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Standard Operating Procedure

LABORATORY ROTARY EVAPORATORS


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Investigator: General Safety Location: OES Revision: 00
1.0 PURPOSE:
Working with hazardous chemicals at high or low pressures requires planning and special
precautions. Procedures should be implemented to protect against explosion or implosion
through appropriate equipment selection and the use of safety shields. Care should be taken to
select glass apparatus that can safely withstand designated pressure extremes. This SP
pro!ides general safety procedures for the use of rotary e!aporators in a laboratory setting.
2.0 SCOPE:
This procedure applies to all "ouisiana State #ni!ersity Personnel that work in a laboratory and
ha!e the potential to use a rotary e!aporator. $t is the intent of this guideline to pro!ide
information on the proper use of a rotary e!aporator in a laboratory at "S# and afford employee
protection while working in a laboratory.
3.0 RESPONSIBILITIES:
nly trained and qualified personnel shall be allowed to work in a laboratory at "S#. %ach
laboratory worker is directly responsible for safe operation of laboratory equipment. Super!isors
are responsible for ensuring that personnel are trained to work safely in a laboratory. &ll
laboratory personnel are responsible for reading and understanding this procedure.
4.0 DEFINITIONS:
'.( )igh !acuum * Typically (+*, millibars or better produced using a !acuum pump.
'.- "ow !acuum . Typically around ,+ millibars produced by a water pump
5.0 REFERENCES:
/ot &pplicable
6.0 MATERIALS and!" E#UIPMENT:
Personal Protecti!e %quipment
Safety Shielding
0otary %!aporator System

$.0 PROCEDURES:
1acuum work can result in an implosion and the possible hazards of flying glass2 spattering
chemicals2 and fire. $mplosion and flying glass can lead to cuts and lacerations. &ny piece of
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LABORATORY ROTARY EVAPORATORS
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glassware under !acuum has the potential to do harm following implosion. The energy imparted
to flying fragments is directly proportional to the !olume of the glass !essel e!acuated $t is a
common misconception that so called 3high !acuum3 4typically (+*, mbars or better5 systems
present a significantly greater hazard than e!eryday !acuums produced by e.g. a water pump
4around ,+ millibars5. These may differ by four orders of magnitude but the forces to which the
glassware is sub6ected is essentially the same.
$.1 7eneral Precautions 8or Working With 0otary %!aporator Systems
9.(.( Personal protecti!e equipment2 such as safety glasses or chemical goggles2 face
shields should be used to protect against the hazards of !acuum procedures.
9.(.- &lways place a safety screen between the operator and glassware under
increased or reduced pressure.
9.(., nly handle these types of equipment in the presence of others.
9.(.' #se hea!y*wall rubber tubing only. Thin*wall rubber tubing and plastic tubing are
not suitable because they collapse lea!ing a partially e!acuated closed system.
9.(.: &lthough glass !essels are frequently used in !acuum systems2 they can explode
or implode !iolently2 either spontaneously from the strain or from an accidental
blow. Therefore2 pressure and !acuum operations in glass !essels should be
conducted behind adequate shielding. 7lass !essels should be designed for the
operation intended2 and should be !isually checked for star cracks2 scratches2 or
etching marks before each use.
9.(.; 8lasks with !olumes of ( liter or larger and the cooling condenser must be
enclosed in tape or plastic mesh to restrain fragments in case of implosion.
9.(.9 7lass dewars should be fully wound in tape or preferably enclosed in a metal
container.
9.(.< The rotation speed and application of !acuum should be done gradually when
using a rotary e!aporator.
9.(.= >o not hold onto the sample whilst it is re!ol!ing? failure of the flask could result
in serious lacerations to the hands.
9.(.(+ Slowly admit air back into the apparatus after e!aporation of the sol!ent is
complete.
9.(.(( Clean the apparatus after use. >o not mix halogenated and non*halogenated
sol!ents in the recei!er.
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$.2 "ow 1acuum 0otary %!aporators
& low !acuum 4typically around ,+ millibars5 rotary e!aporator system uses a water
aspirator reduce the pressure so that sol!ents can be separated. The use of cold traps
is dependent on the sol!ent.
9.-.( )ook up tubing as between the !acuum source and the rotary e!aporator.
9.-.- @ake sure the round bottom 40A5 flask is twice the !olume as your sample
!olume.
9.-., Beep the inside of all tubing as large as possible so the !acuum is strong.
Suggested !acuum tubing size is approximately ,C(;D wall thickness x :C(;D $>.
9.-.' 8ill water bath with deionized water2 set temperature and turn on.
9.-.: Put sol!ent Ecatch potD in place.
9.-.; 8ill ice bucket and place under catch pot to remo!e as many sol!ents as possible
from condenser.
9.-.9 $f required2 hook up the sol!ent trap and fill it with ice.
9.-.< @ake sure tubing from the condenser carrying the warmed water is in the drain.
9.-.= 8ill cooling coils inside condenser and lea!e cooling water flowing if youFre ready
to e!aporate a sample 4#se chiller if you ha!e one5.
9.-.(+ @ake sure !acuum !al!e at top of the condenser is EopenD so youFre not pulling a
!acuum yet when you put on your sample flask.
9.-.(( &ttach the 0A sample flask to the condenser and fasten into place with a clamp.
9.-.(- Start rotation of flask slowly and gradually increase speed.
9.-.(, Slowly close the !acuum !al!e at the top of the condenser . watch for bubbles in
your sampleG &d6ust !acuum as needed.
9.-.(' nce the sample has stabilized2 lower the flask into the water bath.
9.-.(: Continue the process as long as necessary.
9.-.(; $f you need to break the !acuum to the pump to discard sol!ent from the trap or
add ice to the sol!ent trap2 open the !al!e and lea!e the !acuum pump running.
>iscard sol!entCadd ice2 shut !al!e and continue with rotary e!aporation of
sample.
9.-.(9 When completely done with e!aporating all samples2 open !al!e to break
!acuum and continue to run water at least : minutes.
9.-.(< Sol!ents should be poured into proper bottles and labeled for waste collection.
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$.3 )igh 1acuum 0otary %!aporation Set*#p
& high !acuum 4typically (+*, millibars or better5 rotary e!aporator system include the
use of a !acuum pump or a house !acuum system to reduce the pressure so that high
boiling sol!ents and be separated. The system also requires the use of cold traps to
pre!ent sol!ent contamination of the !acuum source.
9.,.( )ook up tubing as between the !acuum source and the rotary e!aporator. Ae
sure to note the in and out labels on the sol!ent trap.
9.,.- @ake sure the round bottom 40A5 flask is twice the !olume as your sample
!olume.
9.,., %le!ate the !acuum pump abo!e the traps to aid in keeping the sol!ents out of
the pump.
9.,.' Ae sure to add an openCclose !al!e between the last trap and the !acuum pump
to aid in sol!ent remo!al from traps
9.,.: Beep the inside of all tubing as large as possible so the !acuum is strong.
Suggested !acuum tubing size is approximately ,C(;D wall thickness x :C(;D $>.
9.,.; #sing dry ice is the recommended method of keeping the atmosphere cold to
condense the sol!ent. $f you choose to use an ice2 rock salt 4used for making ice
cream5 and water slurry please test the system first to see how many traps you
must use to keep sol!ent out of the !acuum pumps as that can damage the
pumps o!er time. & handy way to check this would be a check of the last side*
arm flask before the pump and see if any sol!ent has precipitated. &lso place a
piece of clear Tygon tubing on the out !ent of the !acuum pump and check for
sol!ent droplets that may ha!e formed. $f you are using glass as part of the
connection in a side*arm flask remember to use glycerin to wet the glass. Wear
glo!es to protect your hands and hold the glass next to the point you are applying
pressure when putting the !acuum tubing on.
9.,.9 The temperature of dry ice is *9<.: HC.
$.4 )igh 1acuum 0otary %!aporation Procedure?
9.'.( 8ill water bath with deionized water2 set temperature and turn on.
9.'.- Put sol!ent Ecatch potD in place.
9.'., 8ill ice bucket and place under catch pot to remo!e as many sol!ents as possible
from condenser.
9.'.' )ook up dry ice trap.
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9.'.: 8ill trap with dry ice or flaked ice and rock salt 4if known to work5.
9.'.; &dd a second and e!en a third side*arm flask EtrapD between dry ice trap and
!acuum pump if you are seeing condensation in the clear tubing coming out of
the !acuum pump.
9.'.9 Place secondary I tertiary EtrapsD into an ice bucket to catch any additional
sol!ent fumes carried past the first trap.
9.'.< @ake sure tubing from the condenser carrying the warmed water is in the drain.
9.'.= 8ill cooling coils inside condenser and lea!e cooling water flowing if youFre ready
to e!aporate a sample. 4#se chiller if you ha!e one.5
9.'.(+ @ake sure !acuum !al!e at top of the condenser is EopenD so youFre not pulling a
!acuum yet when you put on your sample flask.
9.'.(( &ttach the 0A sample flask to the condenser and fasten into place with a clamp.
9.'.(- Start rotation of flask slowly and gradually increase speed.
9.'.(, Slowly close the !acuum !al!e at the top of the condenser . watch for bubbles in
your sampleG &d6ust !acuum as needed.
9.'.(' nce the sample has stabilized2 lower the flask into the water bath.
9.'.(: Continue the process as long as necessary.
9.'.(; $f you need to break the !acuum to the pump to discard sol!ent from the trap or
add ice to the dry ice trap2 open the !al!e and lea!e the !acuum pump running.
>iscard sol!entCadd ice2 shut !al!e and continue with rotary e!aporation of
sample.
9.'.(9 When completely done with e!aporating all samples2 open !al!e to break
!acuum from pumpJ disconnect tubing from inlet of !acuum pump and allow
pump to run at least : minutes to dry out any droplets of moisture that might be
inside it.
9.'.(< Shut off !acuum pump after : minutes. $t is possible to plug the !acuum pump
into a timer so that the pump is turned if you forget to watch the time.
9.'.(= Sol!ents should be poured into proper bottles and labeled for waste collection.
$.5 #se of 8laked $ce
8ollow the SP for general rotary e!aporation setup and procedure. This test procedure
is to !erify whether you can use flaked ice 4Ecrushed iceD5 rather than dry ice in your
rotary e!aporation setup with your particular sol!ent4s5. $t will also indicate how many ice
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traps you need with your particular sol!ent4s5. This @#ST be done with each different
sol!ent or a change in temperature with the same sol!ent.
9.:.( $ce the catch pot. This @#ST be done. $t has been found that approximately (C,
of the sol!ent goes past one trap on to the pumpCdrain when the catch pot is
/T iced.
9.:.- Place ice and rock salt inside the Edry iceD trap.
9.:., 0un your rotary e!aporator and watch for sol!ent collection in the catch pot2 and
dry ice trap. &lso watch for any moisture droplets forming at the outlet of the
!acuum pump. '. $f you ha!e &/K moisture at the outlet of the !acuum pump2
you @#ST add another ice trap.
9.:.' While adding the additional trap2 be sure and disconnect the inlet tubing to the
!acuum pump and let it run to dry it out.
9.:.: &dd a side*arm flask EtrapD between the dry ice trap and !acuum pump.
9.:.; Place EtrapD into an ice container to catch any additional sol!ent fumes carried
past the first trap.
9.:.9 $f moisture is gone from outlet of pump2 connect e!erything and youFre ready to
run your rotary e!aporator again.
9.:.< Watch for moisture droplets forming again at the outlet of the !acuum pump.
9.:.= $f you still ha!e moisture 4sol!ent5 droplets forming at the outlet of the !acuum
pump after icing the catch pot2 and ha!ing two ice traps between the condenser
and the !acuum pump2 then you ha!e no choice but you @#ST use dry ice rather
than flaked ice to make it cold enough to chill your particular sol!ent fumes.
%.0 CONTIN&ENCIES:
%.1 $n case of a fire2 explosion2 or gas leak e!acuate indi!iduals from the area and call the
emergency response 4=((5. /otify super!ision and ad6acent personnel as quickly as
possible. bser!e appropriate procedures for personal in6ury or fire as pro!ided in %S
Web site.
%.2 $n case of a chemical spill2 alert others in the immediate !icinity and notify your
super!isor. >etermine the se!erity of the spill and proceed as appreciate. Small spills
may be cleaned up by laboratory personnel. 8or large spills2 notify %S 4:9<*:;'+5 and
Campus Police 4=(( or :9<*,-,(5. $f possible to do so safely 4without risk of o!er*
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exposure52 take action to stop the release. %nsure that extraneous personnel remain at
a safe distance until the spill is completely cleaned*up
'.0 REVIE(S AND REVISIONS:
This procedure shall be re!iewed for compliance and effecti!eness and re!ised as necessary on
an annual basis.
10.0 ATTAC)MENTS and REFERENCE FORMS:
/ot &pplicable
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