe
sightglass,locatedinthecondensingline,forpresenceofmoisture(refertomanualif
moistureisdetected).Replacebatteryifthedisplayisdim(refertomanual).
Every2months,visuallychecktheglovesandtheOringsaroundthemfor
punctures,cracking,orwear;replacetheglovesororingsifcracksarefound.heckthe
Oringsontheantechamberdoorsforcracks;replacetheoringsifcracksarefound.
Cleanthedoorswithamildsolventandcoatthesealingsurfaceswithalightcoatof
vacuumgrease(Apiezon,notsilicone).
Every6months,replacetheoilinthevacuumpump.
Every year, perform maintenance on the vacuum pump as called for in its
manual.

FUME HOODS
1.Process
The fume hoods are used for the handling of smelly, toxic, mutagenic or
carcinogenicvolatilecompounds,includingsolids,liquidsandgases.Thecontinuousair
flowisintendedtopreventtheaccumulationofhazardousvaporsandtheexposureof
workerstosuchvapors.
2.PersonalProtectiveEquipment
Operators should wear goggles, at a minimum. Additional personal protective
equipment should be used if appropriate to the hazard level of the procedure. For
example,workersusingacidicorcausticsolutionsshouldwearanappropriateacid/base
resistantapronandgloves.Workersusinghazardousorganicsolventsshouldweargloves
resistanttothatorganicsolvent.
3.Engineering/VentilationControls
Theoperatorshouldconfirmthatthereisairflowbyobservingaflowindicator
suchasastripofmagnetictapeattachedtothebottomofthesash.Ifairisnotflowing
throughthehood,donotusethehood,callfacilitiesat21655torequestrepairs.The
sashorvelocityscreenshouldbekeptbelowthelevelindicatedbyastickertothesideof
thesash,exceptwhenabsolutelynecessary(e.g.whenbringingoversizeobjectsintothe
fumehood).
4.HandlingProcedures
Avoidplacingequipmentorchemicalsclosetothefrontedgeofthehood(this
cannotbeavoidedinthecaseofverylargeequipment).
Keepthesashglassclean.Donotobstructyourviewwithpaper,notices,decals,
orotheritemsinthesashes.
13

Avoidsuddenmovementswhileworkingatthehood.Walkingbrisklypastthe
hoodcandisruptaircurrentsandpullvaporsoutofthehood.Keepyourheadoutsideof
thefumehood,butsetequipmentandperformtasksasfarbackinthehoodaspossible.
Beforeeveryuse,checkthatthereisairflowbyobservingaflowindicatorsuch
asastripofmagnetictapeattachedtothebottomofthesash.Thesashshouldbeoperated
atthelowestpossibleposition,butnotmorethan18inches.
Avoidusingflammableliquidsinthesamefumehoodasasparksourcesuchasa
magneticstirrer,hotplate,bunsenburner,oranyelectrical/electronicdevice.
5.AccidentProcedures
Ifairflowhasceased,quicklyclosethesashandIMMEDIATELYcallFacilities
ServicesEmergency(7521655)toarrangeforrepairs.Handleafireinthehoodasyou
wouldanyotherfire;attempttoextinguishasmallfireonlyifothersknowyouaredoing
soandifyourescaperouteisnotthreatened.Beaware,however,thattheairflowinthe
fumehoodwillfantheflamesandmaycausethefiretospreadmorequickly.
Ifthereisaspillofflammablematerialinthehood,keepallsparksourcesaway.
Keeplabdoorandwindowsclosed;thefumehoodwillexhausttheroomandkeepitat
negativepressurewithrespecttothehallandotherrooms.Call911toreporttheincident.
TheHazardousMaterialsEmergencyResponseTeamwillsupervisethecleanup.
6.Decontamination
Thefumehoodmayneedtobeemptiedandcleanedpriortosomemaintenance
activities.
7.Maintenance:
Every6months,washthesashwindows.
Thefumehoodsareinspectedbyfacilitiesandthefacevelocityismeasuredand
certified to be between 100150 fpm every 12 months. Notify facilities if the last
certificationwasmorethan12monthsago.

Ultra-Sonicator
1.Process
Thesonicatorisusedforthedispersionofcolloids.
2.HandlingProcedures
Ensure proper filling level with water. Turn on the sonicator and insert the
containerthatcontainsthesamplewhileholdingitwithtwofingers.Dependingonthe
intensityoftheultrasonicwaves,theglasscontainergethotforverybriefperiodsof
time.Whenthecolloidisdispersedremovethesamplefromthebath,andclosethelidof
thesonicatortoavoidevaporationofthewater.

14

3.Precautions
Donotsonicatefragileequippment,suchasmicroelectrodearrays,andUV/vis
quartzcells.Theywillbreakimmediately!
4.Hygiene
Keep the water batch clean. Exchange water with fresh deionized water if
necessary.

Slow Speed Centrifuge

1.Process
TheCentrifugeisusedfortheseparationofliquidmixtures.
2.HandlingProcedures
Thecentrifugehasaswingingbucketrotorcapableofacceptingfourcontainers.
Fortheproperoperationitiscrucialthatthecontainersarebalancedtoatleast0.5g.
Severe damage to the centrifuge can result, if containers are not balanced. After the
containershavebeenproperlyinsertedintothebuckets,thelidisclosedandtheproper
speedischosen(usuallythehighest3,800rpm).Thestartbuttonispressedtoinitiate
theseparation.Incaseofaproblemthecentrifugecanbestoppedbypushingthestop
button.
3.Noise
Thecentrifugeisquitenoise,especiallyifithasnotbeenbalancedwell.Inthis
case,eitherrebalanceorshutthedoorsofthecabinet.
4.Hygiene
Keepthecentrifugeclean.Incaseofaspill,thebucketscanberemovedfromthe
centrifugeandcleanedinthesinkwithdetergentandwater.

High-Speed Centrifuge
1.Process
TheCentrifugeisusedfortheseparationofliquidmixtures.

15

2.HandlingProcedures
Thecentrifugehasafixedrotorcapableofacceptingsixlargeandtwelvesmall
containers.Useonlytheproperpolyethylenecontainerswithaplasticscrewcapno
othercontainersareallowedinthiscentrifuge! Fortheproperoperationitiscrucial
thatthecontainersarebalancedtoatleast0.05g.Severedamagetothecentrifuge
canresult,ifcontainersarenotbalanced. Afterthecontainers havebeenproperly
inserted,theblackcoverisplacedontotherotor(ensuregoodfit),thelidisclosedand
theproperspeedischosen.Thestartbuttonispressedtoinitiatetheseparation.Incaseof
aproblemthecentrifugecanbestoppedbypushingthestopbutton.
3.Hygiene
Keepthecentrifugeclean.Incaseofaspill,therotorcanberemovedfromthe
centrifugeandcleanedinthesinkwithdetergentandwater.

SOLVENT CABINET
1.Process
Thesolventcabinetisusedforthestorageofflammableandcombustibleorganic
liquids.
2.Engineering/VentilationControls
Theflammablescabinethasselfclosingdoors.Italsohasaliponthefloorto
containaspill.
3.HandlingProcedures
Thecabinetshouldnotbeusedtostoremorethan227litres(60USgallons)of
flammableliquids.Upto38litres(10USgallons)canbeoutsidethecabinetatanyone
time.Thecabinetdoorsmustbekeptclosedexceptwhenremovingorreplacingabottle.
Donotuseanydevicetopropopenthedoors.
4.AccidentProcedures
Ifthereisafireintheflammablescabinet,evacuatetheroomandthebuilding
immediatelyandcall911.Thecabinetdoorsshouldcloseontheirown.
Ifthereisaspillintheflammablescabinet,keepallsparksourcesaway.Keeplab
doorandwindowsclosed;thefumehoodwillexhausttheroomandkeepitatnegative
pressurewithrespecttothehallandotherrooms.Call911toreporttheincident.The
HazardousMaterialsEmergencyResponseTeamwillsupervisethecleanup.

16

5.Decontamination
Thesolventcabinetmayneedtobecleanedpriortorepairordisposal.Iforganic
residues are visible, these should be scraped or washed off and added to a properly
labelledhazardouswastecontainer.Ifnoresiduesarevisible,wipethesurfaceswithwet
papertowels.
6.Maintenance:
Ifthedoorsfailtocloseatanytime,adjustthefeetofthecabinet,oilthedoors,or
requestrepairassistancefromthemachinistorthemanufacturer.

REFRIGERATOR/FREEZER
1.Process
The refrigerator/freezer is used for the storage of chemicals. The electrical
components and switches are isolated from the internal atmosphere to prevent the
possibilityofasparkinducedfire.
2.HazardousChemicals
Therefrigeratormaycontainawidevarietyofhazardouschemicals,including
flammable,reactiveortoxiccompounds.Undernocircumstancesshouldfoodordrinkbe
storedinthisfridge.
3.PersonalProtectiveEquipment
Operatorsshouldweargoggles,ataminimum.Workersusinghazardousorganic
solventsshouldwearglovesresistanttothatorganicsolvent.
4.HandlingProcedures
The refrigerator/freezer doors must be kept closed except when removing or
replacing abottle.Openthedoorslowlytopreventagitation ofchemicals containers
storedinthedoorshelves.
5.AccidentProcedures
Ifthereisafireintherefrigerator/freezer,evacuatetheroomandthebuilding
immediatelyandcall911.
Ifthereisasignificantspillofaflammablematerialintherefrigerator/freezer,
keepallsparksourcesaway.Keeplabdoorsandwindowsclosed;thefumehoodwill
exhausttheroomandkeepitspressurenegativewithrespecttothehallandotherrooms.
Call911toreporttheincident.TheHazardousMaterialsEmergencyResponseTeamwill
supervisethecleanup.

17

6.Decontamination
Ifnecessaryfordecontamination,removethefreezerdoorandpivotdownthe
evaporatorassemblytoobtaincompleteaccesstothecabinetinterior.
9.Maintenance:
Wipecleanthewireshelvesperiodically.Cleantheinsidesurfaceofthecabinet
withwarmwaterwithdetergent.Rinsethoroughlywithcleanwarmwaterandwipedry.
Besurethepowerisoffbeforecleaning.
Defrostthefreezerasrequired.
Every6months,cleanthecondensercoilswithasoftbrushoravacuumcleaner
withabrushattachment.Besurethepowerisoffbeforecleaning.
Donotmodifyorworkonanyelectricalcomponents.Contactfacilitiesat752
1655foranyrepairs.

GAS/VACUUM MANIFOLD
1.Process
The gas/vacuum manifold is used for the handling of air or water sensitive
chemicals. It consists of a gas manifold (for delivering either argon or nitrogen), a
vacuum manifold (for evacuating glassware), and a vacuum pump (attached to the
vacuummanifold).Theinertgasissuppliedbyagascylinderviaaregulator,passes
throughthegasmanifold,andthenbubblesthroughanoptionaloilbubbler.
2.HazardousChemicals
The gas/vacuum manifold is used for the handling of air or water sensitive
chemicals.Someofthesechemicalscouldbeverypyrophoric.Otherthanthehazardsof
thechemicalstobehandled,theprinciplehazardsofthegas/vacuummanifoldinclude
explosion due to overpressurization, implosion of evacuated vessels, frostbite from
contactwithliquidnitrogen,andoverheatingduringregenerationofthedryingcatalyst.
Theinertgas,argon,ifventedinsufficientquantities,coulddisplaceenoughairtocause
asphyxiationofpeopleintheroom.However,standardsizeargongascylinderscontain
only330cu.ft.orlessofgaswhileroom203containsapproximately12,000cu.ft.ofair.
Oilbubblers areusedattheexit ofthe gasmanifold. Mercuryshouldnotbe
touchedanditsvaporsshouldnotbeinhaled.
3.PersonalProtectiveEquipment
Operators should wear goggles, at a minimum. Workers using mercury or
hazardousorganicliquidsshouldwearglovesresistanttothosematerials.

18

4.Engineering/VentilationControls
Theoilormercurybubblerservestoallowinertgastoescapefromthemanifold
ifthepressurerisesover1atm.Thebubbleralsoprevents airfromcomingintothe
manifoldThemercurybubblermustalwaysbeheldinoroverabucket,andthevent
from the bubbler must be directed into the same bucket or a different bucket. Thus
mercuryspillsshouldbecontained.Themercurybubblerhasanextrabubblerbeforeit
andanotherafter,tocatchanymercurysuckedbackorblownoutofthemainbubbler.
5.HandlingProcedures
Replacingagascylinder:Closethefinevalveontheregulatorandthevalveon
theold(empty)cylinder.Detachtheregulatorfromtheoldcylinder.Putthecaponthe
oldcylinder.Unstrapandremovetheoldcylinderandputinitsplacethenewargonor
highpuritynitrogen(99.97%)cylinder. Donotmoveacylinderunlessitsprotective
capisinplace.Strapinthenewcylinderandremoveitsthecap.Attachtheregulatorand
openthecylindervalvebutnotthefinevalve.Closethecylindervalveagainandopen
thejointbetweenthecylinderandtheregulatorslightlytoletthepressureescape.This
allowstheconnectiontobeflushedwithgas.Thentightlyattachtheregulator,andslowly
opentheregulatorvalve.
Whenstartingtousethevacuummanifold,confirmthatallofthevalvesleading
totheflexibletubingareclosed,checkthatthetrapbottomsareattachedtothetrap,and
thenputliquidnitrogenintotwoDewarflasksandputthemaroundthetraps.Turnonthe
vacuumpump.Whenfinishedwiththeequipment,reversetheaboveprocedure.Thatis,
turnoffthevacuumpump,openthevalveswhichallowairintothetraps,andremovethe
liquidnitrogenDewarflasksfromaroundthetraps.
WARNINGNOTE: AfteryouremovetheliquidnitrogenDewarflasks,ifyou
seeaclearblue(oxygen)liquidinthetraps,ClosethesashofthefumehoodandLEAVE
IMMEDIATELY. Do not continue with the procedure, because the oxygen may
explosivelyreactwithorganicsinthetrap.Afterabout10minutes,theliquidwillhave
boiledoffandpassedthroughthepump.Iftheliquidwasoxygen,thiswillhavecreateda
temporaryfirehazard(hencetheneedtoleavetheroom).
Evacuatingaflask: Examinetheflaskforcracksbeforeevacuatingit.Thiswill
reducetheriskofimplosion.Alwayssecureevacuatedflasks,sothattheycannotfallor
rollonthebenchtop,andexplode.
Bewareofcondensingargon.Argon'sboilingpoint(185.7C)ishigherthanthat
of nitrogen (195.8C). It is therefore possible to condense liquid argon. If a vessel
containing condensed liquid argon were closed and then removed from the liquid
nitrogencoolant,thevesselwouldexplode.
Bewareofcondensingoxygen. Oxygen'sboilingpoint(183.0C)ishigherthan
thatofnitrogen(195.8C).Itisthereforepossibletocondenseliquidoxygen.Ifavessel
containing condensed liquid oxygen were closed and then removed from the liquid
nitrogencoolant,thevesselwouldexplode.Also,ifliquidoxygencondensedinavessel
ortrapalongwithsomeflammableorcombustiblecompounds,anexplosivereaction
couldresult.
19

Degassing a liquid. Choose a round bottom Schlenk flask of the appropriate

volume.Evacuatetheflaskandthenfillitwithargonornitrogen.Addtheliquidby
syringeorpipette.Closethesidearmstopcockandcooltheflaskinadewarwithliquid
nitrogenuntiltheliquidfreezes.Thenevacuatethevaporphasebyturningtovacuumand
opening the sidearm stopcock. After 1 minute, start thawing the vessel. When some
meltingofthesolidisobserved,turnthestopcocktoargon/nitrogen.Keepthesidearm
stopcockopen.Whenthesolidiscompletelymelted(butnotnecessarilywarmedtoroom
temperature)repeattheprocedure.Atotalofthreecyclesisusuallysufficient.
6.AccidentProcedures
Ifthereisalargefire,evacuatetheroomandthebuildingimmediatelyandcall
911.
Ifthereisasignificantspillofaflammablematerial,keepallsparksourcesaway.
Keeplabdoorsandwindowsclosed;thefumehoodwillexhausttheroomandkeepits
pressurenegativewithrespecttothehallandotherrooms.Call911toreporttheincident.
TheHazardousMaterialsEmergencyResponseTeamwillsupervisethecleanup.
Ifthereisanimplosionorexplosionduetovacuumoroverpressurizationandno
subsequentfire,closeoffthevalvesleadingtoanyvesselscontainingchemicals,remove
theliquidnitrogendewars,turnoffthevacuumpump,allowairintothetraps,andturn
offtheargonsupply.
AfteryouremovetheliquidnitrogenDewarflasks,ifyouseeaclearcolourless
(argon)orclearblue(oxygen)liquidinthetraps, LEAVEIMMEDIATELY.Donot
continuewiththeprocedure,becausetheoxygenmayexplosivelyreactwithorganicsin
thetraporitmayboilsoquicklythattheglasswarebursts.Afterabout10minutes,the
liquidwillhaveboiledoff.Iftheliquidwasoxygen,thiswillhavecreatedatemporary
firehazard(hencetheneedtoleavetheroom)andwillhavemadeitnecessaryfortheoil
inthepumptobereplaced.
7.WasteDisposal
Wasteargongascanbevented.Liquidwastescondensedinthetrapsshouldbe
disposedofinamannerappropriatetotheirnature.Organiccondensatescanbepoured
into aproperly labeled organic hazardous waste container. Waste mercury shouldbe
labeledashazardouswasteandsentfordisposalseparatelyfromotherhazardouswastes.
Spentcatalystispyrophoric;itshouldbewettedpriortoitsdischargeandstored
andtransportedinawetcondition.
8.ApprovalRequired
Nopriorapprovalisrequiredforuseofthegas/vacuummanifold,butuseofthe
equipmentisrestrictedtothosepeoplewhohavebeentrainedinitsusebyacompetent
userandwhohavereadtheseSOPsandsignedontheirtrainingformthattheyhaveread
theseSOPs.

20

9.Maintenance:
Thepumpshouldbeservicedasdescribedinitsmanufacturer'smanual.

BASE BATHS
1.Process
Thebasebathisusedtocleanglassware.
2.HazardousChemicals
Thebasebathcontainsethanolandpotassiumhydroxide.Ethanolistoxicand
flammable.Potassiumhydroxidesolutionsarecaustic.Donotinhalethevaporsfromthe
bath.
3.PersonalProtectiveEquipment
Operatorsmustweargogglesandethanolresistantgloveswithmediumorlong
sleeves.Alabcoatandsplashapronisalsorequired.Donotputyourunprotectedhandin
eitherbath.Thebasebathisnotonlycausticbutitisorganic,soyourskinoffersno
protectionfromanytoxicimpuritiesinthebath.
4.Engineering/VentilationControls
Alwayskeepthebathtightlycoveredexceptwhentransferringitems.Keepspark
sourcesawayfromthebasebath.
5.HandlingProcedures
Topreparethebasebath,dissolve500gKOHin1.5Lofdistilledwater.After
theKOHdissolves,add8Lofethanol.Topreparetheacidbath,add0.5LHClto8Lof
distilledwater.
Towashglasswareinthebaths:Handwashtheglasswarewithsoapandwater.
Rinseofftheglasswarewithdistilledwaterthoroughlyandshakeoffexcesswaterbefore
puttingitintotheKOH/EtOHbath.Leaveitinthatbathforatleastanhour.Removeit
fromthebath,letexcessEtOHdripbackintothebath.Rinseofftheglasswarewith
distilledwaterbeforeputtingitintothediluteHClbath.Leaveitinthatbathforatleast
30minutes.Removeitfromthebath,letexcessHCldripbackintothebath,thenrinse
againseveraltimeswithdistilledwaterandletitdry.
DoNOTputanyofthefollowingitemsintotheKOH/EtOHbath:
volumetricglassware
stopcockkeys
glassfrits/filters
rubberitems

21

IRorUVcellsorNMRtubes
fragileorbrokenglassware
glasswarethatstillhasgreaseorbulkdirtonit
anythingwithmercury,sodium,potassiummetal
anythingwithhighacutetoxicity(e.g.mercury,thalliumorcyanidesalts)
TowashNMRtubes,don'tputtheminthebaths.RinsetheemptyNMRtubes
withacetone,thendiluteHCl,thendistilledwater,thenacetone.Ifthetubesarestill
dirty,rinsethemwithdistilledwaterthenfillthemwithKOH/EtOHfromthebath,leave
themforanhourinthefumehood(nolongerthan1h),thendumpthecontentsbackinto
thebath.RinsewithdistilledwaterthenrepeatwiththediluteHCl.Rinseanddry.If
elementalmetalsolidremainsontheNMRtube,fillitwithaquaregia(3:1HCl:HNO 3)
andleaveitovernightinthefumehood.Thenrinsewithdistilledwaterandrepeatthe
KOH/EtOHandHCltreatments.
TowashUVcells,don'tputtheminthebaths.Handwashwithsoapandwater.
Rinseoffwithdistilledwaterthoroughlyandshakeoffexcesswaterbeforerinsingthem
withacetone,andairdrythem.
To deactivate the base bath: Add dilute HCl very slowly to the base bath to
neutralize it. Check the pH frequently with pH paper. After neutralization, pour the
mixturedownthedrain(ifitcontainslessthan24%alcohol)orpackageashazardous
wastefordisposal(ifitcontainsmorethan24%alcohol).
6.AccidentProcedures
Ifthereisafire,evacuatetheroom,closingthedoorbehindyou.Pullthefire
alarmandcall911.
Ifthereisaspillofthebasebath,keepallsparksourcesaway.Keeplabdoorsand
windowsclosed;thefumehoodwillexhausttheroomandkeepitspressurenegativewith
respect to the hall and other rooms. Call 911 to report the incident. The Hazardous
MaterialsEmergencyResponseTeamwillsupervisethecleanup.
7.WasteDisposal
Afterdeactivation(seeHandlingProcedures),theaqueousphasesmaybepoured
downthedrain(iftheycontainlessthan24%alcohol).Otherwisepackageashazardous
wastefordisposal.
8.Maintenance:
Alwayskeepthebathscovered.Ifevaporationoccurs,topupwithethanolforthe
basebathordistilledwaterfortheacidbath.

WASTE DISPOSAL

22

Alwayscollectheavymetalwastes.Pt,Pd,Rh,Ru,andIrcanberecycledfor
credit.Otherheavymetals(especiallyHg)mustbepreparedseparatelyfordisposal.
OrganicWaste
Separatehalogenatedfromnonhalogenatedchemicals.
Keepthecapon.Donotleavefunnelsinopencontainers.
Dontputanywasteinthebottleuntilthebottleisproperlylabeledwithahazardous
wastelabel.
Experimental procedures involving reactive species (eg. acids, bases, oxidizers,
reducers,metalalkyls,hydrides)shouldincludeaneutralizationasthelaststepinthe
procedure.Neverputreactivespeciesintotheorganicwastebeforesuchaneutralization
step,ortheymayreactwiththeothercomponentsalreadyinthewaste.
Noinorganicsolids,preciousmetals,ormercurymaybeputintheorganicwaste.
Leavea3to4headspaceinthebottle.
OthertypesofWaste
Precious metals are NOT WASTE. Collect them for recycling in properly labeled
containersinthefumehood.
Keepmercurywasteinaseparatecontainer,properlylabeledashazardouswaste.
Unusedsilicagel,alumina,celite:putinaziplocandtheninthegarbage.
Usedsilicagel,alumina,celiteshouldbeputinasolidwastecontainer.
Disposal
Dispose ofwastes promptly,preferably within 3months fromthe start ofwaste
accumulationinthatcontainer.Nowasteshouldbeaccumulatedbeyond9months.

SAFETY PROTOCOL FOR HANDLING OF CARCINOGENS

PrincipalInvestigator:FrankOsterloh(office:7546242)
Otherpersonnel: DanielHewitt,HirokiHiramatsu,JasonMartino,XiubinQi,Alex
Merrill,JinYoungKim(lab:7546241)

Reagents:

Amount Form

Benzened6

20g

liquid

Concent Storagelocation
UseLocation
ration
neat
glove box, organics glovebox,fumehood,
shelf,orflammables ormanifold
cabinet

Theonlycarcinogeninthelaboratoryisbenzene.Wemayinthefuturehandlenickeland
chromium(VI)salts.Allofthesechemicalsmustbehandledaccordingtothefollowing
rules.

23

PersonalProtectiveEquipment:
a)Eyeprotection:Gogglesorfaceshieldmustbeused.
b)Handprotection:Glovesarerequiredwhenhandlingsolvents.Thechoiceof
glovesshouldbedictatedbythenatureofthesolvent.Achartofsolventpermeabilityof
several gloves is shown in the last few pages of the Fisher catalogue. For use with
benzene,SilverShieldglovesarebestwhileVitonglovesareacceptable. Disposable
latex,rubberorbutylglovesdonotofferprotectionagainstthesereagents.Theglovebox
glovesareneopreneorbutylandthereforeshouldnotbeconsideredsufficientprotection;
SilverShieldorVitonglovesshouldbewornoverthegloveboxgloves.
c)Bodyprotection:Alabcoatandpropershoesshouldbeworn.Opentoedshoes
andsandalsarenotpermitted.
Procedures
Thereagentsaretobeusedintheglovebox,thefumehoodoronavacuum/gas
manifold.Iftheyaretobeusedonamanifold,theymustbetransferredintoandoutof
theSchlenkwarebysyringethroughsepta,sothatthevaporsarenotreleasedintothe
room.Alternatively,thereagentscouldbeplacedintheSchlenkwarewhileinafume
hood;theglasswarewouldthenbecappedandcarriedtothemanifold.
EmergencyProcedures:
Whenvolatileliquidorgaseouschemicalcarcinogensarespilledinthefumehoodor
glovebox:
a. Immediately put on additional layers of gloves and be sure the laboratory coat is
buttonedandchemicalsplashgogglesaresecurelyinplace.Putonanaproniflarge
amountsofliquidarepresent.
b. Contain the spill by absorbing it in towels, rags, or other materials. Place spill
materials,towels,rags,orothermaterialsinadoublelayerofplasticbags.Sealthebag
andlabelwithahazardouswastelabel.Leavethebagofspillwasteinthehood.
c.CallEH&S(7521493)forthesaferemovalofcontaminatedabsorbentfromhood.
d.Decontaminatethespillarea.
e.Checkforresidualspillagebylookingforvisiblewetareas.Decontaminateagainif
necessary.
f.Thoroughlywasharms,hands,andface.Assoonaspossible,showerandwashhairif
ClassIIIcarcinogensarespilled.(OurgroupdoesnotuseClassIIIcarcinogens).
Whenvolatileliquidorgaseouschemicalcarcinogens(e.g.benzene)arespilledinthe
generalroom:
a.Evacuatetheroom.
b.CallUCDFireDepartment(911)andEH&S(7521493),inthatorder,forassistance.
c.DonotreentertheroomuntilclearedbyEH&S.
d.ShowerifadvisedtodosobyEH&S.
Spillsofnonvolatileliquidcarcinogens:

24

a.Putonadditionalprotection(gloves,labcoat,apron,disposablebooties).
b.PlacethecontaminatedabsorbentindoublebagsfordisposalbyEH&S.
c.Decontaminatethespillarea.Specifydecontaminationmethod.
d.Checkforresidualspillagebylookingforvisiblewetareas.Decontaminateagainif
necessary.
e.Thoroughlywasharms,hands,andface.ShowerandwashifClassIIIcarcinogens
werespilled.
Spillsofparticulatecarcinogens(e.g.leadsalts):
a.Isolatetheareabybarricadingorothermeanssothatthespillisnotspread.
b. Put on additional protection (gloves, lab coat, apron). If the spill is extensive,
respiratorsand/orimpermeablecoverallsmaybenecessary.ContactEH&S(7521493)
forguidance.
c.Graduallypushparticlesfromoutsideofthespillareatowardsthecenter,usingmoist
towels.DoNotDrySweep!!
d.Pickupparticulatesbyusingmoisttowelsorsponges.Disposeofwasteindouble
plasticbags.CallEH&S(7521493)forpickup.
e.Additionalwetmoppingorspecialvacuummaybenecessarydependingontheextent
ofthespill.CallEH&S(7521493)forguidance.
f.Decontaminatethespillarea.Specifydecontaminationmethod.
g.Checkforresidualspillage.Decontaminateagainifnecessary.
h.Thoroughlywasharms,hands,andface.ShowerandwashhairifClassIIIchemical
carcinogenswerespilled.
Emergencyproceduresforaccidentalinoculation(injectionofcarcinogenbysyringe):
1.Immediatethoroughwashingoftheinjectionsite.
2.ReportingimmediatelytoEmployeeHealthServicesorCowellStudentHealthCenter
formedicalevaluation.Followupifnecessary.
WasteDisposal
In all cases, any used protective equipment, towels, wash water, etc. are
consideredcontaminatedhazardouswaste. Thismustbedoublebagged,labeled,and
disposedofbyEH&S.
ReportingProcedures
Researchers should contact Employee Health Services (7522330) after any
significantexposuretochemicalcarcinogens.|Anyemergencyincidentorexposuretoa
chemical carcinogen must be reported to EH&S or the UC Davis Fire Department
immediately,andfollowedupbyawrittenincidentreporttoEH&Swithintendays.

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