Teaching Tips for TAs

General

CH1010

CH1020

CH1030

CH1040

General

Laboratory Organization. A logical and complete organizational system is essential to the smooth, efficient functioning of the general chemistry laboratories. GH109 and 110, the general chemistry laboratories, are organized according to the following guidelines:

PLEASE LEARN THE ORGANIZATIONAL SYSTEM AND EXERT THE EFFORT REQUIRED TO MAINTAIN THE CLEANLINESS AND THE ORGANIZATION OF THE LABORATORIES. THIS IS YOUR RESPONSIBILITY!

Conservation of Supplies. Items normally considered disposable are recycled in the general chemistry lab. These items include

These items must be washed and glass items must be oven dried following use, then returned to their appropriate storage locations.

Cleaning Glassware. All glassware to be used by students in experiments must be CLEAN. Ideally, each section of students will thoroughly clean the glassware that they have used and place it in the drying oven, so that it will be ready for a subsequent section. In practice, however, students will avoid cleaning glassware if they can get away with it. It is each student's responsibility to properly clean all glassware that s/he uses. However, IT IS YOUR RESPONSIBILITY TO MAKE SURE THAT THE STUDENTS DO THIS. If the students do not clean it, then the responsibility falls to you. A faculty member finding dirty glassware left over from a lab section will seek out the responsible TA to perform the clean up.

Cleaning protocol:
  1. Glassware that has been used to transfer or contain substances dissolved in water may be cleaned as follows:
    • Rinse thoroughly with tap water
    • Remove excess water, then place in the drying oven
  2. Glassware that has been used to transfer or contain organic solvents or solutions may be cleaned as follows:
    • If necessary, rinse with acetone to remove water-insoluble material
    • Rinse thoroughly with tap water
    • Remove excess water, then place in the drying oven
  3. Extremely dirty or contaminated glassware may be cleaned as follows:
    • Place in a bath of Alconox solution overnight, making sure all dirty surfaces are contacted by the solution.
    • Rinse thoroughly with tap water
    • Remove excess water, then place in the drying oven
  4. Glassware that does not respond to Alconox solution may be cleaned as follows:
    • Rinse the glassware with tap water
    • Pour a small volume of concentrated nitric acid into the glass vessel, or submerge the item in concentrated nitric acid; Swirl to clean. BE CAREFUL!
    • Dilute the used nitric acid by slowly pouring it into an equal volume of water. Flush down the drain.
    • Rinse the glassware thoroughly with tap water
    • Remove excess water, then place in the drying oven

Hazardous Waste Collection and Disposal. It is not too much of an exaggeration to say that virtually everything except distilled water is considered to be hazardous waste, and must be handled and disposed of according to EPA (Environmental Protection Agency) guidelines. Hazardous waste disposal is overseen by Mr. David Messier (email: dmessier@wpi.edu), who supplies labels for hazardous waste containers and picks up full containers by appointment. With few exceptions, reagents and solvents used by students must be collected in appropriate containers and disposed of via Dave Messier.

A few substances can still be disposed of in the sink drains, accompanied by a substantial water flush. These include

All other materials must be collected in bottles with official hazardous waste labels. Labels must be properly filled out with the names and weight percentages of the component materials, and toxicity, corrosive ability, potential flammability, and potential reactivity must be indicated. OMISSION OF ANY OF THIS INFORMATION IS A VIOLATION OF EPA POLICY.

Three categories of waste will commonly occur in the general chemistry labs:

  1. Non-halogenated organic solvents. The halogens are the elements, fluorine, chlorine, bromine, and iodine. Organic liquids NOT containing any of these elements are called non-halogenated organic solvents. They include but are not limited to
    • acetone
    • ethanol
    • methanol
    • isopropanol
    • benzene
    • toluene
    • tetrahydrofuran
    • acetonitrile
    • glacial acetic acid
  2. Halogenated organic solvents. These are organic liquids that contain one or more of the elements fluorine, chlorine, bromine, and iodine in their chemical structures. They include but are not limited to
    • chloroform
    • dichloromethane
    • carbon tetrachloride
    • methyl iodide
    • tetrachloroethane
    • dichlorethane
    • freons
  3. "Heavy Metals". These include the transition metals and the heavier elements of groups 13, 14, and 15. Common "heavy" metals, which usually occur in cationic form, are
    • aluminum
    • gallium
    • indium
    • thallium (very poisonous)
    • tin
    • lead (very poisonous)
    • chromium (carcinogen in some forms)
    • manganese
    • iron
    • cobalt
    • nickel
    • copper
    • zinc
    • cadmium (very poisonous)
    • mercury (very poisonous)
    • uranium

When any of these three categories of substance is to be used in a general chemistry experiment, THERE MUST BE PROPERLY LABELLED AND SIZED WASTE CONTAINERS AVAILABLE IN ALL HOODS IN GH109/110. Again, it is your responsibility to inform students of the need to properly dispose of these substances, to show them where and how to do it, and to make sure they do it.

Safety Matters

The following safety matters must be vigorously and strongly addressed:

  1. Safety goggles/glasses. TAs and faculty are expected to strongly enforce the following safety goggles/glasses requirement: All faculty, TAs, and students must wear ANSI-approved safety goggles or glasses over the eyes AT ALL TIMES in the laboratory. An individual will be allowed two warnings. On the third offense, the individual must leave the laboratory. THIS IS THE RESPONSIBILITY OF THE TA.
  2. Sitting on lab benches and tables. STUDENTS ARE NOT ALLOWED TO SIT ON LABORATORY BENCHES AND TABLES. Please prevent students from doing so at all times. Again, allow two warnings. The third offense by an individual means s/he must leave the lab. THIS IS THE RESPONSIBILITY OF THE TA.
  3. Proper clothing. Student must wear appropriate clothing to the laboratory. Sandals, shorts, and skimpy tops are not allowed. Long pants, reasonably heavy shoes, and T-shirts, sweatshirts, or long sleeved flannel shirts are good.
  4. Food and Drink. Students are not allowed to bring food or drink into the laboratory under any circumstances. Neither are you!

Weekly TA Laboratory Meetings. It is our policy that all general chemistry TAs should carry out each experiment in advance of the week in which the experiment is to run. This serves several purposes.

  1. It gives the TA some experience with the experiment.
    • What happens?
    • What are potential problems?
    • What are the expected results?
    • What are the difficult aspects?
    • What questions are students likely to ask?
    • How should you respond to them?
    • What should you discuss in your prelab briefing?

    Doing the experiment in advance makes you more of an expert, and better able to teach the students about the experiment. It enables you to learn lab techniques that you may not have experienced, and therefore are not in a position to teach.

  2. It tests the experiment, reveals the bugs, and gives us time to fix them before the experiment runs in student hands. This enables a better experience for everyone.
  3. It gives you, chemists, an opportunity to get into the lab and do what chemists do.

We expect you to take the lab run-throughs seriously; to come on time, to follow the rules (wear your safety glasses), to focus on the experiment at hand, to carry it out to the best of your ability, to pinpoint problems, to offer solutions, and generally to contribute to making the lab program one of high quality. To competently teach the lab, you must have as thorough an understanding of each experiment as your are capable of achieving.

Lab Protocol

Please print a fresh copy of the experiment in the AM before you meet your section so that you are up-to-date on any changes.

Please arrive at least 30 minutes before your lab is to begin, so that you can make sure that all required materials are available, turn on instruments if necessary, and prepare the blackboard if necessary.

When you arrive in lab, please go through a mental checklist to make sure that everything is ready to go for the experiment. Ask yourself the following questions:

  1. Are all of the lights on?
  2. Is the door unlocked so students can get in?
  3. Are there 16 Labkits available?
  4. Are the necessary supplies available in your lab room? This would include reagents for the experiment, and glassware or hardware. The following items are frequently (though not always) needed:
    • 2-mL graduated pipets
    • 5-mL graduated pipets
    • Extra syringe pipet pumps
    • thermometers
  5. Are the distilled water and acetone wash bottles full?
  6. Are appropriate labelled waste bottles available in the hoods?
  7. If instruments are required, are they turned on, warmed up, and ready to go?
  8. Is your techniques demonstration set up and ready to go?

    Getting everything together and ready prior to lab is your responsibility. Scurrying around for stuff that you forgot during the lab is unprofessional--please don't do it.

    Please collect the Preparation Questions (prelab) from students as they enter the lab. Students should not work on these during the laboratory.

    Please circulate during lab and query students about their activities.

    Please use the full 3 hours of the laboratory period. A pair of students that

    • completes all experimental work
    • completes the notebook writeup, including answers to all questions

    within the 3-hour lab period may leave when finished. ALL OTHER STUDENTS MUST REMAIN FOR THE FULL 3 HOURS. Those students for whom the 3-hour period is not enough to complete the notebook writeup may turn in their notebooks before 4 PM on the following day. Students have paid for a 3-hour lab period. We owe that time to them, and they owe it to us!

    Please be sure that you understand how an aspirator trap functions. The proper way to close off the atmosphere vent is to fold the vent tube over, then clamp it with a screw clamp. The aspirator trap should be set up as follows: the hose connected to the long glass tube going thru the rubber stopper should be connected to the aspirator sidearm of the faucet. A short piece of tygon tubing should be placed on the short glass tube going thru the rubber stopper; this is the atmosphere vent. The hose attached to the sidearm of the test tube should be connected to the student apparatus requiring suction.

    As students finish the experiment,

    • Make sure they clean all glassware
    • Make sure they clean their lab bench area
    • Make sure the balances are clean--if they are not, designate 2 students to clean them
    • Collect any glassware or hardware used during the experiment and return it to its proper storage location.
    • Make sure hazardous waste collection bottles are CAPPED.
    • Make sure all gas and water taps are turned OFF.
    • Make sure all instruments are OFF.

    Some important DON'TS:

    1. Don't remove YOUR safety glasses in the lab. If you do it, students will certainly do it.
    2. Don't sit down in the lab. UNLESS ALL CAN SIT, NO ONE SHOULD SIT.
    3. Don't leave the lab during the period unless you have a very good reason. If you must leave, inform the responsible faculty member. Under no circumstances are you to leave students alone in the lab.

    In each lab period, we will teach the students via demonstration at least one basic laboratory technique. Please learn each technique correctly, practice it, and add it to your laboratory repertoire.

    Initial Laboratory Meeting

    The first laboratory meeting in CH1010 must be used to get the new freshman student off on the right foot. It serves a dual purpose. First, students must be oriented to the laboratory. Second, they must perform the first experiment. The orientation phase, which will usually be handled by the responsible faculty member, should take about 1 hour. Following orientation, 2 hours will remain in which the students can perform the first experiment.

    Orientation. Included in the orientation phase of the first meeting should be

    • Introductions of personnel (faculty, TA)
    • Safety matters
      • Safety Goggles/Glasses policy
      • Book bag/backpack storage
      • Fire extinguishers
      • Eyewash stations
      • Shower
      • Regulations re. contact lenses; food/drink; clothing; hair
    • Hazardous Waste Disposal--location of waste bottles, procedures for handling
    • Lab Organization
    • Glassware recycling policy
    • Glassware cleaning policy and procedures (demonstrate how to clean Pasteur pipets, graduated pipets, and vials); location of drying oven; removing hot items from drying oven.
    • Location and use of analytical balances
    • Proper use of a Pasteur pipet (demonstrate)

    Experiment. Following the orientation, the faculty member or TA should give a prelab briefing on the first experiment. The students should then perform the experiment.

    Molecularity: Fundamental Properties

    Setting Up for the Lab

    Locate the materials for the experiment, which should be stored in a cabinet in GH110. They include

    • pycnometers--numbers on bulb and capillary stopper must be matched.
    • metal samples

    Make sure a table showing the density of water as a function of temperature is posted in the lab.

    Turn on analytical balances.

    Prelab Briefing

    In your prelab briefing, you should deal with the following things:

    • Demonstrate important techniques:
      establishing a clean work area
      using a Pasteur pipet
      filling the pycnometer
      transporting the pycnometer
      using the aspirator trap
      cleaning/drying the pycnometer
      using the analytical balance
    • Discuss any changes to the written procedure
    • Tell students exactly what they are supposed to do: duplicate determinations of pyc volume, duplicate determinations of the density of one metal sample.

    You are not expected to discuss background theory at all in your prelab briefing.

    Running the Lab

    Students should work in groups of 2. Assign each group a sample of metal for which they are to determine the density.

    Circulate while students work. Question them about what they are doing and why.

    Make sure students place used Pasteur pipets in the drying oven before they leave. Collect all pycnometers, which should be emptied of water and metal sample.

    Make sure the balances and balance area are clean before leaving lab.

    Molecularity: Quanta

    Setting Up for the Lab

    Locate the materials for the experiment, which should be stored in a cabinet in GH110. They include

    • Light tubes (H2, He, Ar, Ne, Hg)
    • Power supplies for light tubes
    • Spectroscopes
    • Nichrome wires
    • Cobalt viewing glass
    • Cation solutions for flame tests

    Prelab Briefing

    You are not expected to discuss background theory in your briefing.

    Be sure to:

    1. Demonstrate the proper technique for lighting a bunsen burner. Instruct students to hold extinguisehd matches under cold water, then discard in the waste baskets--do not leave lying on lab benches. Caution students to turn off the gas completely when finished with a burner.
    2. Demonstrate proper procedure for doing a flame test.
    3. Demonstrate and explain how to use a spectroscope properly. clearly explain how to read the scale.
    4. In your prelab briefing, please do NOT tell students what they are expected to see in the flame tests and spectroscopes. The idea is for them to tell us what they see, in written words.

    Running the Lab

    1. Students must wear safety goggles/glasses at all times except when looking thru spectroscopes.
    2. To minimize stray light entering the spectroscopes, close all window shades except one, which should be an end one. Leave on one bank of fluorescent lights, preferably the one nearest the windows. A semidark room will also improve flame test visibility.
    3. The flame test for a particular ion should be repeated 3 times to test for reproducible behavior.
    4. Students should make observations of the following aspects of the flame tests:

      • color
      • duration of color (how long does the color persist?)
      • changes in intensity of color (does it dim gradually, does it brighten over time?)
      • changes in color
      • does the color appear immediately when the wire enters the flame, or is there a lag time?

      There may be other salient observations as well.

    5. Students should look at 4 light tubes with the spectroscopes (hydrogen, helium, neon or argon, and mercury).
    6. Please ask students to complete the experiment and hand in the notebook before leaving lab. They do not need an extra day to finish the writeup.

    Reactivity: The Copper Cycle

    Setting up for the lab.

    Locate the materials for the experiment which are stored in a cabinet in GH110. They include

    • Copper metal, in the form of pre-1981 pennies
    • Saturated aqueous sodium hydrogen carbonate (NaHCO3)
    • Filter paper, cut to fit the Labkit Hirsch funnels*
    • Concentrated HNO3 and H2SO4

    In each hood, set up

    • A bottle of conc HNO3 (bottle cap must NOT be lined with cardboard)
    • A bottle of conc H2SO4 (bottle cap must NOT be lined with cardboard)
    • A bottle of acetone
    • Heavy metal waste bottle
    • Acetone waste bottle
    Prelab briefing. You discuss and demonstrate techniques for
    • Measuring out conc HNO3 using a Pasteur pipet. Pasteur pipets deliver 30-40 d/mL.
    • Suction filtration. Show students
      • how to set up the Hirsch funnel, filtration collar, and sidearm test tube
      • how to connect the sidearm test tube to the aspirator.
      • How to wet and seat the filter paper
      • How to apply suction for filtration, and release it when filtration is finished
    • Go over the products of the first reaction with them, and provide them a balanced equation. Encourage them to speculate on the identities of products in subsequent steps. Give them hints, but make them struggle with the identification problem. Please do not hand them the answers on a silver platter.
    • In step 3, please have them add 7 mL of water to the solid first, then add 0.5 mL of conc H2SO4 (acid to water, not water to acid).
    • In part 4, please tell students to suction off all water before putting acetone into the funnel.

    Running the Lab

    Students should work in pairs.

    Students will need guidance with filtration procedures. Help them on an individual basis.

    Forces and Bonding: Conductivity

    Setting up for the lab

    1) Please locate in the GH110 cabinet 330-ohm, 0.25-watt resistors (at least 200)
    LEDs (at least 200)
    9-V battery clips (at least 200)
    4 x 10-hole perfboard pieces (at least 200)
    9-V batteries (at least 16)
    Dropper bottles containing solvents, 2 per solvent
    Solvents: acetone
    ethanol
    methanol
    dichloromethane
    dimethylsulfoxide
    dimethylformamide
    Vials or dropper bottles containing pure substances, 2 per substance. A complete list of substances is available.

    2) Preparing supplies of substances

    a) Duplicate sets of reagents

    Arrange solvent and pure substances at a convenient location in each lab. An alphabetical arrangement of substances is preferred.

    3) Set up waste bottles in the hood for

    heavy metals (transition metals, Pb, Sn)
    chlorinated organic solvents (CH2Cl2)
    non-chlorinated organic solvents

    Pre-lab Briefing

    You are not expected to discuss background theory.

    You should cover the following topics:
    1. A simple series circuit
    2. Preparation of a desired volume of a solution of specified molarity
      • by weighing
      • by dilution of a concentrated stock solution
    3. Making small stirring rods from melting point capillaries--DEMONSTRATE!
    4. Tell students that you will be giving them a sheet showing 10 substances, 2 solvents, and 3 commercial products, and that they are to perform the following conductivity tests:
      • Each of the 2 solvents
      • Each substance pure--10 tests in all.
      • Each substance as a 0.1 M solution in each solvent--20 tests in all.
      • Each of 3 household substances. Solids should be tested as is and also in aqueous solution. Liquids should be tested as is. This will involve between 3 and 6 tests.
    5. Show students how to organize their tests in the 12-hole well plate:

      Row 1,Hole 1
      Solvent 1
      Row 1,Hole 2
      Solvent 2
      Row 1,Hole 3
      Solvent 3
      Row 2,Hole 1
      Substance 1
      Row 2,Hole 2
      Substance 1
      Row 2,Hole 3
      Substance 1
      Row 3,Hole 1
      Substance 2
      Row 3,Hole 2
      Substance 2
      Row 3,Hole 3
      Substance 2
      Row 4,Hole 1
      Substance 3
      Row 4,Hole 2
      Substance 3
      Row 4,Hole 3
      Substance 3

      To save time, recommend that students calculate the mass of, say, substance 1 required to prepare 1 mL of a 0.1 M solution; to weigh out 3 x this mass; and to partition this total equally among the 3 well-plate depressions for the substance.

    6. Waste disposal priorities (see below under Running the Lab). Students are not to simply empty their well plates into the sink! They must dispose of each 1-mL volume of solution according to the priorities below.

    Running the Lab

    1) Assigning solvents and substances to students.

    30 subsets of the master list of substances/solvents are available. Each subset includes water plus 2 other solvents, 10 or 11 pure substances, and 12 household products. Please print these out for distribution to your students.

    Each pair of students in a section should be assigned one of the subsets. Give the subset sheet to the student pair, and instruct them to return it to you filled out before leaving lab. If you have more than a total of 30 student teams in ALL of your sections, you should make copies of some subsets to cover the number of student teams in excess of 30. For example, if in your 3 sections you have a total of 36 student teams, you will need to make copies of 6 of the subsets in order to cover all 36 teams. You should, of course, also keep copies of the subsets for yourselves.

    2) Conducting the experiments. Conductivity tests involving the solvent, dichloromethane, should be carried out in the hood. Other tests, including glacial acetic acid solvent, may be done on the lab bench.

    3) Disposal priorities

    Priority 1: Heavy metal waste--heavy metal waste jar

    Priority 2: Chlorinated organic compounds--chlorinated organics waste bottle (1 L)

    Priority 3: non-chlorinated organic compounds--nonchlorinated organics waste bottle (4 L)

    Priority 4: non-heavy metal inorganics--most can be flushed

    Thus a sample that contains, say, acetone and a heavy metal compound must be placed in the heavy metal waste. A sample that contains dichloromethane and NaCl must be placed in the chlorinated solvent waste, etc.

    TA results

    Molecularity: Covalent Molecules

    Setting Up for the Lab

    Locate the molecular model kits in a locked cabinet in GH109a. Inspect all kits for correct content (inside of lid), make up from spare parts kits if necessary.

    Prelab Briefing

    The purpose of the workshop is to learn something about VSEPR by building models of covalent molecules based on Lewis structures. The models show us what we believe the molecule looks like in 3-D.

    Students should be told to

    1. Get a model kit
    2. Check the contents of the kit
    3. Proceed through the model building exercises. For each molecule or ion, they should
      • Develop an acceptable Lewis structure
      • Build a model of the species
        • For species with lone pairs and single bonds only, ball for central atom should have a number of holes consistent with the number of electron groups around the central atom in the Lewis structure. For species with a double bond, the central atom ball should have one more hole than the number of electron groups (a double bond is counted as 1 electron group, but requires 2 holes).
        • Lone pairs on the central atom(s) should be explicityly represented using short fat gray sticks.
        • Show them how to use the kit to make a double bond
      • Draw a stereochemical structure using the wedge-hash system. You will have to teach them the wedge-hash system.
    4. When finished, again check the kit for contents and turn it in.

    You may have to teach students how to draw Lewis structures. We went thru a systematic approach, which is detailed in Chapter 3 of Concepts of Chemistry. This chapter also discusses VSEPR.

    Running the Lab

    Circulate and help students when they run into trouble. Make sure they build the structures correctly, and address all of the questions.

    Molecularity: Synthesis of Bis(dithiocarbamato)nickel; Stoichiometry of Reaction

    Setting Up for the Lab

    1. Set out the 0.3 M stock solutions of NiCl2.6H2O and Nadtc.3H2O in labelled plastic bottles. At most 100 mL of each solution is required per section. Please label the bottle caps as well as the bottles. li>Set out labelled plastic bottles (label caps as well) in which to collect left over stock solution from the students. This can be used in another section, or evaporated down to recover the starting materials.
    2. Set out a box of 5.75" Pasteur pipets in each lab.
    3. Cut filter paper for the Hirsch funnels.
    4. Set out plastic rulers.
    5. Check aspirator traps for proper set-up and function.
    6. Near each aspirator trap set up a clamp, a ring with wire gauze, and a burner.
    7. Check hood to make sure proper waste receptacles are available. These include heavy metal waste, chlorinated solvent waste, non-chlorinated solvent waste.

      Prelab Briefing

      Present the problem:

      • Using Job's Method, determine the stoichiometry of the precipitation reaction

        NiCl2(aq) + xNadtc(aq) ---> Ni(dtc)x + NaCl
      • Purify and crystallize the product. Characterize it if desired.

      Demonstrate proper pipetting technique. Stress the need for accuracy in pipetting.

      Demonstrate the process of filtration thru a plugged Pasteur pipet

      • Show how to seat the plug using a ramrod
      • Show how to mount the pipet in the aspirator suction tube
      • Show how to transfer the mixture to be filtered to the pipet
      • Show how to collect the filtrate in the aspirator trap for disposal

      Remind students how to carry out a Hirsch funnel filtration.

      Remind them that each pair of students will do two experiments using assigned volumes of NiCl2 and Nadtc stock solutions. They are to record final height data before leaving the lab.

      Caution them about contaminating the stock solutions. Show them how to properly place the bottle caps on the bench when accessing the stock solution bottles.

      Running the Lab

      Circulate, help students master the techniques.

      About halfway thru the experiment, you should obtain a bin of ice for the rextallization part of the expt.

      As students finish their filtrations, collect their Pasteur pipet filters and arrange them according to Ni/dtc ratio. When all filters have been collected, students can measure and record data on the data collection sheet.

      Forces and Bonding: Solids

      Setting Up for the Lab

      Locate the crystal model kits and make sure that there are sufficient balls of each color for each kit. Station the kits in one of the labs, 4 kits per bench.

      Prelab Briefing

      Briefly tell the students that they will be making models to represent the lattices of crystalline solids. They will begin by looking at closest packing and unit cells in metals, and will proceed to ionic solids during the lab. Review the atom counting rules (vertex, edge, face, and body). These have now been put directly in the lab procedure.

      Running the Lab

      Students have trouble interpreting the directions in some places, and unless watched tend to "skip by" some of the steps without seeing what they are supposed to see. It is very important to circulate constantly during this lab to make sure all of the students are looking at the models correctly.

      Forces and Bonding: Phase Distribution

      Setting Up for the Lab

      Locate or prepare 25- or 50-mL dropper bottles containing tetrachloroethane (solvent), acetone (solute), isopropanol (solute), ethanol (solute), and methylethyl ketone (solute). Place these in the hoods in one of the labs.

      Locate 1-mL GC syringes in the instrument room.

      Check out all 3 gas chromatographs for proper operation. Verify for each GC that gas tanks of He, H2, and air are reasonably full.

      Prelab Briefing

      Note: Because the lab will be run in two 1.5-hour shifts, the prelab briefing must be no longer than 30 minutes.

      Though it is discussed in the background section, discuss in simple terms how gas chromatography works, and how the instrument is designed. Spend some time explaining the significance of the GC Attenuation setting.

      Set up the problem to be investigated. The goal is to examine the manner in which a (liquid) solute partitions itself between two (immiscible) solvents, water and tetrachloroethane. Based on the distribution, one can draw conclusions about the relative strengths of intermolecular forces that operate between the solute molecules and the molecules of each solvent. If a particular solute prefers to be in the tetrachloroethane layer more than the water layer (as judged by the sizes of GC signals for the solute arising from the two layers), it is reasonable to conclude that this is a result of more favorable intermolecular forces between the solute and one of the solvents. The first purpose of the experiment then, is to find out which of the two solvents is favored by a particular solute, and to try to understand this in terms of the molecular structures of solute and solvent. Students should then predict which solvent will be favored by a second solute before they actually investigate it.

      Running the Lab

      Because this is an instrument lab, there is the usual potential problem of too much time spent standing around waiting for instrument access. To solve this we will use a "shift" system. In advance of the experiment, students in a section will be notified by email that half of them are to come at the regularly scheduled time; and the other half are to come 1.5 hours later. When the first group of students arrives

      • Give the prelab briefing to this group
      • Designate one of the solutes to be investigated
      • Divide them into three groups, one group per GC
      • Have each group prepare a vial containing equal volumes of the two solvents (water and tetrachloroethane), and a second vial containing a small amount of the designated solute
      • Take students to the instrument room and thoroughly demonstrate
        • Syringe rinsing
        • Syringe filling
        • Sample injection/computer activation
        • Data file (chromatogram) retrieval
        • How to extract retention time/signal area from the chromatogram
        • How to return the computer to the collect screen so that another series of injections can be made
      • Please be sure to stress to students the importance of reproducibility in injection volume/signal area, and the importance of getting good, reproducible signal areas for the solute signal in each solvent.
      • Tell students to begin their investigations. They do not need to print any chromatograms.
      • When a group finishes with the initial investigation (GC behavior of each solvent alone, of solute alone; and GC behavior of the solute partitioned between solvents), instruct the group to add a few drops of acetone to the vial, shake, and let stand for 2 minutes. Then repeat the GC investigation for this new situation. When the second group finishes, instruct them to add 0.5 mL of one solvent or the other to the vial, shake, and let stand for 2 minutes. Then repeat the GC investigation for this new situation.
      • Tell the groups that they will exchange data when finished

      When the second group arrives, give them the prelab briefing. The first group can continue on the GCs during the briefing, but must stop when the second group is ready to enter the instrument room.

      Students can, if motivated, discover the equilibrium concept from this experiment. Their GC data should show the RATIO of the concentration (signal area) of solute in solvent 1 to that in solvent 2 is the same in all experiments (the original expt with equal volumes of the two solvents and 5d solute; after addition of more of one of the solvents; and after addition of more solute):

      [Solute]H2O/[Solute]TCE = K (constant)

      This is the so-called partition coefficient. It is less than 1 when the solute prefers TCE, and greater than 1 when the solvent prefers water. You can discuss this during your prelab briefing if you want.

      Fundamentals: Graphing

      Setting Up for the Lab

      Several data sets are available for students to plot. Students in a particular section should all do the same data set. Enough copies of the set should be available so that each student gets one.

      Prelab Briefing

      Students are expected to have read the Background section of the experiment before coming to class, so all you should do in the prelab briefing is distribute the data and remind students what they are expected to do (discover the functional relationship between the 4 variables by making appropriate plots of the data). They should spend the 3-hour lab period making hand plots, then should redo the plots on a spreadsheet after the period is over.

      Running the Lab

      Students may need hints at various points in order to make progress. For example,

      • They may not realize that they have to select subsets of data within which only one of the three independent variables changes. Don't tell them this up front, but if it is clear that a pair of students does not know how to start, help them with this.
      • When they obtain a curved plot, they may not know what to do. Help them with this via a questioning process, rather than by telling them directly what to do.
      • They may have difficulty determining the slope and intercept of a linear plot. This is a good chance to distinguish "directly proportional" from "linearly related."
      • They may not know how to synthesize a single equation from equations determined from the data subsets. The subset equations take the following forms for variables x, y, z, and w (dependent variable):

        w = C1/x
        w = C2*y
        w = C3*z + C4

        Guide them to the general form

        w = K*y*(z + C4/C3)/x

        Ask them how to determine the value of K

      Forces and Bonding: Calorimetry

      Setting Up for the Lab

      The following items should be available in the lab:

      • Calorimeters and stirrers
      • thermometers (2 per student pair)
      • 100-mL graduated cylinders
      • burets
      • beakers and watch glasses for storing acid and base solution
      • 2 M NaOH, 2 M HCl, 2 M H2SO4

      Prelab Briefing

      Discuss the fundamental equation of calorimetry, q = -CcalDT.

      Discuss the logistics of collecting time-temperature data.

      Running the Lab

      Collect the Preparation, then give your prelab briefing.

      Each pair of students should be assigned two volumes of one of the acids to react with 50 mL of NaOH solution.

      Circulate, discuss technique with students, discuss what they expect their results to show.

      As students obtain data, prod them to think about whether or not their results are self-consistent.

      When students finish, they should rinse and return the calorimeter and stirrer, thermometers, graduates, and storage beakers.

      Reactivity: Synthesis of the Lewis Adduct of Cu2+ with Imidazole; Stoichiometry of Reaction

      Setting Up for the Lab

      Locate the reagents and equipment for the experiment, which include

      • Cu(NO3)2.2.5H2O
      • imidazole
      • stock solution of Cu(NO3)2.2.5H2O in water
      • stock solution of imidazole in water
      • Bunsen burners, rings, and wire gauzes
      • disposable spectrometer cells

      Set up the Spectronic 20 spectrometers, power them up. Power up the Hitachi U-2000 spectrometers.

      Set up top-loader balances.

      Prelab Briefing

      Briefly go over the experimental procedure, but do NOT give away the stoichiometry of the reaction. Remind students of the steps involved in suction filtration.

      Running the Lab

      Circulate while students are working; ask them what they have observed; give them tips on techniques.

      As students finish, be sure they

      • hand in their products
      • clean Pasteur pipets and graduated pipets by rinsing thoroughly with tap water, and place in the drying oven
      • Rinse Erlenmeyer flasks thoroughly with tap water and return to the Labkit

      Equilibrium: Vapor Pressure

      Setting Up for the Lab

      Locate the equipment and reagents for the experiment, which should be in a cabinet in GH110. They include

      • Large glass syringes
      • Small septum caps
      • Graduated pipet sections for use as rulers
      • 5-mL plastic syringes
      • Extension clamps
      • Bunsen burners/wire gauzes
      • Organic liquids: methanol, chloroform, ethanol

      Locate large beakers for use as water baths.

      Be sure a tank of nitrogen gas equipped with a regulator is available.

      Measure and record atmospheric pressure (barometer in GH07).

      Prelab Briefing

      Give a detailed explanation of the experimental procedure.

      Running the Lab

      Circulate and make sure students carry out the procedure properly. Some things to watch out for:

      • Sticky syringe plungers--frequent rotation of the plunger is necessary.
      • Proper reading of liquid and plunger levels.
      • Plunger should not rise above level of liquid in heating bath.

      Equilibrium: Solubility

      Setting Up for the Lab

      Locate the required equipment and materials:

      • Large beakers (750-1000 mL) (stored in Large Glassware cabinet)
      • 8-inch test tubes
      • Bunsen Burners
      • Iron rings/wire gauzes
      • Salts: KNO3, KClO3, KBrO3
      • thermometers

      Prelab Briefing

      Briefly discuss the solubility product concept.

      Running the Lab

      This lab is straightforward. Students should do the experiment in duplicate. In the second run, they should take a mass of salt calculated to produce temperatures falling between the temperatures observed in the first run.

      Equilibrium: Cobalt Complexes

      Setting Up for the Lab

      The following reagents should be available:

      • CoCl2.6H2O
      • 6 M ethanolic HCl (add concentrated HCl to an equal volume of ethanol)
      • Silver acetate

      Prelab Briefing

      Your briefing should not give away any of the expected experimental results. However, you should emphasize to students that their goal is to use Le Chatelier's Principle and their observations to complete the partial chemical equation presented in the Background section of the experiment. The results of their qualitative experiments should be sufficient to allow them to write a complete equation.

      Running the Lab

      Circulate; encourage students to apply Le Chatelier's Principle to make the connections between their experimental observations and the partial chemical equation in the Background section.

      Equilibrium: Bronsted-Lowry Acids and Bases

      Setting Up for the Lab

      You will need to make available the components of a microburet:

      • #5 1-hole rubber stopper
      • Plastic Pasteur pipet
      • Screw clamp

      Solutions of acids and bases must be available:

      1. 0.10 M Potassium hydrogen phthalate.
      2. 0.05 M NaOH
      3. 0.05 M HCl
      4. 0.10 M HNO3
      5. 0.10 M HCOOH
      6. 0.10 M CH3COOH
      7. 0.10 M NaHSO4
      8. 0.10 M CCl3COOH
      9. 0.10 M NaHCOO
      10. phenolphthalein indicator, 0.10 g/L
      11. methyl red indicator, 1.0 g/L

      Prelab Briefing

      Running the Lab

      Equilibrium: Conjugate Acids and Bases

      Setting Up for the Lab

      Locate pH meters in GH109A. Make available microburet components.

      A number of solutions must be available:

      Prelab Briefing

      Running the Lab

      Equilibrium: Binding of Lewis Bases to the Fe(CN)52- Ion

      Setting Up for the Lab

      Prelab Briefing

      Running the Lab

      Dynamics: NMR

      Setting Up for the Lab

      Locate the notebook containing NMR spectra of unknowns.

      Prelab Briefing

      Students should already be pretty comfortable with NMR, so your briefing does not have to be extensive. You may want to have them predict a spectrum from structure, and assign a structure from spectrum to make sure everyone is up to speed.

      Running the Lab

      Students should work in groups of 3. Each group should be assigned a molecular formula. Group members should figure out all possible isomeric arrangements consistent with the formula, and should predict the appearance of the NMR spectrum for each. Once they have done this, give them the NMR spectra for all unknowns with that formula, and tell them to deduce the isomeric structure that gives rise to each spectrum.

      Grading Scheme

      Preparation question: 5 points
      Lab notebook: 15 points as follows:
      5 points for possible structures
      6 points for NMR spectrum reasoning
      4 points for correct structure

      Dynamics: Infrared Spectroscopy

      Setting Up for the Lab

      Locate the large desiccator in GH109A. This contains NaCl crystals, crystal holders, and instrument mounting plates.

      Locate the samples in a cabinet in GH110. These should be in small plastic bottles.

      Prelab Briefing

      Briefly discuss the type of molecular motion that is observed in IR spectroscopy.

      DEMONSTRATE sample preparation technique and cell handling for liquid samples.

      DEMONSTRATE sample preparation technique and cell handling for solid samples.

      DEMONSTRATE the operation of the FTIR spectrometer and associated computer.

      Running the Lab

      Because there are only 3 FTIR spectrometers, students should be assigned to 6 groups, 2 groups per instrument.

      Assign two liquid and two solid samples to each group.

      Before running any spectra, each group should draw the structure for each of its assigned samples, and should predict the general appearance of the IR spectrum, focussing on stand-out features such as O-H, N-H, C-H, C=O, and C(3)N stretches.

      Each group should print each spectrum only once. If they want additional copies of their spectra, they can photocopy the originals following the lab.

      Grading Scheme

      Preparation: Question 1: 1 point
      Question 2: 2 points
      Question 2: 2 points

      Lab notebook: Focus question 1: 10 points
      Focus question 2: 3 points
      Focus question 3: 2 points

      Kinetics: The Reaction of Benzaldehyde and Acetone

      Setting Up for the Lab

      Benzaldehyde(2.0M)Acetone(1.00M)NaOH(3M)Comment
      12 mL12 mL27 mLtotal volume, one experiment
      18 mL18 mL40.5 mLwith 50% excess
      900 mL900 mL2024.5 mLtotal volume, 50 experiments
      1.80.9006.07moles solute needed
      190.852.2243grams solute needed

      In this experiment, we assume that the cloudiness always appears after the same amount (number of moles) of product has been produced, since we always work in the same total volume. Thus the inverses of the measured times give us a measure of the rate. We cannot obtain an actual rate in molarity per time, because we do not know how much product has been produced at the point of cloudiness (only that the amount is the same in every case).

      Suppose that in one experiment, your average time was 40 seconds, and in the next experiment, 80 seconds. Then the rates for the 2 experiments would be proportional to (NOT equal to) 1/time:

      Rate of first experiment ~ 1/40 = 0.025
      Rate of second experiment ~ 1/80 = 0.0125

      So its clear that the first rate is twice as large as the second.

      Similarly, in two experiments in which the concentrations of all participants (benzaldehyde, acetone, and OH-) are the same, the reciprocal of the measured time is proportional to the rate CONSTANT. This is relevant to the temperature data. A plot of 1/t versus T is equivalent to a plot of k versus T, as long as the 1/t values are all obtained under the same concentration conditions.

      Potential pitfalls include:

      1. The importance of very accurate reagent concentrations
      2. Pipetting techniques
      3. Inadequate mixing of reagents
      4. Inconsistencies in time measurements.

        Sample data:

        TVol benzvol acetonevol EtOHvol H2Ovol NaOHtime,s
        200.50.51.0123
        200.50.51.0130
        200.50.51.0129
        200.50.50.50.5249
        200.250.250.51.0271
        200.250.250.51.0272
        00.50.51.0462
        400.250.250.51.012

      Prelab Briefing

      Running the Lab

      Kinetics: The Reaction of Cr3+ and EDTA

      Setting Up for the Lab

      Solution Preparation:

      1. 0.10 M aqueous EDTA. To prepare 250 mL of 0.10 M EDTA, dissolve 9.306 g (25 mmole) Na2EDTA (MM = 336.21 g/mole)in about 100 mL of hot water in a beaker. Cool the solution, transfer quantitatively to a 250-mL volumetric flask, and add water to the mark. Alternately, 12.5 mmole H4EDTA (MM = 292.24 g/mole) and 12.5 mmole Na4EDTA (MM = 380.18 g/mole) may be used. (Scale the synthesis as necessary.)

        Pipet 50-mL aliquots of the stock solution to beakers, and use 6 M HCl or 6 M NaOH to adjust the solution pH to the values specified above. Then transfer to labelled storage bottles.

      2. 0.0125 M aqueous Cr(NO3)3.9H2O. Dissolve 3.125 mmole (1.250 g) Cr(NO3)3.9H2O (MM = 400.15 g/mole) in sufficient water to give 250 mL of solution.

      Power up thermostat baths, set for 35 oC.

      Set up and power up Spectronic 20 spectrometers. Power up Hitachi U-2000 spectrometers.

      Set out plastic spectrometer cuvets.

      Prelab Briefing

      Running the Lab

      Kinetics: The Reaction of I- and Hydrogen Peroxide

      Setting Up for the Lab

      Solution Prep

      0.2 M KI solution--dissolve 33.2 g KI in enough water to give 1.00 L of solution.

      0.2 M Na2S2O3 solution--dissolve 31.62 g Na2S2O3 in enough water to give 1.00 L of solution.

      0.4 M H2O2 solution--Add 35.34 mL of 30% H2O2 to enough water to give 1.00 L of solution.

      0.2% by weight starch solution--Slurry 2 g soluble starch in enough water to give 1.00 L of solution. Heat the slurry over a burner until the starch dissolves.

      Buffer solutions, pH 2.2 to 8 at 20 oC. These solutions are prepared by mixing various volumes of two solutions, A and B, to give a total volume of 20 mL. Solution A is 0.4 M sodium hydrogen phosphate (Na2HPO4) prepared by dissolving 143.2 g of Na2HPO4.12H2O in distilled water to give 1.0 L of solution. Solution B is 0.2 M citric acid prepared by dissolving 42.0 g of H3C6H5O7.H2O (or 38.4 g H3C6H5O7) in sufficient distilled water to give 1.00 liter of solution. Addition of 3-5 mL of ethanol will retard the growth of mold.

      mL Solution AmL Solution BpH
      0.4019.62.2
      1.2418.762.4
      2.1817.822.6
      3.1716.832.8
      4.1115.893.0
      4.9415.063.2
      5.7014.303.4
      6.4413.563.6
      7.1012.93.8
      7.7112.294.0
      8.2811.724.2
      9.3510.654.6
      9.8610.144.8
      10.309.705.0
      10.729.285.2
      11.158.855.4
      11.608.405.6
      12.097.915.8
      12.637.376.0
      13.226.786.2
      13.856.156.4
      14.555.456.6
      15.454.456.8
      16.473.537.0
      17.392.617.2
      18.171.837.4
      18.731.277.6
      19.150.857.8
      19.450.558.0

      Prelab Briefing

      Running the Lab

      Kinetics: Enzyme Catalysis

      Setting Up for the Lab

      Students should do this experiment in groups of 3. We need sufficient solution for 30 groups. Each group will require about 5 mL of each "cocktail"; about 0.5 mL of glucose oxidase stock solution; and about 1 mL of glucose stock solution. All solutions should be prepared using pH7 phosphate buffer.

      Glucose oxidase stock solution: Dissolve 2.5 mg of glucose oxidase in enough phosphate buffer to give 100 mL of solution. STORE SOLUTION AT JUST ABOVE 0 oC UNTIL THE DAY OF THE EXPERIMENT.

      Glucose stock solution: Dissolve 18.0 g of D-glucose in enough phosphate to give 100 mL of solution.

      ABTS/HRP stock solution: Dissolve 0.2744 g of the diammonium salt of ABTS in phosphate buffer to give a total volume of 10.00 mL. Add 40 microliters of horseradish peroxidase suspension.

      0.1 M Phosphate Buffer, pH 7: Dissolve 1.200 g NaH2PO4 in distilled water to give 100 mL of solution. Add small volumes of concentrated NaOH solution to bring pH to 7.00.

      Cocktail #1. Use the following volumes of the above solutions to prepare 100 mL of cocktail:

      • 80 mL buffer
      • 5 mL of ABTS/HRP stock solution
      • 10 mL of glucose stock solution
      • 5 mL of distilled water

      Cocktail #2. Use the following volumes of the above solutions to prepare 100 mL of cocktail:

      • 80 mL buffer
      • 5 mL of ABTS/HRP stock solution
      • 5 mL of glucose oxidase stock solution
      • 10 mL of distilled water

      Requirements for one group of 3:

      • 5 mL cocktail #1
      • 5 mL cocktail #2
      • 0.5 mL glucose oxidase stock
      • 1.0 mL glucose stock

      Total requirements for 30 groups:

      • 150 mL cocktail #1
      • 150 mL cocktail #1
      • 15 mL glucose oxidase stock
      • 30 mL glucose stock

      Add 50% for waste.

      Prelab Briefing

      Running the Lab

      The 8 AM labs will be done in shifts--see yesterday's email. Students will work in group of 3. This will give 10 groups in a section.

      In addition to the 3 spectrometers in the general chem lab, there are 2 downstairs in GH07 that we can use. So assign 2 groups per spectrometer. Groups will carry out alterate 6-minute runs at the spectrometer.

      We will need two sets of reagents (cocktails 1 and 2, glucose stock, glucose oxidase stock), one in 109A and one for downstairs.

      Please SIGN OUT a stopwatch to each group that does not have one.

      For kinetics runs, students should mix the reagents directly in the cuvet, shake the cuvet, and place it in the spectrometer. They should take an absorbance reading at each minute mark, ending at 6 minutes.

      With 2 groups per spectrometer, the total minimum time required to obtain data is 7 runs per group * 6 min per run * 2 groups = 84 minutes. This cuts it close, so they will have to work efficiently.