Every effort has been taken to ensure that these

Chemistry 217Chemical Principles IHome Laboratory Manual 2012/14 Course TeamLab Manual Authors:Editor:Cover Photography and Design:Visual Presentation:Laboratory Manager:Laboratory Kit Manager:Laboratory Research AssistantLaboratory Coordinator:Home Lab Advisors:Course Coordinator:Photography & Illustrations:Lawton Shaw Rob Carmichael ScottMcGavin and Dietmar KennepohlErna DomineyBlaise MacMullin and Ian GrivoisDigital Media Technology UnitElaine Goth-BirkigtNeil SextonCarmen AllenRobert D. CarmichaelMelissa GajweskiJim RobinsonDarinka RisingKlaus ThomsonNyron JaleelLawton ShawBlaise MacMullin Elaine Goth-Birkigt Ian Grivois Neil Sexton Carmen Allen and Robert CarmichaelEvery effort has been taken to ensure that these materials comply with therequirements of copyright clearances and appropriate credits. AthabascaUniversity will attempt to incorporate in future printings any correctionswhich are communicated to it.Athabasca University students are allowed to make a print copy of thismanual from an electronic file.Athabasca University 2012Printed in CanadaSLID#C100312CHEMISTRY 217 ContentsGeneral InformationIntroduction …………………………………………………………………………………………… 3Organization ………………………………………………………………………………………….. 4Home Lab Kit Request …………………………………………………………………………… 6Safety Pledge ……………………………………………………………………………………… 7Receiving and Returning your Chemistry 217 Home Lab Kit ……………….. 8Materials to be Provided by the Student ………………………………………………… 9Evaluation of Students’ Work ………………………………………………………………. 10Writing Laboratory Reports …………………………………………………………………. 11Graphs …………………………………………………………………………………………………. 22Getting Started …………………………………………………………………………………. 23Straight-line Graphs …………………………………………………………………………. 24Checklist …………………………………………………………………………………………… 27Problems ………………………………………………………………………………………….. 28Further Reading ……………………………………………………………………………….. 29Answers to Problems ……………………………………………………………………….. 30Safety ……………………………………………………………………………………………………. 31Safety Rules ……………………………………………………………………………………… 32Some General Advice Regarding Laboratory Work ………………………….. 34Medical Information Form ……………………………………………………………….. 36Chemistry Laboratory Accident Form ………………………………………………. 38WHMIS ……………………………………………………………………………………………… 40Hazard Symbols ……………………………………………………………………………….. 41Common Apparatus …………………………………………………………………………….. 42Checklist of Equipment Contained in Each Student Kit ……………………….. 46Experiments ………………………………………………………………………………………….. 49The Candle Experiment ……………………………………………………………………….. 51Block A ExperimentsExperiment A1: Mass and Volume Measurement …………………………….. 61Experiment A2: The Use of a Spectrophotometer† …………………………….. 79Experiment A3: Acid-Base Titrations ………………………………………………. 107†These labs require formal reports.HOME LAB MANUAL FOR 2012–14 Experiment A4: The Determination of the Universal Gas Constant† … 127Block B ExperimentsExperiment B1: Solutions ………………………………………………………………… 139Experiment B2: The Determination of an Enthalpy ChangeExperiment B2: That Cannot Be Measured Directly …………………………. 155Experiment B3: The Reactions and Identification ofExperiment B3: Some Common Cations …………………………………………. 171Experiment B4: Quantitative Determination of Phosphorus ……………. 179Block C ExperimentProject C: The Stoichiometry of a Reaction† …………………………………….. 191AppendixTable of Reagents ……………………………………………………………………………….. 203Glossary …………………………………………………………………………………………….. 205How to Return Your Home Lab Kit …………………………………………………….. 213Index …………………………………………………………………………………………………… 216†These labs require formal reports.CHEMISTRY 217 AcknowledgementsThe 2012/14 version makes only a few minor corrections to the manual. Inthe previous 2011/12 version of the CHEM217 lab manual incorporates amajor positive change to the home lab kit the SpectroVisspectrophotometer. The lead author wishes to thank Neil Sexton ElaineGoth-Birkigt and Rob Carmichael for their work on the implementation ofthis improvement.The authors’ gratefully acknowledges all the contributions and suggestions forimprovement to the 2003/04 first version of this manual by Christy Tkachuk andRobert Carmichael (Summer 2002). Special thanks to Elaine Goth-Birkigt andRoberta Franchuk for checking all the B1–B4 home-lab experiments (Fall 1995) andagain to Elaine Goth-Birkigt with the help of Neil Sexton and Richie Golonka forthe construction and testing of the simple spectrophotometers (2002). Thanks againto Neil Sexton and Rob Carmichael for their to incorporate the inclusion of the 10mL short burette in 2009. The author also wishes to thank Blaise MacMullin for allhis photography work (Summer 2002). Finally the candle image photos reprintedon page 51 are courtesy of the NASA John H. Glenn Research Center. Thanks arevery warmly extended to Dr. Daniel L. Dietrich of NASA’s John H. Glenn ResearchCenter Cleveland OH for all the additional information he provided about thecandle flames in microgravity.The experiments described in this laboratory manual are mainly variations ofsimilar experiments that may be found described in the laboratory manuals of otheruniversities or in commercially produced lab texts. Each experiment has beenmodified and rewritten keeping the particular needs of Athabasca Universitystudents in mind. The author acknowledges the following sources:Practical Inorganic Chemistry Manual University of Essex 1965. (Exp A1)Rayner-Canham Geoff. Foundations of Chemistry in the Laboratory. Reading MA:Addison-Wesley 1983. (Exp. A1)Frantsi Susan A. Chemistry Experiments: A Student Manual for Off Campus Use.Indianapolis IN: IUPUI. (Exp. B1 and Safety Pledge)Solomon Sally Lee Alan and Bates Donald. J. Chem. Ed. 70(5) 411. (Exp. B4)Robinson E. A. Ronald J. Gillespie Irma Hoogendoorn and John E. Bauman Jr.Laboratory Manual to Accompany Chemistry. Newton MA: Allyn and Bacon 1986. (Exp. B2)Laboratory Manual Chemistry 209 Athabasca University. (Exp. A3)Beran Jo A. Laboratory Manual for Fundamentals of Chemistry. New York: John Wileyand Sons 1981. (Exp. A4)Weiss Gerald S. Robert K. Wismer and Thomas G. Greco. Experiments in GeneralChemistry 2nd ed. New York: MacMillan 1985. (Exp. A1)HOME LAB MANUAL FOR 2012–14 Nelson John H. and Kenneth C. Kemp. Laboratory Experiments for Brown and LeMayChemistry: The Central Science 3rd ed. Englewood Cliffs NJ: Prentice-Hall 1985.(Exp. A2)Laboratory Manual Chemistry 320 Athabasca University. (Exp. A2)CHEMISTRY 217 General InformationGeneral InformationHOME LAB MANUAL FOR 2012–141 2CHEMISTRY 217 General InformationIntroductionAthabasca University is very pleased to offer and welcome you to thehome laboratory component of Chemistry 217. Although the laboratorycomponent of this course will involve a lot of work we hope that you willfind the experience both intellectually stimulating and enjoyable. One ofthe benefits of having an all-home laboratory component in a course suchas ours is that it gives students the ultimate in flexibility in planning andperforming your experiments.If you were to take a course such as Chemistry 217 in a traditional collegeor university you would probably be expected to attend a three-hourlaboratory session every week for 10–12 weeks. During this time youwould complete 10–12 experiments and would receive somewhere in theorder of 30 hours of laboratory instruction. In our course you will spend30-40 hours of laboratory time spread over a time frame of your choosing and will complete 10 at-home experiments. This includes one introductory“kitchen chemistry” experiment and 9 home lab experiments using thehome-study laboratory kit.Your preparation and organization before beginning your homelaboratory experiments is vital!At this time we would like to bring to your attention several points thatwill enhance your laboratory experience and minimize any potentialproblems.1.Home-study lab work. Before doing any experiments you will berequired to do some “kitchen chemistry” (Candle Experiment) at home and submit a short lab report. This will allow you to sharpen yourobservation and report writing skills without having the pressure ofthe home lab experiments. In addition this is an excellent opportunityfor you to receive feedback from your laboratory tutor before divinginto the bulk of your experimental work.2.Hours of work. Each experiment may take a full evening to complete.3.Home-labs. The home lab kit can be requested from the AthabascaUniversity science lab any day of the week (see page 6). Kits can bereturned by mail (postage prepaid) to the Athabasca University sciencelab.4.Feedback. In many freshman laboratory courses students submit theirlaboratory reports shortly after having completed an experiment andthe reports are returned a few days later before the students attemptthe next experiment. In the Athabasca system this is clearly notpossible. After completing your first home laboratory experiment youwill have to write up the report submit it by mail to your tutor andthen wait for some feedback. We hope that the response can beHOME LAB MANUAL FOR 2012–143 provided before you begin your second home laboratory experiment but if you decide to do your experiments close together or if it takesyou a long time to write your reports this may not be possible.Remember if you have difficulty in writing your laboratory report contactyour tutor. Also remember to keep a duplicate copy of all yourexperimental results—we will suggest a method for doing this in thesection of this manual titled “Writing Laboratory Reports.” Note:Return of lab reports is up to each individual tutor. Your tutor may ormay not return corrected lab reports for security/course integrityreasons. However you will be given feedback by phone or mail.5.Preparation. Before you begin each home lab experiment prepareyourself by reading the entire experiment finding and labelling all theequipment and reagents you will require a view the video clips forthat particular experiment (view the safety/intro clip first) and finallycontact your tutor to find out any “hints for success” in the experiment.Note: As of May 2009 a new ~10 mL ‘short’ burette is being used inExp. A3 and Project C. The video clips for these experiments has notbeen updated yet and still shows the use of the old ‘syringe/glassbead/serological pipette / burette’ apparatus. And as of February2011 the new SpectoVis Plus spectrophotometer replaces the oldsimple spectrophotometer in Exp. A2. The video clips for ExperimentA2 has not been updated yet and still shows the use of the old homemade apparatus. All Videos are now found in Moodle:http://science.lms.athabascau.ca/mod/book/view.php?id=2504OrganizationThe laboratory component of Chemistry 217 comprises 30-40 hours of homelab experiments and assignments. In the past all this work would becompleted in two day-long sessions in a supervised lab. In the all-home labformat the experiments have been grouped into three “blocks.” Pleaserefer to the contents page of this manual for a list of the experiments thatyou will be doing.Block AThe experiments in Block A are microlab experiments designed to introduceyou to some of the basic techniques used by chemists: the use of burettes andpipettes spectrophotometers gravimetric analysis and volumetric analysis.We hope that you have been exposed to at least some of these techniques inyour previous chemistry courses; however we realize that such exposuremay have occurred several years ago. In addition to providing you with anintroduction to basic laboratory techniques the experiments in Block A aredesigned to reinforce some of the theoretical concepts that you will havestudied in Units #’s of Chemistry 217. Thus for example Experiment A4 is4CHEMISTRY 217 General Informationconcerned with the ideal gas law. Note that Experiment A2 A4 and ProjectC require formal reports.Block BThe experiments in Block B are also designed to reinforce concepts learnedin the course such as enthalpy gravimetry and colligative properties. Allthat is required for a lab report is to fill out the observation sheet at the endof each experiment.Block CThe instructions for completing the Project in Block C are intentionallymuch vaguer than those given for the experiments in Blocks A and B. Theexperiment requires students to use some of the techniques that haveencountered earlier in the course. Students are expected to have deducedtheir own detailed procedure for this experiment. Your tutor will ask thatwritten procedures for the Project in Block C be submitted before you beginthe final experiment. Note that this Project is to be written up as a formalreport.All students will complete a short online quiz at the end of Block C. The labquiz can be found in Moodle and is open book. This quiz will coverlaboratory safety techniques and procedures and the basic principles uponwhich some of the experiments are based. If necessary the quiz can becompleted by telephone.As you can see a total of 10 home-study experiments are described andothers may be added as we find it necessary to modify the course. You willbe required to complete a short report for A1 and A3 experiments. Formalreports are required for Experiments A2 A4 and C. Finally the candleexperiment and each of the microlab experiments in Block B require that youfill out the accompanying report form. Thus each student will complete atotal of 10 experiments.We suggest that you work through each block of experiments in the orderthey are presented.HOME LAB MANUAL FOR 2012–145 Home Lab Kit RequestIf you are unsure about any of the following instructions on how to receiveyour Chemistry 217 home lab kit please contact the Science Lab Coordinatorat:1-800-788-9041 ext. 6729 (North America) 780-675-6729 (Athabasca) or780-481-3704 (Edmonton) orby e-mail at [email protected] that in 2012 there is a $40.00 Chemistry 217 lab fee included in yourcourse tuition that helps to pay for the shipping of the kit.If you think you might be eligible for a lab exemption please contact theLab Coordinator or consult the Web page:http://science.athabascau.ca/Labs/exemptions/chemistry.phpThe following procedure should be observed in obtaining a Chemistry 217all-home lab kit for home study.1.Complete your Safety Pledge (see next page).2.Complete your TME1 and wait for it to be marked.3.Then fill out the online lab kit request form at:http://science.athabascau.ca/Labs/resources/chemistry.phpCHEM 217 Kit Request6CHEMISTRY 217 General InformationSafety Pledge for the Home LaboratoryThis Safety Pledge can also be completed online when making the home labkit request.Safety Rules1.Wear approved eye protection at all times doing your lab activities.2.Confine long hair when doing your lab activities.3.Perform no unauthorized experiments.4.Select a safe site for lab activities in your home that is well ventilated and protected from spills children and pets.5.Keep all chemicals and equipment out of the reach of children andpets.6.If possible keep all unauthorized people out of your selected site whenchemicals are in use to avoid any unforeseen accidents. If anyone isallowed to observe you or participate in experiments follow all of theproper safety rules.7.In case of a chemical spill clean up thoroughly with paper towels anddispose of chemicals out of the reach of children and pets.8.If chemical spills occur on people or clothing rinse thoroughly withlots of running water and seek medical attention if necessary.9.Have no food or drink in the lab area. Be sure to thoroughly clean uplab site and all utensils used after working on labs.I have read the above rules and will observe them at all times during mychemistry course._________________________________Print name_____________________________Student ID No._________________________________Signature_____________________________DateHOME LAB MANUAL FOR 2012–147 Receiving and Returning your Home LabKitYour CHEM217 Home Lab Kit is shipped to you via courier (groundtransportation). Typically you will receive your kit 2-3 weeks after you makeyour lab kit request.1.After you receive your kit ensure that all the materials are included inthe kit (a check-in list of materials will be provided). Contact the ScienceLab if any replacements are required at 1-800-788-9041 ext. 6277.2.After completing the experiments at home return the kit to the ScienceLab at Athabasca University. It would be wise to insure the kit for atleast $800.00.Your Chemistry 217 home lab kit may be returned to location 1 below viaprepaid ground courier. Please indicate on the waybill you are returning‘Educational Materials’. For students living in Edmonton or Calgary the kitcan also be dropped off at locations 2-4 listed below:1.AU in Athabasca; AU Science Lab Athabasca University 1 UniversityDrive Athabasca AB T9S 3A3. (Use Prepaid Waybill)2.AU-Edmonton Learning Centre; 12th floor 10030-107 St. N. Tower Edmonton AB T5J 3E4. (drop off location only)3.AU-Calgary Learning Centre; 1040-7th Ave. SW Calgary AB T2P 3G9.(drop off location only)-location will change in 20134.NAIT; only when AU labs are in progress—Check lab schedule 11762 – 106 St. Rm G-207. (drop off location only)Note: The contents of the home lab kit may be changed from time to time or mayvary from one location to another. Your tutor will advise you if any additionalitems should be included or if any items should be deleted from the list.Once back at Athabasca University the lab manager or technician willcheck the kit over for damage.*If you are unsure about any of the following instructions on how to receiveyour Chemistry 217 home lab kit please contact Mr. Neil Sexton the ScienceLab Kit Manager at:1-800-788-9041 ext. 6277 (North America) 780-675-6277 (Athabasca) orby e-mail at [email protected].* You will not be charged for general disposable items. However you will be charged forreplacing any broken or lost non-disposable items.8CHEMISTRY 217 General InformationMaterials to Be Provided by the StudentWhen working on your Chemistry 217 laboratory experiments each studentmust provide himself or herself with the following items:a lab coatan electronic calculatora lab notebooka pen a pencil and a rulera supply of metric graph paper (i.e. 1 mm 1 mm squares).Notes:1.Lab coats can usually be purchased at college or university bookstores army surplus stores or similar establishments. In case of difficulty see“Uniforms—Retail” in the “yellow pages” of your telephone directory.2.A lab notebook should be bound. The preferred size is approximately23 cm 29 cm.Some other items need to be supplied for specific experiments.HOME LAB MANUAL FOR 2012–149 Evaluation of Students’ WorkAll students will work individually. Pairing up and the pooling of data solutions etc. is not permitted unless the laboratory tutor or professorspecifically asks you to do so. Note that the penalties for plagiarizinglaboratory reports are identical to those incurred for other types ofplagiarism. You must attain an average of 60% for laboratory work in orderto pass the course. The grade for laboratory work is determined as follows:Candle ExperimentShort Report5%Block AExperiment A1Experiment A2Experiment A3Experiment A4Short ReportFormal ReportShort ReportFormal Report5 %5 %Block BExperiment B1Experiment B2Experiment B3Experiment B4Report SheetReport SheetReport SheetReport Sheet5%5%5%5%Block CProject CLab Quiz (online)Total10Formal Report20 0%CHEMISTRY 217 General InformationWriting Laboratory ReportsIn Chemistry 217 you will be expected to produce two distinctly differenttypes of laboratory report: “short reports” and “formal reports.” Somehints designed to assist you in writing each type of report are given below.Note: Good laboratory report writing begins with preparing your labnotebook before the experiment taking thorough lab notes and writingdown your observations as they happen.Short ReportIn a short report we do not require that you provide a detailed descriptionof how the experiment was carried out (see procedure instructions below) or give a detailed discussion of the results obtained. In general thefollowing format must be used.1.Title and DateExperiment title and date performed as well as your name andID number.2.Purpose of Experiment (note there is no introduction or theory sectionrequired)Clearly state the what scientific principle is being tested determined orverified. Do not rewrite what is in the lab manual. Note: There may bemore than one major objective as well as a few minor objectives. This isa good place to write out the relevant chemical reactions/equations.Example: To determine the purity of a given solution of iron (II) sulfateheptahydrate by titration with a standard solution of sodium dichromate. Aminor objective is to learn how to properly clean calibrate and operate a buret.3.ProcedureIn the short report reference the appropriate pages in your lab manual noting only any changes or modifications to the procedure.Example: The experiment was carried out as described in Experiment X3 ofthe Chemistry 217 Laboratory Manual pp. _____ except that ammoniumiron(II) sulfate hexahydrate was used instead of iron(II) sulfate heptahydrate.4.ObservationsExample: When the sodium hydroxide/sodium sulfite mixture was added tothe potassium permanganate solution the solution initially turned green andthen a brown precipitate of manganese(IV) oxide was produced.HOME LAB MANUAL FOR 2012–1411 5.ResultsIn general the instructions for each experiment include a suggestedformat for presenting your results. The numerical results should belisted in the order they were obtained and are best placed into a neat carefully labelled table. Use more than one table if necessary; i.e. donot mix unrelated data sets.6.CalculationsAll calculations should be presented clearly (i.e. titled answerunderlined) and should be carried out using the appropriate number ofsignificant figures. By clearly setting out your results and calculationsyou make it easier for your instructor to grade your report. Any erroranalysis and/or discussion can be included at this point.7.Answers to QuestionsDon’t forget that the questions pertaining to the experiments aresometimes provided separately. Hint: Always rewrite the question onthe lab report page and provide your answer below. Show all yourwork as part marks are given.8.ConclusionYou would usually include a sentence or short paragraph thatsummarizes your…