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University of Stirling School of Biological & Environmental Sciences Laboratory Risk Assessment Form Instructions for completing form: if using MS Word view as Normal Layout, zoom to 100%. Type information within the boxes provided. These will expand to accommodate the text. Before printing check File, page setup, page size is A4. 1. Title of Work Activity. Determination of soil exchangeable cations and cation exchange capacity 2. Description of Work Activity (describe Method/Working Procedure/Protocol, including safety precautions and emergency procedures where necessary). Exchangeable cations and cation exchange capacity 1.0 M potassium chloride Dissolve 74.56g KCl in distilled water. Transfer to a 1000ml flask and make to volume with distilled water. 0.01M sodium hydroxide Dissolve 0.4g NaOH in distilled water. Transfer to a 1000ml flask and make to volume with distilled water. Prepare in a fume cupboard . Strontium nitrate/hydrochloric acid solution Dissolve 10 g strontium nitrate in distilled water. Transfer to a 100 ml volumetric flask and dilute to volume with distilled water. Pipette 8.9 ml conc. hydrochloric acid into a 100 ml flask half full of distilled water. Cool and dilute to volume. Mix the two solutions in a reagent bottle. Prepare in a fume cupboard . phenolphthalein indicator Dissolve 1g of phenolphthalein in 100ml ethanol then mix with 100ml distilled water stirring constantly. Filter if a precipitate forms and transfer to a reagent bottle. 0.5 and 1 mmol c L -1 Mg standards Pipette 0.6 and 1.2 mL stock Mg standard solution into 100 mL flasks. Pipette 4 ml strontium nitrate/hydrochloric acid mixture into each flask and make to volume with KCl solution. 1 and 2 mmol c L -1 Ca standards Pipette 2 and 4 mL stock Ca standard solution into 100 ml volumetric flasks. Pipette 4 ml strontium nitrate/hydrochloric acid mixture into each flask and make to volume with KCl solution. Exchangeable cations are displaced by leaching soil with a solution of potassium chloride. In the leachate, exchangeable calcium and magnesium are determined by atomic absorption spectrometry and exchangeable acidity by titration against standard sodium hydroxide solution. We will ignore the generally small contributions from Laboratory Risk Assessment Form Ver. 1.0 Page 1 of 7 Reference number: E4-

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University of StirlingSchool of Biological & Environmental SciencesLaboratory Risk Assessment FormInstructionsforcompletingform:if usingMSWordviewasNormal Layout, zoomto100%.Type information witin te !o"es provided.Tese will e"pand to a##ommodate tete"t.$efore printing #e#% &ile, page setup, page size is '(.1. Title of Work Activity.etermination of soil e!changeable cations an" cation e!change ca#acity2. escri#tion of Work Activity (describe Method/Working Procedure/Protocol, including safety precautions and emergency procedures where necessary).Exchangeable cations and cation exchange capacity1.0 M potassium chloride Dissolve 74.56g KCl in distilled water. Transfer to a 1000ml flask and maketo volume with distilled water.0.01M sodium hydroxide Dissolve 0.4g Na! in distilled water. Transfer to a 1000ml flask and maketo volume with distilled water. "re#are in a fume $u#%oard.Strontium nitrate/hydrochloric acid solutionDissolve 10 g strontium nitrate in distilled water. Transfer to a 100 ml volumetri$ flask and dilute to volume with distilled water. "i#ette &.' ml $on$. h(dro$hlori$ a$id into a 100 ml flask half full of distilled water. Cool and dilute to volume. )i* the twosolutions in a reagent %ottle. "re#are in a fume $u#%oard.phenolphthalein indicator Dissolve 1g of #henol#hthaleinin 100ml ethanol then mi* with 100ml distilled water stirring $onstantl(. +ilter if a #re$i#itate forms and transfer to a reagent %ottle.0.5 and 1 mmolc L-1 Mg standards"i#ette 0.6 and 1., m- sto$k )g standard solution into 100 m- flasks. "i#ette 4 ml strontium nitrate.h(dro$hlori$ a$id mi*ture into ea$h flask and make to volume with KCl solution.1 and 2 mmolc L-1 a standards "i#ette , and 4 m- sto$k Ca standard solution into 100 ml volumetri$flasks. "i#ette 4 ml strontium nitrate.h(dro$hlori$ a$id mi*ture into ea$h flask and make to volume with KCl solution. /*$hangea%le $ations are dis#la$ed %( lea$hing soil with a solution of #otassium $hloride. 0n the lea$hate1 e*$hangea%le $al$ium and magnesium are determined %( atomi$ a%sor#tion s#e$trometr( and e*$hangea%le a$idit( %( titration against standard sodium h(dro*ide solution. 2e will ignore the generall( small $ontri%utions from e*$hangea%le Na and K and $al$ulate effe$tive C/C as the sum of e*$hangea%le Ca1 )g and a$idit(.i. 2eigh 5 g 340.01 g5 of dr( soil into a $lean 50 ml %eaker. 6dd ,5 ml #otassium $hloride 3KCl5 solution and stir thoroughl(.ii. "la$e a filter #a#er in a funnel over a 100 ml $olle$ting %ottle. "our the soil sus#ension through the filter. 2hen the li7uid has drained1 lea$h the soil with 8 further ,5 ml #ortions of KCl1 allowing ea$h to drain %efore adding the ne*t 3total of 100 ml lea$hing solution5. 9etain the lea$hate for anal(sis of Ca1 )g and a$idit( on$e drainage has sto##ed.iii. Determination of e*$hangea%le Ca and )g :sing a measuring $(linder1 transfer ,5 ml of the lea$hate to a $lean %eaker and add 1 ml strontium nitrate solution. Determine the $on$entrations 3as mmol$ l;15 of Ca and )g in the lea$hate %( atomi$ a%sor#tion s#e$tro#hotometr( 366< 3?5=H Mg Ca CEC + + =CECMg CaBaseSat5 3 100 +=!. Location (list laboratories in which work will be carried out).$U$% &'( an" (B)**". The follo+ing gro,#s of #ersons may be at risk- Aca"emics Technicians St,"ents 'isitors .leaners /aintenance 5. 0a1ar"o,s /aterials ,se" as Ra+ /aterials (Complete C!""/#isk $ssessment !ummary !heet. %ist all compounds, which are harmful, irritant, corrosi&e, flammable, to'ic, teratogenic, and carcinogenic or ha&e an (% or M(%, microorganisms, dust etc. )ick the appropriate bo'es for ha*ard classification, route of contact and personal protecti&e e+uipment).See anne! sheet#.0a1ar"o,s s,bstances create" as interme"iates or by2#ro",cts.3one$. /etho" of is#osal of Waste. Categorise waste as laboratory drain, normal landfill or specialist disposal. Categories for specialist disposal are i) sol&ents (non,chlorinated hydrocarbons and alcohols, chlorinated sol&ent, acetonitrile or others. -... sol&ents containing acetonitrile, ben*ene and tetrahydrofuran must be kept separately, ii) solids (acid, o'idising and to'ic). Consult the !afety $d&iser if you are in any doubt about which compounds are compatible or the correct method of disposal.)he following persons are responsible for the disposal of specialist wastes/ %. Risks 4"entifie" in the Work Activity. (%ist all C!"" associated risks and others such as/ , flammability, naked flames, manual handling etc. below, together with the protecti&e measures re+uired). #0!1 P#(2(-)$)02( M($!3#(!!odium hydro'ide solution/ corrosi&e Wear lab coats, glo&es and use eye protection. Prepare reagent in fume cupboard.$tomic absorption spectrophotometer/ naked flame and compressed gases0nstrument should be set up by a technician or other competent member of staff and operated only under super&ision."ydrochloric acid/ corrosi&e Wear lab coats, glo&es and use eye protection. Prepare reagent in fume cupboard.Laboratory Risk Assessment Form Ver. 1.0"age , of 5&. 0as a +ritten Emergency 5roce",re been #re#are"6 4es-o 0f so it should be attached to this form or incorporated into the Written Working Procedure (section 5). )his should include procedures for the emergency shutdown of e+uipment, dealing with spillages of large amounts of chemicals (especially corrosi&es and &olatiles) or the mi'ing of incompatible chemicals and specialist first aid treatment (e.g. for phenol burns).S#illages of aci" sho,l" be ne,tralise" imme"iately +ith so"i,m carbonate #o+"eran" the area thoro,ghly +ashe" ,# +ith +ater.S#lashes of aci" on the skin sho,l" be irrigate" imme"iately +ith #lenty col" +ater.S#lashes of aci" to the eye sho,l" imme"iately be irrigate" thoro,ghly +ith +ater from an eye irrigation #oint.Seek me"ical attention for any aci" b,rns.4nstr,ctions for emergency sh,t"o+n of the AAS are #rovi"e" besi"e the instr,ment. 5ress the re" b,tton to initiate safe sh,t"o+n an" t,rn off gases at cylin"er +hen the flame is e!ting,ishe".10. 4s S#ecial Training or S,#ervision Re7,ire"64es-o )he super&isor will appro&e straightforward work in progress)he super&isor will specifically appro&e the scheme of work in section 5)he super&isor will pro&ide super&ision personally to control the work6urther information (if yes selected)/AAS m,st be o#erate" by a laboratory technician or other com#etent member of staff11. 4f this #roce",re is restricte" to name" in"ivi",als #lease name them belo+.12. Restrictions on ho,rs of +ork..an any of these #roce",res be carrie" on 8o,t of ho,rs9 or by lone +orkers6

4(! -%one working6irst aid pro&ision essentialut of hours (7 pm 8 9.:; am) permitted$re there any additional precautions, which need to be taken for 1!. When sho,l" this assessment an" the control meas,res ne!t be revie+e"6 ?ate/ @anuary 5;;A)(.Accre"itation.!ignature of $ssessor/-ame/ r 4an :rieve?ate/ :B @anuary 5;;7Laboratory Risk Assessment Form Ver. 1.0"age 8 of 5

Laboratory Risk Assessment Form Ver. 1.0"age 4 of 5);. User Training Recor"Trainee-0 ha&e read and fully understood the risk assessment prepared for the abo&e work acti&ity. 0 understand the risks created and agree to use the control measures specified. 0 ha&e recei&ed the training necessary to carry out the work.S,#ervisor-0 am satisfied that this person has been trained and is capable of carrying out the work described.)rainee signature )rainee name (printed) !uper&isor signature ?ateLaboratory Risk Assessment Form Ver. 1.0"age 5 of 5