Puri Ls Labormtory Sate Introduction Ope of the objectives of this laboratory session will be to introduce standard safe laboratory nyetices and to raise your awareness OF He hazards and potential risks present when working. jn a premical enviionnieni, Lé, a workplace where convolted products are used, Controlled products Jnclude laboratory chemicals, solvents, fitels, food additives, chemicals used in manufacturing. Cleaners, and pharmaceutical products, Clearly, chemical environments are not limited to tnivensity chemistry laboratories; engineers, medical professionals, technicians, scientific hesearchers, product desipners, mechanies, and numerous others regularly work in a chemical vavironment, Chemicals and procedures have an inherent level of hazard that poses an associated Sekof injury. While hazards cannot be changed, risk ean be reduced through the employment of ote laboratory prictices, Good planning and safety-consciousness reduces the likelihood of svoidents, Nevertheless, accidents do happen, so it is important that you know how to respond to them appropriately and expediently, jon your ‘TA will guide you through a number of safety-related ” During this laboratory ses exercises, including: an introduction and demonstration of safely equipment an ingoduction to Material Safety Data Sheets (MSDS's) and the labeling of chemical waste Wve the lab due to unsafe laboratory re asked to I cenario where workers Wel «case study practices, You will be assigned to a Safely Team, with whom you will Team will be responsible for implementing and monitoring lab safety practices for your entire lab room during one future lab session; for more details, see page 9 of this manual. This sponsibility will require some group planning ahead of your assigned session, s0 you should exchange contact information with your team members, Sinee the laboratory program is a professional environment, and to protect your privacy, we strongly suggest that you use es for online correspondence. s. Your Safety conduct these exerci: University of Manitoba e-mail add Procedure Your TA will guide you through a number of laboratory safety exercises. In your Data Sheets you will need to: # Jabel a safety equipment map # list potential hazards that you observ «outline safety information for a chemical used in the abandoned experiment fill out a hazardous waste disposal tag for this chemical nthe abandoned experiment (case study)and $485 in Olmsted, John Il; Williams, Greg; Burk, Robert C Canadian eds.; John Wiley and Sons Ltd: Mississauga, Canada, 2010, 1y of energy and heat changes associated with chemical reactions snd sons such as phase changes. The measurement of heat changes is carried ch is usually an enclosed compartment in which the change in heat you use a simple insulated calorimeter. If we consider the calorimeter and its contents to be the system, then the surroundings is of the calorimeter. The calorimeter that you will use is open to the atmosphere, very experiments will be conducted under constant pressure conditions. In this case, the Theat that will be measured are emthalpy changes. If we assume that the calorimeter is 'y insulated such that there is no exchange of heat with the surroundings, then the inside the system, AHastem, is zero: AHgaxx = 0 a) vide the system into components that can exchange heat energy. The calorimeter (ghoninum cup and outside jacket, Styrofoam middle, stirer, lid, thermometer) can exchange hest scab the contents. If the volume of contents inside the calorimeter is similar for each calorimetry experiment, we can assume that the amount of heat exchanged with the calorimeter, dea is proportional to the change in temperature, AT.a it experiences: gas = Cos AT @ schere the proportionality constant Cay is the heat capacity of the empty calorimeter. Changes in temperature are always measured as: AT = Teva ~ Tosti @ In this experiment the calorimeter is calibrated using a reaction whose enthalpy is known: the reaction of calcium metal with acetic acid solution. Acetic acid is a weak acid in aqueous solution, which is in equilibrium with acetate and hydronium ions: CHsCOOH (ag) + H20 () == CH3COO (ag) + HO* (aq) 4) Calcium metal reacts with hydronium to give calcium cations and hydrogen gas: Ca(s) + 2HsO" (aq) > Ca? (ag) + H2(g) + 2120 (0) eo [As hydronium cations are consumed, by the reaction in (5), the equilibrium in (4) shitts to the fight to produce more hydronium cations. The overall process and its enthalpy changes Mons is Ca(s) + 2 CHsCOOH (aq) — Ca®* (ay) + 2 CH3COO (ag) + He (8) (6) AHyn = 424.8 koIf calcium metal is the limiting reagent, then the heat released by the reaction, gy is fea oO imol Ca where cy is the moles of calcium metal. This heat is absorbed by the calorimeter and the final solution that it contains. Assuming no heat lost to the surroundings: gra = AHexa * MHoywen = geat + Guision Joa = OD “ The heat absorbed by the solution. quoi, depends on its mass, msaiaion and its specitic heat, ‘Coouaion- For the reaction of Ca metal in acetic acid, the specific heat remains fairly constant throughout the reaction with Coisise = 4.10 ¢ °C" [1]. Substituting this and equations 2 and 7 into equation 8 we get: Cot MTeai + Crotation Mscition MTeat + AHoa x —"S+_ = OKI o) Once the calorimeter is calibrated it can be used to measure other changes in energy. Heat of hydration of sodium acetate Sodium acetate is a basic ionic salt that can exist in both its anhydrous form (NaCHsCOO) and as a trihydrate salt (NaCH;COO-3H20). Both forms of solid sodium acetate are highly soluble in water. The dissolution processes for the anhydrous salt can be represented by the following chemical equation: NaCHsCOO (s) — Na* (ag) + CHsCOO™ (aq) AH, (10) The enthalpy change of dissolution, Ah, is the net change in the energy of interaction between the relevant species. Within the solid crystal, ionic attractions between the anions and cations dominates, resulting in a lattice energy that needs to be overcome in order to dissolve the salt. Once dissolved, ion-dipole interactions between the ions and water molecules dominates. Dispersion, dipolar interactions, and hydrogen bonding between acetate and water molecules are also present. For the trihydrate salt, the dissolution process is different: NaCH3COO:3H20 (s) > Na* (ag) + CHyCOO- (ag) + 3 H20 (I) AH; (11) In the crystal structure of the trihydrate salt, ionic attraction is still a dominant force. However, there are also ion-dipole interactions between the water molecules and the Na’ cation. In the crystal structure, each Na* cation has an octahedral geometry where the Na’ is coordinated to six Oatoms, five from water molecules and one from the acetate anion, Once again, the lattice energy must be overcome to dissolve this salt; once dissolved, the ions interact with water as before, and the water molecules that were part of the crystal become part of the water of the solution. Using Hess’ Law, we can use equations 10 and 11 to determine the enthalpy of hydration of the sodium acetate salt: NaCHsCOO(s) + 3H20(/) + NaCH3COO-3H20 (s) AH: Ai AH2 (12) AH; is the net change in intermolecular interaction in the species on the two sides of chemical equation 12. 28Procedure Calibrati -alorimeter A. Weigh the calorimeter on a top-loading balance that reads to the ni &. Add 100 mL of 5% v/v acetic acid to the calorimeter using a graduated cylinder, and then rest £0.01 g. weigh it. 3. Keep track of the temperature i the calorimeter lid. 4. Weigh by difference a 0.45 + 0.05 g sample of calcium metal in a clean, dry weighing bottle. 5. Lift the calorimeter lid and add the calcium to the calorimeter then quickly replace the lid. Swirl the contents as you keep track of the temperature inside the calorimeter until it stops rising for at least a minute and record this value. 6. Dry all parts of your calorimeter gently with a paper towel. Why? Solution can spill out of the aluminum cup and wet the Styrofoam and the outer metal jacket - make sure you dry these too. 7. Repeat steps 1 ~ 6 a minimum of three times. ide the calorimeter by using a digital thermometer through Dissolution of sodium acetate salts 8. Add 100 mL of distilled water to the calorimeter using a graduated cylinder, and then add the lid. Weigh it and keep track of its temperature as before. 9. Collect a 10.0 + 0.5 g sample anhydrous sodium acetate in a, dry weighing bottle. 10. Lift the calorimeter lid and add the salt to the calorimeter then quickly close the lid. Swirl the contents as you keep track of the temperature inside the calorimeter until it stops rising ot falling for at least a minute and record this value. 11. Reweigh the calorimeter then dispose of its contents down the sink with lots of water. Dry the all parts of the calorimeter with some paper towel as before. 12. Repeat steps 8 — 11, this time with sodium acetate trihydrate. Analysis 1, Determine the heat capacity of the calorimeter, Ceat in J °C ' for all three trials, and calculate the average value. Provide all of these values in your report; provide full calculations only for Trial 1. 2. Determine the enthalpy of dissolution per mole for each of the two sodium acetate salts (anhydrous and trihydrate, AH; and AHp, respectively). The average heat capacity of the final sodium acetate solutions is 3.96 J g! °C"! [1]. Determine the enthalpy of hydration of sodium acetate, AH3. Reference [1] Laliberté, M. J. Chem. Eng. Data 2009, 54, 1725-1760.Discussion A detailed overview of how to write a lab report and a Discussion is provided on pages 1] ~ 18 of this manual. Your discussion should address questions asked in the Introduction and/or Procedure sections. In addition, you should consider the following points when writing your report: jeral_ point # Alldiscussion and answers to questions must be based on your observations, data, and results State specific values when you discuss them. * Ifpossible, predict what effect a source of error will have on the final result. the crror systematic, giving results that are consistently higher (or lower) than expected? Is the error instead random, i.e., does the error causing results to be sometimes higher and example, is sometimes lower than the actual v: ‘¢ When discussing sources of error, stick to what is confirmable and what is recorded in your observations. If you need to speculate, stick to reasonable and logical explanations. Do not discuss factors that have little or no effect on your results. nent ect pe wt What is the accuracy of your measurements and how are they linked to your quantitative values? © You have calibrated your calorimeter. Considering the level of accuracy of this experiment at absorbed by the calorimeter versus the amount of heat absorbed by the In other words, could you have ignored the heat and the amount of hea solution, was calibration necessary’ absorbed by the calorimeter? We assume that there is no heat exchange with the surroundings. How true is this? How would you improve upon the accuracy of your results for this experiment? You measured the enthalpies of dissolution of anhydrous sodium acetate and sodium acetate trihydrate, and the enthalpy of hydration of sodium acetate salt. Indicate whether these es are endothermic or exothermic, and rationalize why by considering the changes in proc intermolecular interactions in these processes.