Lab Summary

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School

University of Waterloo *

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Course

121

Subject

Chemistry

Date

Dec 6, 2023

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pdf

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8

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Procedure: Use the blue requisition slips on top of the bench turrets to sign out the following items from the Storeroom: 1 evaporating dish 1 Buchner funnel 1 500 mL vacuum flask 1 length of vacuum tubing Pick up from the side bench, equipment drawers or cabinets: 1 Bunsen burner 1 metal rod 1 ring clamp 1 wire gauze 155 mm, #1 filter paper De-ionized (DI) water : DI water is used for all experiments in the first-year chemistry lab. Tap water (from the bench sinks) is only used for washing your hands and washing dishes. When you arrive in the lab each day, fill your wash bottle with DI water from the labelled taps at the side bench sinks. (Ask your TA if you can't find it!) This will save time as you will always have DI water when you need it. Empty your wash bottle at the end of each lab, do not store DI water in your locker. A note on significant digits (significant figures) in procedures: Values in the procedures are always written with the appropriate number of significant digits, thus, the digits in the value indicate the accuracy required in your measurement. If you are asked to measure 5.00 mL of a liquid, you must choose a measuring tool that will measure with an accuracy of ‡ 0.01 ml, a pipette or burette would be required. However, if you are asked to measure a volume of 5 mL, (this would mean 5 ‡ 1 mL) a graduated cylinder would be adequate. Reaction 1 : Copper metal to copper (Il) nitrate (Time required: 10-15 minues) Obtain a length of copper wire (99.99% pure) and a piece of sandpaper from the side bench. Sand the wire to remove any coating that may have been added by the manufacturer to prevent corrosion / oxidation. After sanding, take the wire to the analytical balance room to weigh. From the list on the balance room wall find the number of the analytical balance you are to use. You share this with the students working beside you. Only the students performing the weighing are allowed inside the balance room, no spectators please. All digits displayed on the analytical balances should be recorded (this will give you a mass in grams with 4 decimals, that is, these masses are accurate to 1/10000th of a gram). Record the mass of your copper wire on your data sheet.
Back at your workbench, place the copper wire in a labelled 250 mL beaker (you need to be able to identify which beaker is yours) so that the wire sits flat on the bottom of the beaker. This is done so that the entire piece of wire is immersed in the small volume of acid you will add at the next step. (Coiling the wire works well here.) Take the beaker containing your wire and a 10 mL graduated cylinder to the fume hood. In the fume hood, add 10 mL of concentrated (15.8 M) nitric acid, HNO3, to the wire in your beaker. Once you have added acid to your beaker, place it towards the back of the fume hood and move away from the fume hood to let others begin their reaction as well. This reaction is very easy to observe from several metres away. Let the nitric acid and the copper wire react in the fume hood while you observe and record a description of this step of the reaction on your data sheet. Do not remove the beaker from the fume hood yet! After the wire has dissolved, swirl the beaker in the fume hood to remove any gasses trapped in the solution. This may take a while! You may safely remove your beaker from the fume hood when no gas is observed upon swirling and the solution is bright blue. Observe and record a description of this step of the reaction on your data sheet. This chemical change may be represented by the equation: Cu (s) + 4 HNO3 (aq) → Cu(NO3)2 (aq) + 2 N02 (g) + 2 H20 (I) Reaction 2: Copper (Il) nitrate to copper (Il) hydroxide (Time required: 5 minutes) Back at your workbench, dilute the resulting solution with ~25 mL of deionized (DI) water. Locate the 6.0 M NaOH on the side dispensing bench. Measure ~ 25 mL into a small beaker or graduated cylinder and bring it back to your workbench. Slowly add -25 mL of 6.0 M NaOH to the diluted Cu(NO3)2 solution while stirring. The solution should be strongly alkaline (pH >10) after this addition. pH paper is available on the side bench for testing the pH of this solution. If the pH is too low at this step, add an additional ~5 mL of NaOH and check the pH again. Repeat this ~5 mL addition if necessary. Observe and record a description of this reaction on your data sheet. Reaction 3: Copper (Il) hydroxide to copper (Il) oxide (Time req'd: 20-70 minutes) Separation and purification of a gelatinous precipitate such as Cu(OH)2 is difficult because its separation by filtration proceeds slowly. After separation, the process of washing it on filter paper to remove soluble salts is time-consuming and not very effective. Since Cu(OH)2 decomposes upon heating to form a non-gelatinous precipitate, CuO, the copper will be recovered at this stage as CuO rather than Cu(OH)2. Heating step: 10 - 15 minutes Set up a heating apparatus as shown. You control this set up, position your clamp such that you will be able to use a small, easily controlled flame.
Heat the mixture gently, stirring continuously to prevent bumping, until the boiling point is reached. Continue to heat gently for one minute to better coagulate the CuO and to ensure that all the blue Cu(OH) has been converted to black CuO. At this point the solid black CuO should separate from the clear liquid supernatant. Observe and record a description of this reaction on your data sheet. Filtration step: 10 - 60 minutes Once you have produced solid CuO, you will need to isolate it from the aqueous solution using vacuum filtration. Set up a vacuum flask with a Buchner funnel as shown, and filter as described in Appendix C In order to quantitatively transfer all of the CuO from the beaker to the Buchner funnel, swirl the beaker gently before adding solution to the funnel. When no more of the thick solution can be poured or scraped into the funnel, use three ~10 mL portions of deionized water to rinse the remaining CuO out of the beaker into the Buchner funnel. Add each ~10 mL portion of water, swirl and/or stir the beaker to remove as much CuO as possible with each rinsing, then use this rinse water to wash the precipitate on the filter paper. Allow as much of the rinse water as possible to drain from the precipitate before adding the next portion of rinse water. Before this rinsing, the CuO is wet with solution that contains considerable NaNO and NaOH. The purpose of washing is to replace this solution with water. After all the CuO has been collected on the filter paper, discard the filtrate into the appropriate waste container in the fume hood. Observe and record a description of the solid CuO on your data sheet. Reaction 4: Copper (Il) oxide to copper (Il) sulphate (Time req'd: ~10 minutes) The next step is to convert the CuO to CuSO4 by the action of dilute sulphuric acid, H204. Copper sulphate is water-soluble and dissolves as it is formed from CuO. In the process, the Cu?+ ion is hydrated; that is, it forms Cu(H20)4+ . Because of the high solubility of CuSO4, the crystalline compound will not be isolated but converted to Cu. Locate the 3 M H≥SO4 in the dispensing fumehood, be sure to read the label on the bottle carefully. Measure ~ 20 mL into a small beaker or graduated cylinder and bring it back to your workbench. (This volume is an excess of H2SO4 and does not need to be accurately measured.) Transfer most of the CuO from the filter paper back into the beaker in which it was precipitated. Then, holding the filter paper over the beaker with a pair of tweezers, use ~20 mL of 3 M H2SO4 to rinse the remaining CuO from the filter paper into the beaker. A small amount of this now acidic solution can also be used to rinse any CuO solid from the Buchner funnel. Droppers
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