STANDARD OPERATING PROCEDURE

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USE OF AUTOCLAVES 1. Introduction This SOP discusses the procedure and safety guidelines for the use of Teflon-lined, stainless steel laboratory autoclaves. The autoclave is a closed stainless steel vessel with an internal cup and lid made of Teflon. The instrument can be charged with reagents, and closed. Under e ternal heating, the contents will be raised to higher temperatures and pressures than within an unsealed container. The autoclaves are specifically designed for harsh chemicals, high temperatures and high pressures. !. Scope This procedure applies to all staff, students and visitors of the "dvanced Porous #aterials $roup in the school of %hemistry at the University of #elbourne that wor& in the laboratory and have the potential to use the autoclave for solvothermal or hydrothermal e periments. '. Safety Personnel who operate the autoclave must be trained to understand proper pac&aging, loading, labelling, as well as operation and emergency procedures.

General precaution ! Personal protective e(uipment )PP*+ including safety glasses or face shield, closedtoed footwear, and laboratory coats must be worn when charging or opening autoclaves, and heat-insulating gloves must be put on when removing the autoclaves from the oven. Only trained laboratory personnel can operate the instrument. -eagents used in the vessel must not react to release gas. This will lead to e cessive pressure build-up. .efore every use both the stainless steel shell and the Teflon liner should be visually inspected for crac&s, pitting, rust, metal creep or e cessive wear " Steel #ell t#at are crac$ed or fla%ed in any %ay &u t 'e di carded . /arn or distorted Teflon liners should be replaced. /hen charging the autoclave with reagents, the Teflon liner should never be filled more than 01 percent )filling fraction+. This will ensure that there is sufficient headspace for vapour formation and fluid e pansion when the vessel is heated. 2itric acid should not be used with organic materials to prevent the formation of nitro e plosives.

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-eactions which are highly e othermic or which release large (uantities of gas )such as an o idant and an organic compound+ should not be performed in the autoclave. Perchloric acid should NEVER be used in the vessel. 3o not overheat the autoclave. The ma imum temperature is !11 4%. 3o not e ceed the pressure limit for each run. 5t should be verified if the pressure e pected is within the limits of the device. %hec& relevant vapour pressure tables. This model has a spring-assisted pressure plate system that will release energy should the pressure within the vessel e ceed the autoclaves specifications. 2othing must ever be done to inhibit the function of the pressure plate system. The spring must be replaced if it shows signs of e cessive wear. "fter heating, the autoclaves must be allowed to naturally air cool on a heat-resistant plate. The autoclaves should NEVER be (uenched in water. "fter use, the autoclaves must not be opened until they are fully cool. *ven then, they should be opened with care because the contents may still be under pressure.

Ri $ of i&plo ion or e(plo ion! #aterials should not be autoclaved if they6 %ontain radioactive material. %ontain or are suspected of containing ha7ardous chemicals )solvents or corrosives+. %hemicals that will become unstable8volatile at elevated temperatures. %ontaminated sharps. Incident Re pon e! 5f any in9ury occurs see& first aid or, if necessary, see& medical assistance. 5f clothing is soa&ed in hot water8steam, remove clothing and cool the in9ured part in cool water. Place a notice on the autoclave indicating that it is not to be used until the cause of the incident is determined, procedures enacted to prevent future incidents, and the autoclave is deemed safe for operation. "ll other non-emergency incidents are to be reported to *:;S Spill Clean Up! <isibly inspect the autoclave and inside of the oven prior to cleaning any ruptured e(uipment. Spills may occur from a boil-over or brea&age of containers. 2o operation of the autoclave is allowed until the spill is cleaned up. The operator is responsible for clean-up of spills. %ontain the spilled material using materials from the spill &it to absorb or contain the spill. /ait until the autoclave and materials have cooled to room temperature before starting the cleanup inside the autoclave. -eview the #aterial Safety 3ata Sheets )#S3S+, if appropriate, to determine the protective e(uipment, spill cleanup, and disposal protocols that are necessary.

STANDARD OPERATING PROCEDURE

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%lean the e(uipment and wor& area in order to collect and remove all spilled materials. 3ispose of the waste following the protocol appropriate for the material. 5f materials have been intermingled, follow the cleanup and disposal protocol for the most ha7ardous component of the mi ture.

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Licence and Per&it "ccording to "ppendi . from "S ='='-!11> Pressure *(uipment ? :a7ard @evels, no licences are re(uired for use of the autoclaves.

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Trainin) and Co&petency The trainee must have already mastered an understanding of and have been given the instruction in the use of autoclaves by an approved trainer )the instrument supervisor or any trained member of the "dvanced Porous #aterials $roup. %ompetency will be assessed by close observation of the trainee by the instrument supervisor or an approved trainer. The training records are stored in the "dvanced Porous #aterials @aboratory Safety Aolder.

B.

Ri $ A e &ent -efer to the following ris& assessment forms6 Use of autoclaves, assessed 1C81D811. Use of oven, assessed 1C81D811. Use of electrically operated e(uipment, assessed !181B81D. /aste solvent disposal, assessed 1C81181C.

D.

E*uip&ent and +aintenance , -andlin) and Stora)e , La'ellin) "utoclaves to be engraved with uni(ue numbers. Only matched autoclave parts are to be used. 2o mi -matching of lids to bodies allowed. 2o person shall operate the autoclave unless the autoclave is in good repair. Users are not to ma&e repairs. "utoclaves shall be maintained and repaired by (ualified persons. 5f the autoclave does not operate e actly as e pected, a notice shall be placed on the autoclave indicating that it is not to be used until the problem is diagnosed and corrected. "utoclaves are to undergo visual inspection prior to use, and stringently inspected every si )B+ months.

Si)na)e Signage indicating E:a7ardous Process UnderwayF must be displayed when autoclaves in use.

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0.

Operatin) Procedure

Fi)ure ." Schematic of autoclave. Loadin) Autocla/e ! 1. Place the desired reagents into the Teflon Liner )charging+. 3o not mi incompatible materials 3o not overload, leave sufficient room for steam circulation. The ma imum volume allowed is 01 percent. !. Place the stainless steel Bottom Plate into stainless steel Autoclave Body and ensure that the Bottom Plate is in the correct place. '. *nsure that the lip of the Teflon Liner is free from any li(uid8solid by gently cleaning with a Gimwipe. =. Place the Teflon Lid onto the Teflon Liner. 2othing should impede good contact between the lid and liner. >. $ently place the charged Teflon Liner into the Autoclave Body. B. Place the Lower Pressure Plate onto the Teflon Lid ensuring that the spring cavity is facing s&ywards. D. Place the Spring into the spring cavity of the Lower Pressure Plate. Only undamaged springs should be used. 0. Place the Upper Pressure Plate onto the Spring/Lower Pressure Plate/Autoclave Body assembly spring cavity side down. C. Screw the stainless steel Screw Cap onto the Autoclave Body assembly until finger tight. Then secure the autoclave assembly into a vice and tighten the lid with a spanner. 3o not over-tighten ? un-tighten by a H turn from full tightness. 3o not cross-thread the Autoclave Body and Screw Cap. 11. Transport the autoclave assembly8s to the reaction ovens )-oom '1D+. 3o not e cessively tilt the autoclaves. Spilling into assembly may occur. /arning ? charged autoclaves are heavy.

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11. %ommence hydrothermal8solvothermal reaction by placing the autoclave assembly8s into the reaction oven. The oven may be preheated or cold. /ear heat-insulating gloves when placing autoclaves into a preheated oven. Unloadin) Autocla/e ! 1. Put on appropriate PP* including heat-insulating gloves and safety glasses or face shield prior to handling heated autoclaves. !. Open oven door and gently remove the autoclave8s and place them on a thermalresistant plate to cool down. "llow the autoclave8s to cool down naturally. Do not *uenc# the temperature by placing autoclave8s into cold water. Shut down the oven if necessary prior to removal of autoclave8s. '. Place the autoclave assembly into the vice and secure. =. Unscrew the Screw Cap of autoclave using the spanner. Only open an autoclave when completely cooled. >. $ently remove the Pressure Plate/Spring/Teflon Liner assembly from the Autoclave Body by slowly pressing the Bottom Plate upwards. -emove the Pressure Plates and Spring prior to removing the Teflon Liner and Teflon Lid. B. -emove the reactant from the Teflon Liner and process as re(uired. D. /hen complete, clean the Teflon @iner and dry. Place the autoclave assembly into the designated storage bo . *nsure that all matched autoclave parts are stored together )screw cap, pressure plates, autoclave body, etc.+. C. Control and Cali'ration Stringent visual inspections of the autoclaves are to be performed every si )B+ months to e amine their structural integrity. The autoclave should be ta&en out of use if there is any evidence of damage, deterioration or metal creep on the thread of the autoclave body, lid or other stainless steel components. 11. 0a te Di po al Solvent 3isposal6 3ispose of solvents in the appropriate waste container )e.g. /ater soluble waste solvent, water insoluble waste solvent, halogenated waste solvent+. 11. Rele/ant Docu&ent , Reference Standard Operating Procedures and <apour Pressure Tables6 Use of laboratory oven, "dvanced Porous #aterials @aboratory, School of %hemistry, The University of #elbourne, <ersion 1.1, 1D81D811. Parr Operating nstructions! Parr Acid "igestion Bombs, Parr 5nstrument %ompany, 2o. !=C#. Parr Safety in t#e Operation of Laboratory $eactors and pressure vessels , Parr 5nstrument %ompany, 2o. !'1#.

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Perry, -.:., 3./. $reen, and I.O. #aloney, Perry%s C#emical &ngineers% 'andboo(. 0th ed. !110, 2ew Jor&6 #c$raw-:ill. 1 v. )various pagings+. -is& assessments applicable to the SOP are listed in Section B. 1!. Si)na)e , Su&&arie , Te&plate %ompetency Training -ecords Aorm ? "ttached, see page 0. %opies of this form are to be stored and filed and in the "dvanced Porous #aterials %ompetency -ecords Aolder. 1'. Appended +aterial The following formula is provided from "S ='='-!11> Pressure *(uipment ? :a7ard @evels to what these vessels were calculated to. APPENDI1 2 NU+ERICAL +ET-OD OF DETER+INING -A3ARD LEVELS FOR PRESSURE VESSELS )5nformative+ 2. GENERAL The ha7ard levels of pressure vessels in Table 1 are based on the following numerical method )see %lause !.!.'+. 24 +ET-OD 3etermine ha7ard level value ):+ from *(uation .1. ' ) p * +c +f +s /here6 ' p * +c K ha7ard level value, in megapascal litres K design pressure, )see @egend to Table 1+, in megapascals K volume )see 2ote ' of Table 1+, in litres K compressibility and mass factor )see 2ote 1 of Table 1+ K 1 for li(uid K 11 for gas +f K contents )fluid+ factor )see 2ote 1 of Table 1+ K 11L1.> for non-harmful li(uids )e cept as provided in Table 1 note >+ K 1.1 for non-harmful gas K 111.> for harmful li(uid or gas K 11 for very harmful li(uid or gas K 1111 for lethal li(uid or gas +s K location or service factor K 1 unless one of the following conditions apply K ' for one of the conditions in 2ote =)a+ of Table 1 K 11 for more than one of the conditions in 2ote =)a+ of Table 1 K '1 for P M>1 #Pa )see 2ote =)b+ of Table 1+ . . . .1

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K 1N' for one of the conditions in 2ote =)c+ of Table 1 K 1N11 for more than one of the conditions in 2ote =)c+ Table 1 K ' for human occupancy vessels )see 2ote =)a+ of Table 1+ The pressure vessel calculations obtained from information provided by the manufacturing company6 p K 1.! #Pa * K 1.1 @ +c ) 1 +f K 11 +s K 1 : K p * +c +f +s therefore ' K 1.! 1.1 1 K 1.! #pa.@ K :a7ard @evel * )negligible ha7ard+ 11 1

Obtaining the ha7ard level from the ha7ard level value as given below6 :a7ard level value ):+ O11 P11 P11
= ' !.>

:a7ard @evel * 3 % . "

P11!.> to O11' to O11 to Q11 M110.>

= 0.>

The contents )fluid+ factor used for the calculations was very harmful li(uid )11+, however most of the chemicals that will be used, will fall under either the harmful or non-harmful categories further reducing the ris& levels.

STANDARD OPERATING PROCEDURE

SP R "P#11B Page 0 of 0 <ersion6 1.1 3ate6 1081D811 -evise by6 1081D811 -eplaces6 28" /ritten by6 @u %ao -eviewed by6 3ana #organ "uthorised by6 -achel %aruso

"dvanced Porous #aterials @aboratory, School of %hemistry, The University of #elbourne

ADVANCED POROUS +ATERIALS LA2ORATOR5 CO+PETENC5 TRAINING RECORDS 6 AUTOCLAVES Co&petency

3ate Trainee Trainer

Date

Na&e

Uni/er ity,Dept"

Trainer