a JCHAS 723 14 Gears Case study - Incident investigation Laboratory explosion Laboratory accidents are not uncommon; evaluating the cause of an incident can help the organization take preventive measures, assess worker skills, and design appropriate training, All accidents are the result of, either unsafe acts, unsafe conditions, or both. This paper analyzes a procedure which resulted in an explosion and property damage in a laboratory facility, evaluates potential causes, and provides recom. mendations to prevent a reoccurrence. By Russell Phifer cause of the accident and (2) provide recommendations for future guidelines to prevent a recurrence. The Site was inspected and those involved with the incident were interviewed, Included in A Postdoctoral Research Associate the review was the researchers labora~ was performing a synthesis of hydro- ory notebook, the facility Chemical symethylfurfural (HME) in a thick TYygiene Plan, and research papers walled glass tube closed with a Teflon provided by the Post-Doc covering stopper when the tube exploded Phy- Similar experiments sical damage was limited to the che- tical hood where the process was being performed, The hood facing yNcIDENT SUMMARY was severely cracked and the hotplate on which the synthesis was being The procedure was one of a group of Iheated was severely damaged. There projects fanded by an intemationel were no reported injuries. pharmacy-sponsored grant. Approxi- ‘The objectives of this investigation nately 39 similar expertinents are part and report are to (1) determine the of this project. The abjectve ofthe experiment was usd Pils Cw afland wah tH conversion of sucrose into Be tree tal LLC What che, hydroxymethyifurtral using siies-sul- A one tetas ea frie acid as a catalyst. The process INTRODUCTION/OBJECTIVES of 5 ml of a saturated sodium chloride solution, and 91m of dimethylsulfox- ide. The procedure called for heating these components in a thick walled glass tube with a Teflon screw top at 150 °C for 6h with constant stizring using a small magnetic stir bar. The stirring speed was reportedly set at 200 rpm. A silicone oil bath placed fon top of a Coming PC 420 hot plate was used for heating the reaction. The hot plate had reportedly not been used previously, though no one inter- viewed was able to identify if it was new or simply new to this laboratory. ‘The instruction manual for the hot- plate was reviewed for this investiga- tion.’ The procedure was performed in chemical hood, with the experiment Thutp://eatalog2 coming com/Life- ee ene es a utilized 500 mg of sucrose, 250mg of sciences/media/pdi/hotplate_digital whiferss fahcom) catalyst, an aqueous phase consisting pdt Terese © Dison of Chemical Hea and Satay of he Aran Chemical Society i duaotog/ 10 /iehas.2014.08,001 sever ie Al ight sen 10.1016 jehas:2014,04.001 ‘Please cite this article in press as: Phifer, R., Case study — Incident investigation, J. Chem, Health Safety (2014), doi:itp x doi ore!CHAS 723 1-4 apparatus placed approximately 15-20em from the sash, which was completely lowered. There was a simi- lar experiment placed approximately 30 cm to the right ofthe subject experi- ment. The other procedure used a dif- ferent model hotplate and a different carbohydrate (cellulose), but was otherwise essentially identical. Also in the hood, placed along the right rear wall, were approximately 14 contain- ers, some of which were labeled hazar- dous waste or otherwise identified as waste, These included some flammable organic materials in small quantity ‘The hood had a posted face velocity, cf 102 cfm; the most recent test date was August 27, 2012, Approximately 4h into the proce- dure, there was an explosion in the hood, which also subsequently initiated a small fire involving the hotplate power wire and the silicone oil bath, The sash withstood the explosion but was badly cracked. The heating pad was badly damaged, and the experiment glassware destroyed. At the time, the Post-Doe was at his desk which is located approximately 10m from the hood and slightly around a comer. He could not have observed the reaction from this location, He indicated he heated the silicone oil bath to 150 °C prio: to placing the apparatus im the bath, and checked on the tem- perature and the reaction “periodi- cally” during the first 4h of the planned 6-h procedure and did not notice a rise in temperature OBSERVATIONS. ‘The experiment apparatus was care. fully inspected to attempt to deter- mine the cause of the explosion, The thick walled glass tube and beaker in which the tube was immersed were obliterated; the Teflon stopper showed no specific defects, but the o-ring could not be located. The hot- plate showed signs of severe down- ward depression, with the surface top compressed through two layers of insulation and an aluminum bot- tom. The inside electronics of the hotplate showed little or no damage visible from the underside. The hotplate model, Coming PC420D, like other similar models, has failed before to properly maintain tempera- ‘ure, At the University of California ~ Berkeley, the same model reportedly overheated while the heat control was in the “off” position.’ Hot plates tend to cycle on and off rather than out- putting a constant temperature, This can result in drifting of the desired ath temperature by up to +10°C. In addition, virtually no commercial laboratory ‘hotplate is _explosion- proof, so ifthe bath material is heated above its flash point a fire and/or explosion could occur.® The hood itself was inspected; aside from the adjacent experiment, there ‘were approximately 14 other contain- ers of chemical or waste in the hood at the time of the incident. Ultimately, the cause of the accident was failure 10 properly monitor the procedure. Based on inspection of ‘the equipment in the aftermath of the explosion, it appears the temperature of the bath was allowed to rise well above the planned 150 °C endpoint, resulting in an increase in pressure in the closed reaction above the thresh- ld of the thick-walled tube. It is pos- sible there was.a defect in the tube that, ‘was not noticed prior to the experi- ment; itis also possible the tempera ture controller on the hotplate failed. ‘That problem could have been avoided if an external temperature controller (an available option for ‘the hotplate; there are numerous on the market) had been utilized to con- vol the temperature of the oil bath. Instead, the temperature controller monitoring the hotplate surface was the only control device. While itis also possible that the rubber o-ring on the ‘Teflon stopper failed, the release in pressure was sufficient to damage the hhood sash, the top of the hood, and severely damage the hotplateina down- ward direction, indicating the system was overly pressurized. If either the o- ring or Teflon stopper had failed, the pressure release would likely have been Thup://ehs uer.edu/laboratory/hot- platesafetyadvisory20110715 pat ‘http://www ilpi.com/inorganic/ slassware/heatsources html upinstead ofin all directions. The cause of the smoke and fire that melted the ‘hotplate wiring was the silicone oil bath catching fire, indicating a strong like- lihood that a temperature above 250°C was reached, as this is generally the flashpoint or decomposition point of silicone oil. The boiling point, though not provided by the manufacturer's MSDS, is approximately 120°C. INTERVIEWS ‘The department chair was interviewed. He also provided pictures talcen by the ‘county HazMat team who responded to the pulled alarm, He noted that the incident equipment and chemicals were subsequently removed and the area cleaned, though the hotplate and other reaction equipment were available for inspection at the time of the site visit “The researcher has one patent pend- ing on catalytic oxidation of furfural ‘compounds and has co-authored sev- ‘eral professional papers related to this experiment and similar projects. His ‘current field ofresearch is carbohydrate conversions. He discussed his back- ground, reviewed the experiment pro- cedure, and when asked about laboratory safety training, indicated it hadnot been provided at the University He was unable to provide any docu- ‘mentation of isk or hazard assessments ‘completed before or as part of his eur- rent project, It was his opinion that the explosion was the result of a hotplate ‘malfunction. ‘The Principal Investigator involved with the research project on carbohy- drate conversions was interviewed, His specialties include development ‘of novel synthetic methodologies and reagents for organic synthesis as well as synthesis and evaluation of novel small molecules as cancer chemother- apeutics. He teaches organic chemistry and organic spectroscopic analysis at the university, ‘Also interviewed was an Associate Professor teaching analytical chemis- ty at the university. His research involves the development of chemical and biological sensors. Both professors indicated they believe the experiment failed due to a hotplate malfunction, 2 Journal of Chemical Health & Safety, Mayllune 2014 10,1016) jehas:2014.04,001 Please cite this article in press as: Phifer, R, Case study — Incident investigation, J. Chem, Health Safety 2014), doitip//dx doi ore!JCHAS 723 14 Both felt the research associate was a _‘iability to the university. Had he 3 Initial employee laboratory safety competent, qualified, and experienced eceived such training, he may not ‘taining should be completed within ‘chemical researcher have been working alone, and may the fist two weeks of employment. “Also mferviewed wasthe Director of -~“haVe “monitored “the experiment This taining should be presented by Favironmental Health & Safety at the more closely, particularly the tem- the Environmental Health & Safety university: He was interviewed tegard- perature of the oil bath. While not office and should inchude documen- ing general safety practices, chemical _-S€r™mane to this investigation, this tation of satisfactory completion. hygiene training. and other aspects of Wasthesecondlaboratory explosion ‘The EH&S office has the expertise ulely implementation associated with _ iolving this particular researcher. and resources necessary to provide the Departments of Chemistry & Bio. 5 Based on anecdotal evidence, the effective training, Observations indi- Chemistry, He stated that the BH&S izamediate response to the incident cate that faculty and staff do not Office isnot involved in the presenta, Bears tohave been appropriatein necessarily have the time oF tion of chemical hygiene or other lab all tespects. Due to the presence of __resoutrees to take that responsibility. Safety taining for the Department of smoke, the building alarm was ‘The Post-Doc should receive train Chemisty pulled promptly, the building was ing in laboratory safety as well as evacuated, and the county HazMat Chemical Hygiene training as team was called required by the OSHA standard CONCLUSIONS/CONTRIBUTING 6 While not specifically within the DIRECT CAUSES scope ofthis investigation, the Che- rical Hygiene Plan which was 1 The most likely primary cause ofthe RECOMMENDATIONS reportedly reviewed & revised in accident is a rapid, uncontrolled Jue 2013 subsequent to the inci- increase in temperature of the reac- 1 Closed system experiments invol- dent, lists obsolete sources in the tion, resulting in a pressure buildup ving the addition to heat should be Introduction and appendix; the in excess of the procedure appara. constantly monitored, ideally with 1981 Prudent Practices for Handling ‘tus’s containment ability. There is no ‘an external temperature controller Hazardous Chemicals in Labora- evidence of @ runaway reaction 0 control the heat of the bath tories has been revised three times ‘Causing the explosion based on the instead of the hotplate surface. If since that version, in 1983, 1995 and ‘components no controller is to be utilized, the again in 2011, There have been sig- 2 Since the thermal stability of sili- temperature should be checked at nificant changes in best practices cone oil (polydimethylsiloxane) is least every 10min. Heating of any since the 1981 version; the newest Sharply decreased by the presence reaction in a closed system repre-_vetsions the basis for changes othe foftrace impurities capable ofattack- sents a potentially hazardous proce- __-on-mandatory Appendix A of the ing the siloxane bond, the fie may dure. Thisisnoted inboldtypein the OSHA’ Laboratory Standard in hhave been the result of the experi-_ Chemical Hygiene Plan 2015.'"The changes suggest numer- rent components contacting the ol 2 Risk assessments should be per oussigniicant modifications to Che- altertheexplosion-The fre may also formed and documented for each __mical Hygiene Plans in the areas of have been initiated by the hot oil research experiment prior to begin- __petsonnel responsibilities, duties of contacting the hotplate electronic ng work, with the Principal knves- a Chemical Hygiene Oificer, empha- components and wiring tigator responsible for approving the _sis on “program”, elements of risk 3 Other possible contributing factors _ procedure in writing assessment, safety culture, and the include: failure to thoroughly 3 The policy against working alone in _ physical layout and equipment in inspect and/or test the hotplate the laboratory, particularly during the laboratory. Also, the Chemical before its initial use; not utilizing the use of “hazardous procedures Hygiene Plan specifies monthly eva- fan extemal heating controller, the oF work with highly oxicmaterials", ‘ation of ‘chemical hood perior- high density glass tube may have should be strictly enforced. mance, but this is apparently only been defective, and the lack of an 4 Hoods that are being used for performed annually. A more thor- cllective preventive maintenance esearch experiments should not ough review and significant revi- program for laboratory equipment. also. be used for waste storage, sions to the University Chemical 4 There is no documented evidence Waste should be properly labeled, _ Hygiene Plan (CHP) are needed. that the PostDoc researcher has stored with secondary containment, 7 The Safety Committee needs tocom- ever received any laboratory safety and moved to the central accumula. "it to. performing regular safety tuaining. This is a serious violation tion area weekly, as specified by the _ispections and documenting those of regulations, presenting potential CHP. inspections Titips//www osha gov/pls/oshaweb/ owadisp show_document?p_table= STANDARDS&p_id=10107 ‘Journal of Chemical Health & Safety, May/June 2014 3 Ties ie is cle np les R, Ce way not vegan, 1. he els Say G18, ap 10.10164j,jchas.2014.04.001 * ma 7BAS 14 APPENDIX A. PHOTODOCUMENTATION Post- incident picture of equipment setup Tube/stopper setup Teflon stopper from subject experiment * Journal of Chemical Health & Safety, Mayllune 2014 Please cite this article in press as: Phifer, R, Case study ~ Incident investigation, J. Chem, Health Safety (2014), doitip/dx doi ore! 10,1016) jehas:2014.04,001