Quenching of Pyrophoric Materials · Quenching of Pyrophoric Materials Hazardous Operation SOP Rev....

QuenchingofPyrophoricMaterialsHazardousOperationSOP

Rev.Date:2017-03-28

QuenchingofPyrophoricMaterialsH250

Examples:tert-ButylLithium,sec-ButylLithium,n-ButylLithium,DiethylZinc,Organoaluminumcompounds(asEt3Al,

Et2AlCl,EtAlCl2,Me3Al),RaneyNickelcatalyst

WORKING ALONE1 is PROHIBITED while quenching PYR materials

ThisSOPisnotasubstituteforhands-ontraining.PrintacopyandinsertintoyourlaboratorySOPbinder.

Department: Chemistry

DateSOPwaswritten: Thursday,March23,2017

DateSOPwasapprovedbyPI/labsupervisor: Friday,March24,2017

PrincipalInvestigator:Name:F.Fischer

Signature:______________________________

InternalLabSafetyCoordinatororLabManager:Name:StephenvonKugelgen

LabPhone:510.301.1058

OfficePhone:510.642.8252

EmergencyContact:Name:StephenvonKugelgen

PhoneNumber:510.301.1058

Location(s)coveredbythisSOP: TanHall674,675,676,679,680,683,684

1.Purpose

This SOP covers the precautions and safe handling procedures for the Quenching of PyrophoricMaterials.

Allmaterialsmentionedinyourlaboratory“PyrophoricMaterials”(PYR)ClassSOParecoveredbythishazardousoperationsSOP.

Also,thisSOPcoversanymaterialssynthesizedusingpyrophoricliquidsorsolids.

1Whenincludedinastandardoperatingprocedure,foranydurationoftime,apersonisworkingalonewhenperformingataskinalaboratoryandtheycannotbeseenorheardbyotherworkers,andwhenassistanceisnotreadilyavailable.Inthiscontext,ataskisanyportionorsectionofanoperationorjob,anddoesnotrefertoajobinitsentirety.


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Ifyouhavequestionsconcerningtheapplicabilityofanyrecommendationorrequirementlistedinthisprocedure,contactthePrincipalInvestigator/LaboratorySupervisororthecampusChemicalHygieneOfficeratucbcho@berkeley.edu.

2.Physical&ChemicalProperties

Forphysicalandchemicalpropertiesonpyrophoricmaterials,pleaserefertoyourlaboratory“PYR”SOPandtospecificSafetyDataSheets(SDS)ofchemicalsinuse(SeeSection11–SDSLocation).

3.PotentialHazards

When exposed to moisture or air, these reagents may ignite spontaneously. When quenchingpyrophoricmaterials,theindividualhazardsofthepyrophoricsandthesolvent,aswellasthehazardofthemixture,mustallbeconsidered,andproceduresforsafequenchingmustreflectthisconsideration.

As defined by the Globally Harmonized System of Classification and Labeling of Chemicals (GHS),pyrophoricsaredesignatedbyfollowingHcode:

H250Catchesfirespontaneouslyifexposetoair

4.EngineeringControls

Thefollowingisthesetofengineeringcontrolsrequiredwhenquenchingpyrophoricmaterials:

• Work under an inert atmosphere (e.g., argon, nitrogen) using a Schlenk line, in a glove box,vacuummanifold,oranyenclosedinertenvironment.

• If procedure is done in the fume hood, use the sash as a safety shield. For hoods with ahorizontalslidingsash,positionthesashallthewaydown,standbehindtheslidingwindowsandreacharoundtoperformthemanipulationsrequired.Forhoodswithverticalslidingsash,keepthesashaslowaspossible.

• Faceshieldsaretobeusedwhenthereisnoprotectionfromthehoodsashorwhenthehoodsashisopen.

• Remove any flammables (squirt bottles containing solvents, oil baths) and combustibles(Kimwipes,papertowels)fromtheworkarea.

• LaboratoriesandroomswherePyrophoricsareusedmusthavegeneralroomventilationthatisnegativepressurewithrespecttothecorridorsandexternalenvironment.Thelaboratory/roomdoormustbekeptclosedatalltimes.

5.PersonalProtectiveEquipment

Ataminimum,thefollowingPPEmustbewornatalltimes:

EyeProtection

A. ANSIZ87.1-compliantsafetyglasseswithsideshields,orchemicalsplashgoggles.

• OrdinaryprescriptionglasseswillNOTprovideadequateprotectionunlesstheyalsomeetANSIstandardandhavecompliantsideshields.

B. Ifthepotentialforexplosion/splashingexists,andadequatecoverageisnotprovidedbythehoodsash,afaceshieldmustbeworn.

SkinProtection


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A. Wearnon-syntheticclothingunderlabcoat.

B. Flame-resistant lab coat (Nomex IIIA, NFPA 2112) must be worn when working withpyrophorics.

C. Acombinationoffireresistant(FR)liners,coveredwithapairofchemical-resistantdisposablegloves (e.g.nitrileglovesor thosespecified in the specificSDS),mustbewornATALLTIMES.The following products are Approved FR Liners: Ansell Kevlar® Goldknit® Lightweight 70-200andHanzExtremityWearNomex®UtilityLiners.

D. Longpants,closed-toe/closed-heelshoes,coveredlegs,andankles.

6.FirstAidProceduresandMedicalEmergencies

Intheeventofaninjury,notifyyoursupervisorimmediatelyandEH&Swithin8hours.

GototheOccupationalHealthFacility(TangHealthCenter,oncampus); ifafterhours,gotothenearestemergencyroom(AltaBates,2450AshbyAveinBerkeley);or

Call911(fromacellphone:510-642-3333)if:

• itisalifethreateningemergency;or

• younotareconfidentinyourabilitytofullyassesstheconditionsoftheenvironmentand/orthe condition of the contaminated/injured person, or you cannot be assured of your ownsafety;or

• thecontaminated/injuredpersonisnotbreathingorisunconscious.

Please remember to provide a copy of the appropriate manufacturer SDS (if available) to theemergency responders or physician. At a minimum, be ready to provide the identity/name of anyhazardousmaterialsinvolved.

Incaseofskincontact

Ifskincontactoccurs,and/orskinorclothingareonfire,immediatelydrenchinthesafetyshowerwithcopious amounts of water for no less than 15 minutes to remove any remaining contaminants. Ifpossibletodosowithoutfurtherinjury,removeanyremainingjewelryorclothing.

Incaseofeyecontact

Rinse thoroughlywith plenty ofwater using an eyewash station for at least 15minutes, occasionallyliftingtheupperandlowereyelids.Removecontactlensesifpossible.

Ifswallowed

DoNOT induce vomiting unless directed otherwise by the SDS. Never give anything bymouth to anunconsciousperson.Rinsemouthwithwater.

Needlestick/punctureexposure

Washtheaffectedareawithantisepticsoapandwarmwaterfor15minutes.

Ifinhaled

Moveintofreshair.


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7.SpecialHandling,Storage,andDisposalRequirements

Pyrophoricreagentscanbehandledandstoredsafelyaslongasallexposuretoatmosphericoxygenandmoisture or other incompatible chemicals is avoided. Never leave a container with a residue of apyrophoricmaterialopentotheatmosphere.

Lab-specific informationonhandling and storagemaybe included in Section12 - Protocol/Proceduresection.

HandlingandStorageofPyrophoricMaterials

• Processistobeperformedunderaninertatmospheregas(useargongasinthecaseoflithiummetal).

• Liquids may be safely transferred without the use of a glove box by employing techniquesdiscussedinyourlaboratory“PYR”ClassSOP(syringeandcannulatechniques).

DisposalofPyrophoricReagents• Neverleaveacontainerwitharesidueofapyrophoricmaterialopentotheatmosphere.• Anyunusedorunwantedpyrophoricmaterialsmustbedestroyedbyfollowingthespecific

destructionprocedure(s)includedinyour“HazardousOperationSOP–QuenchingofPyrophoricMaterials”.Asanalternativetoquenching,rememberthatpyrophoricchemicalscanbedisposedofashazardouswaste(contactEH&Sforguidanceondisposal).

• RinsetheemptycontainerthreetimeswithaninertdryCOMPATIBLEsolvent.Therinsesolventmustbetransferredinandoutofthecontainerunderaninertatmosphereusingthesyringeorcannulatechnique.

• Solventrinsesmustbedisposedofashazardouswaste.

8.ChemicalSpillandFireResponse

PyrophoricSpillResponse• Inthecaseofaspill,announcethesituationloudlyintheimmediateareaandhaveanynearby

personsmovetoasafelocation.• Immediatelyeliminate/removeallnearbyignitionsources.

• Ifspilloccursinafumehood,coverwithMet-L-X,drysand,orothernon-combustiblematerial,closethehoodsashandifpresent,presstheredpurgebutton.

• If a spilloccursoutsidea fumehood, coverwithMet-L-X,dry sand,orothernon-combustiblematerial,andstandawayfromthespill.

• Locateandhaveaproperfireextinguisher(drychemical-based)readyincaseofignition/fire.

• Useclean,non-sparkingtoolstocollectabsorbedmaterialandplaceintoloosely-coveredmetalorplasticcontainersreadyfordisposal.

• Do not use combustible materials (paper or cloth towels) to clean up a spill, as these mayincreasetheriskofignitingthereactivecompound.

• Ifyoucannotassessthesituationwellenoughtobesureofyourownsafety,donotapproachthespill.

• Keepothersfromenteringcontaminatedarea(e.g.,usecautiontape,barriers,etc.).

• Reportthespillto510-642-3073.


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PyrophoricFireResponse• Call911(fromacellphone:510-642-3333)foremergencyassistanceandforassistancewithall

fires,evenifextinguished.• Ifthespill ignites,andifyouaretrainedandyoufeelcomfortabletodoso,extinguishthefire

withanappropriatefireextinguisher.Useonlydrychemicalfireextinguishers(classesABCorD).DonotuseaCO2extinguisher.

• AcanofMet-L-Xordrysandintheworkarea,withinarm’sreach,mightbehelpfultoextinguishanysmallfireasitcansmothertheflames.

• Donotusewatertoextinguishapyrophoricchemicalfireasitmayenhancetheintensityofthefire.Anexceptiontothiswouldbeinthecaseofskincontactorignitedclothing/skin.Inthesecases,rinsinganyunreactedchemicaloffisofprimaryimportance.

BeAWARE:Smallflamesatthetipoftheneedlescanbeproduced–expectthistooccur,anddonotpanic.ThecanofMet-L-X/sandisinthehoodtoquicklyextinguishthosesmallflames.

CarbonDioxide,Foam,Halon,andFireblanketareUNSUITABLEforextinguishingmetalalkylfires.

9.CleaningandDecontamination

Lab-specificinformationondecontaminationmaybeincludedinSection12-Protocol/Procedure.

• WearingproperPPE,laboratoryworksurfacesmustbecleanedattheconclusionofeachprocedureandattheendofeachworkday.

• Decontaminateallequipmentbeforeremovingfromadesignatedarea.

10.HazardousWasteDisposal

LabelWaste

• Labelallwastecontainers.SeetheEH&SFactSheet,“HazardousWasteManagement”forgeneralinstructionsonproceduresfordisposingofhazardouswaste.

DisposeofWaste

• Disposeofregularlygeneratedchemicalwastewithin6months.

• CallEH&Swithquestions.

11.SafetyDataSheet(SDS)Location

SDScanbeaccessedonlineathttp://ucsds.com


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12.Protocol/Procedure-QuenchingofPyrophoricMaterials

Procedure/Use Scale EngineeringControls/Equipment

PPE (eye, face, gloves,clothing)

Procedure Steps and Special Precautions forthisProcedure

1.Quenchingoftert-butyllithium(t-BuLi)remaininginbottleorleftafterreactions.

Upto20mLofcommercialt-BuLisolution,dilutedincarriersolvent.Quenchingoft-BuLiinamountsgreaterthan20mlatatimeisnotpermitted.

Seenoteforappropriateglasswaresizeselection.

Minimalquantitieswillbeleftafterreactionscarriedoutatscaleslistedinyourlaboratory“PYR”ClassSOP.

Asanalternativeto

ConductinacleanfumehoodwiththesashaslowaspossibleusingSchlenktechniques,oraninertatmosphereglovebox.

EyeProtection:Wearfittedsafetygogglesorsafetyglasseswithsideshields.

FaceProtection:Faceshieldsaretobeusedwhenthereisnoprotectionfromthehoodsash.

HandProtection:Confirmcompatibilityofglovematerialwithchemicalbeingused.Glovesmustbeinspectedpriortouse.Washanddryhandsafteruse.

Generalguidance:

Forindirectcontact(closed-systemproceduressuchastransfersviasyringeorcannula)ANDdirectcontact(opensystemproceduressuchasspillhandling,wipingofresidualpyrophorics)withpyrophoricmaterial-acombinationoffireresistant(FR)liners,coveredwithapairofchemical-resistantdisposablegloves(e.g.nitrileglovesorthosespecifiedinthespecificSDS)),mustbewornATALLTIMES.ThefollowingproductsareApprovedFRLiners:AnsellKevlar®Goldknit®Lightweight70-200andHanzNomex®FlameResistantUtility

NoteonGlasswareSize:Ifquenching20mLofpyrophoricsolution,thepyrophoricmaterialwillbedilutedin380mLofinertsolventtostartthequenchingprocedure(5%wtsolution).Inthiscase,therequiredsizeforthequenchingvesselis1L,noless.-QuenchinginaFUMEHOODusingaSchlenkline-Generalconsiderations:

Quenchingproceduresusuallyinvolvethereactionofthepyrophoricmaterial,underinertatmosphereandonanicebath,withareagentthathasareactivehydroxylgroup.

AnyreactionorsuspensioncontainingthesereagentsMUSTbequenchedcarefully!Alltransfersmustbedoneunderinertatmosphereusingthesyringeorcannulatechniques.

AdditionofmaterialmustbedoneSLOWLY,underadequatestirring/mixing.

Wheneverquenching,besurethatitisnotdoneinasealedvesselaspressurewillbuildup.Thebestsituationistohaveaninertgasflowinginwithasmallexitneedleconnectedtoabubbler.

Ifyou’requenchinginaRBflaskoranyfloatingvesselinabath,clampit.Ifthesolutionlevelislow,youcandiluteitwithsomeinertsolventsuchastolueneorhexanefirsttolessthan5%wt.Procedure:

Transferthet-BuLisolutiontothequenchingvessel,bringthetemperatureofthequenchsolutionto-78oCusingadryice/isopropanolbath,turnonthestirrer.

Beforeproceedingwiththequenchingofthe


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quenching,rememberthatanyquantitiesoft-BuLicanbedisposedofashazardouswaste.

ObtainPIapprovalifhigherscaleisnecessary.

LinerGloves.Clothing:WearNomexIIIA(NFPA2112)labcoat;wearnon-syntheticclothingunderlabcoat;fulllengthpantsorequivalent;andclose-toedandclose-heeledshoes.

pyrophoricsolution,immediatelyproceedwiththecleaningoftheemptybottle.

RinsetheemptycontainerthreetimeswithaninertdryCOMPATIBLEsolventsuchastolueneorhexane.Therinsesolventmustbetransferredinandoutofthecontainerunderaninertatmosphereusingthesyringeorthecannulatechnique.

Aftertheemptycontaineristriple-rinsed,removethesure-sealcapandleaveitopeninthebackofthefumehoodovernight.

Disposeofthesolventrinseashazardouswaste.

Proceedwiththequenchingofthepyrophoricsolutionbyaddingisopropanolslowlytothequenchingvesselusingasyringeoranadditionfunnel,underadequatestirring,untilnomorebubblingisobserved.

Keepthesolutioncoolduringthequenchingprocessbycontrollingthefeedrateofthealcohol.

Onceyou'veaddedtheisopropanol,addthefollowingsolventsinsequence,usingthesamestep-wisecaution:ethanol,methanol,andwater.

BeVeryCarefulwiththeadditionofwater!Evenaftermethanolhasbeenadded,thelithiatecanstillreactviolentlywithwater,especiallyistherehasn'tbeensufficientmechanicalstirringofthesolution.Addwaterinsmallaliquots.Theadditionofwaterdoesnotneedtobeconductedunderaninertatmosphere.Syringes(plasticorglass)areidealtoolstomaketheseadditions.

Oncetheadditionofwateriscomplete,letthesolutiontemperaturecomebacktoroomtemperaturewhilestirring.

Stirforanadditional2hoursbeforedisposingoftheaqueousorganicwaste.

-QuenchinginaGLOVEBOX-


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Generalconsiderations:

AnyreactionorsuspensioncontainingthesereagentsMUSTbequenchedcarefully!AdditionofsolventsmustbedoneSLOWLYwithadequatestirring/mixing.

Ifthegloveboxisequippedwithafridge,DONOTopenthefridgeduringthequenchingprocess.

Procedure:

TurnOFFthegloveboxcirculation.

Removebottlesure-sealcaporreactionvesselcapandaddastirrerifnecessary.

Typically,asolutionoflessthan5%wtofpyrophoricinaninertsolvent(suchasdryanddegassedhexaneorheptane)iscreated,followedbytheslowadditionofdryanddegassedisopropanoloralessvolatilealcoholsuchasoctanol,underadequatestirringuntilnomorebubblingisobserved.

Placeacaponthequenchingvesselandputthebottle/vesselinazip-topbagbeforetakingitoutoftheglovebox.

Movethequenchingvesseltoacleanfumehood.Alwaysplacethequenchingvesselinasecondarycontainerfortransfertothefumehood.

Purgethegloveboxfor20-30minutes.

Underadequatestirring,addwaterSLOWLYtothequenchingsolutionuntilnomorebubblingisobserved.Thisstepdoesnotneedtobeconductedunderaninertatmosphere.Syringes(plasticorglass)areidealtoolstomaketheseadditions.

BeVeryCarefulwiththeadditionofWATER!Evenafterisopropanolhasbeenadded,thelithiatecanstillreactviolentlywithwater,especiallyistherehasn'tbeensufficientmechanicalstirringofthesolution.Thereforethewatermustbeaddedinsmallaliquots.


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RinsetheemptycontainerthreetimeswithaninertdryCOMPATIBLEsolventsuchastolueneorhexane.

Aftertheemptycontaineristriple-rinsed,leaveitopeninthebackofthehoodovernight.

Solventrinsesmustbedisposedofashazardouswaste.

Notes AnydeviationfromthisSOPrequiresapprovalfromPI.


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Procedure/Use Scale EngineeringControls/Equipment

PPE (eye, face, gloves,clothing)


2.Quenchingofpyrophoricliquids,suchas,butnotlimitedto,sec-BuLi,n-BuLi,Grignardreagents,remaininginbottleorleftafterreactions.

Upto100gofpyrophoricmaterialasaneatliquidorinsolutioninacarriersolvent,either

a)assuppliedinthereagentbottle,uptoamaximumof200mLtotalvolume,or

b)dilutedafteruseinareactionaccordingtothePyrophoricsSOP.

Quenchingofpyrophoricmaterialsinamountsgreaterthan100gor200mLofcommercialsolutionatatimeisnotpermitted.

ConductinacleanfumehoodwiththesashaslowaspossibleusingtheSchlencktechniques,oraninertatmosphereglovebox.




Generalguidance:

Forindirectcontact(closed-systemproceduressuchastransfersviasyringeorcannula)ANDdirectcontact(opensystemproceduressuchasspillhandling,wipingofresidualpyrophorics)withpyrophoricmaterial-acombinationoffireresistant(FR)liners,coveredwithapairofchemical-resistantdisposablegloves(e.g.nitrileglovesorthosespecifiedinthespecificSDS)),mustbewornATALLTIMES.ThefollowingproductsareApprovedFRLiners:Ansell

NoteonGlasswareSize:Ifquenching100gofpyrophoricmaterial,thepyrophoricmaterialwillbedilutedin500mLofinertsolventtostartthequenchingprocedure(20%wtsolution).Inthiscase,therequiredsizeforthequenchingvesselis1L,noless.-QuenchinginaFUMEHOODusingaSchlenkline-Generalconsiderations:



AdditionofmaterialmustbedoneSLOWLY,underadequatestirring/mixing.


Ifyou’requenchinginaRBflaskoranyfloatingvesselinabath,clampit.Ifthesolutionlevelislow,youcandiluteitwithsomeinertsolventsuchastolueneorhexanefirsttolessthan20%wt.Procedure:

Transferthedilutedsolutiontothequenchingvessel,placeaniceundertheflask,andturnonthestirrer.

Beforeproceedingwiththequenchingofthe


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Seenoteforappropriateglasswaresizeselection.Minimalquantitieswillbeleftafterreactionscarriedoutatscaleslistedinyourlaboratory“PYR”ClassSOP.

ObtainPIapprovalifhigherscaleisnecessary.

Kevlar®Goldknit®Lightweight70-200andHanzNomex®FlameResistantUtilityLinerGloves.Clothing:WearNomexIIIA(NFPA2112)labcoat;wearnon-syntheticclothingunderlabcoat;fulllengthpantsorequivalent;andclose-toedandclose-heeledshoes.

pyrophoricsolution,proceedwiththecleaningoftheemptybottle.

RinsetheemptycontainerthreetimeswithaninertdryCOMPATIBLEsolventsuchastolueneorhexane.Therinsesolventmustbetransferredinandoutofthecontainerunderaninertatmosphere.

Aftertheemptycontaineristriple-rinsed,removethesure-sealcapandleaveitopeninthebackofahoodovernight.

Disposeofthesolventrinseashazardouswaste.

Proceedwiththequenchingofthepyrophoricsolutionbyaddingisopropanolslowlytothequenchingvesselusingasyringeoranadditionfunnel,underadequatestirring,untilnomorebubblingisobserved.

Keepthesolutioncool(50oCorbelow)duringthequenchingprocessbycontrollingthefeedrateofthealcohol.






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-IfquenchinginaFUMEHOODusingdryice-Inthefumehood,placea5-gallonbuckettallenoughtoholdthecontainerofpyrophoricmaterialwithsixinchesofheighttospare.Fillthebucketwitha1-3inchesofdryiceandaddaninertsolventsuchastoluenetocover.Allow5minutesforthesolventtocoolandthecontainertofillwithanatmosphereofCO2.LowerthecontainertothebottomofthebuckettoimmerseitintheCO2atmosphere,carefullyuncapit,andslowlypourthecontentsontodryice.Rinsethewallsoftheemptycontainerintothebuckettwicewithasmallamountoftoluene,thenisopropanol.Gentlystirthedryicewithaspatulaorrodtomixtheisopropanolintothequenchingsolutionandallowtowarmtoroomtemperatureandsitatroomtemperaturefortwohourspriortodisposal.

-IfquenchinginaGLOVEBOX-Generalconsiderations:

AnyreactionorsuspensioncontainingthesereagentsMUSTbequenchedcarefully!AdditionofsolventsmustbedoneSLOWLYwithadequatestirring/mixing.


Procedure:


Removebottleorreactionvesselcapandaddastirrerifnecessary.

Typically,asolutionoflessthan20%wtofpyrophoricinaninertsolvent(suchasdryanddegassedhexaneorheptane)iscreated,followedbytheslowadditionofdryanddegassedisopropanoloralessvolatilealcoholsuchasoctanol,underadequatestirringuntilnomorebubblingisobserved.

Placeacaponthequenchingvesselandputthe


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bottle/vesselinazip-topbagbeforetakingitoutoftheglovebox.



Continuethequenchingprocedureinacleanfumehoodwithsashclosed.



Oncetheadditionofwateriscomplete,stirforanadditional2hoursbeforedisposingoftheaqueousorganicwaste.

RinsetheemptycontainerthreetimeswithaninertdryCOMPATIBLEsolventsuchastolueneorhexane.





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Procedure/Use Scale Engineering

Controls/EquipmentPPE (eye, face, gloves,clothing)


3.Quenchingofpyrophoricsolids.

Upto10gofmaterial.

Seenoteforappropriateglasswaresize

Minimalquantitieswillbeleftafterreactionscarriedoutatscaleslistedinyourlaboratory“PYRClassSOP.

Asanalternativetoquenching,rememberthatanyquantitiesoft-BuLicanbedisposedofas

ConductinacleanfumehoodwiththesashaslowaspossibleusingtheSchlenktechniques,oraninertatmosphereglovebox.




Generalguidance:

Forindirectcontact(closed-systemproceduressuchastransfersviasyringeorcannula)ANDdirectcontact(opensystemproceduressuchasspillhandling,wipingofresidualpyrophorics)withpyrophoricmaterial-acombinationoffireresistant(FR)liners,coveredwithapairofchemical-resistantdisposablegloves(e.g.nitrileglovesorthosespecifiedinthe

NoteonGlasswareSize:Ifquenching100mLofpyrophoricsolution,thepyrophoricmaterialwillbedilutedin500mLofinertsolventtostartthequenchingprocedure(20%wtsolution).Inthiscase,therequiredsizeforthequenchingvesselis1L,noless.-IfquenchinginaFUMEHOODusingaSchlenkline-Generalconsiderations:



AdditionofmaterialmustbedoneSLOWLYandensureadequatestirring/mixing.


Ifyou’requenchinginaRBflaskoranyfloatingavesselinabath,clampit.Procedure:


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hazardouswaste.

specificSDS)),mustbewornATALLTIMES.ThefollowingproductsareApprovedFRLiners:AnsellKevlar®Goldknit®Lightweight70-200andHanzNomex®FlameResistantUtilityLinerGloves.Clothing:WearNomexIIIA(NFPA2112)labcoat;wearnon-syntheticclothingunderlabcoat;fulllengthpantsorequivalent;andclose-toedandclose-heeledshoes.

Typically,asuspensionoflessthan20%wtofpyrophoricinaninertsolvent(suchashexaneortoluene)iscreated,followedbytheslowadditionofisopropanolusingasyringeoranadditionfunnel,underadequatestirringuntilnomorebubblingisobserved.

Duringthequenchingprocess,keepthesolutioncool,50oCorbelow,byapplicationofanexternalcoolingbath(icebath)andbycontrollingthefeedrateofthealcohol.





RinsetheemptycontainerthreetimeswithaninertdryCOMPATIBLEsolvent.



-IfquenchinginaGLOVEBOX-Generalconsiderations:

AnyreactionorsuspensioncontainingthesereagentsMUSTbequenchedcarefully!Additionofsolvents


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mustbedoneSLOWLYwithadequatestirring/mixing.


Procedure:


Removebottleorreactionvesselcapandaddastirrerifnecessary.

Typically,asuspensionoflessthan20%wtofpyrophoricinaninertsolvent(suchasdryanddegassedhexaneorheptane)iscreated,followedbytheslowadditionofdryanddegassedisopropanoloralessvolatilealcoholsuchasoctanol,underadequatestirringuntilnomorebubblingisobserved.

Placeacaponthequenchingvesselandputthebottle/vesselinaZiplocbagbeforetakingitoutoftheglovebox.





Oncetheadditionofwateriscomplete,stirforanadditional2hoursbeforedisposingoftheaqueousorganicwaste.


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RinsetheemptycontainerthreetimeswithaninertdryCOMPATIBLEsolvent.



Notes AnydeviationfromthisSOPrequiresapprovalfromPI.Procedure/Use Scale Engineering

Controls /Equipment

PPE(eye,face,gloves,clothing) Procedure Steps and Special Precautions forthisProcedure

4.QuenchingofgloveboxtrashcontaminatedwithPyrophoricMaterials.

Asmall(<1quart)ziplockbagofdrygloveboxtrash(kimwipes,pipettes,weighpaper,etc.)contaminatedwithtracesofpyrophoricmaterial

Minimalquantitieswillbeleftafterreactionscarriedoutatscaleslistedinyourlaboratoryspecific“PYR”ClassSOP.

LargerquantitiesofPYRchemicalscanbedisposedofashazardouswaste.

ObtainPIapprovalifhigherscaleis

Thisoperationshouldbeperformedinthesinkin674Tanimmediatelyfollowingremovalfromtheglovebox.

EyeProtection:Weartight-fittingsafetygogglesorsafetyglasseswithsideshields.

FaceProtection:Faceshieldsaretobeusedwhenthereisnoprotectionfromthehoodsashorwhenthehoodsashisinopenposition.


Generalguidance:

Forindirectcontact(closed-systemproceduressuchastransfersviasyringeorcannula)ANDdirectcontact(opensystemproceduressuchasspillhandling,wipingofresidualpyrophorics)withpyrophoricmaterial-acombinationoffireresistant(FR)liners,coveredwithapairofchemical-resistantdisposable

AfterworkingwithPyrophoricMaterialsintheglovebox,quenchingofcontaminatedtrashshouldbeperformedinthesinkin674Tanimmediatelyfollowingremovalfromtheglovebox.

Allflammablematerialsmustberemovedfromtheareaaroundthegloveboxantechamberandtheadjacentfumehoodpriortobeginningtheprocedure.

GeneralProcedure:

Removethecontaminatedtrashfromthegloveboxinasealedziplockbag.Inasecondarycontainerinthefumehood,quicklyopenthebaganddrownthetrashwithwater.Theremaybeanexothermicreactionorevenbriefflareups,butthesmallquantityofpyrophoriccompoundshouldberapidlyquenchedandtheminimalquantityofflammablematerialinthetrashshouldbeeasilyextinguished.

Letthesoakedtrashquenchinthebagfortwohours.Visiblyinspectthetrashforanyunquenchedresidues(e.g.floatingair-filledvials,pipettesstickingoutofthewater,etc.)beforeappropriatelydisposingofthesolidwasteandwaterquench.


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necessary. gloves(e.g.nitrileglovesorthosespecifiedinthespecificSDS),mustbewornATALLTIMES.ThefollowingproductsareApprovedFRLiners:AnsellKevlar®Goldknit®Lightweight70-200andHanzExtremityWearNomex®UtilityLiners.Clothing:WearNomexIIIA(NFPA2112)labcoat;fulllengthpantsorequivalent;andclose-toedandclose-heeledshoes.



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13.DocumentationofTraining(signatureofallusersisrequired)• Prior to conducting any quenching of pyrophoric materials, designated personnel must provide

training to his/her laboratory personnel specific to the hazards involved in working with thissubstance,workareadecontamination,andemergencyprocedures.

• ThePrincipalInvestigatormustprovidehis/herlaboratorypersonnelwithacopyofthisSOPandacopyofthepyrophoricmaterialSDSprovidedbythemanufacturer.

IhavereadandunderstandthecontentofthisSOP:

Name Signature Identifier Date

Quenching of Pyrophoric Materials · Quenching of Pyrophoric Materials Hazardous Operation SOP Rev....

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