CHM 114 Study Guide - Final Guide: Volumetric Flask, Pipette, Burette

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28 Sep 2016

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Purpose: the purpose of the experiment was to learn how to properly use three volumetric instruments to determine the density of an unknown substance. This includes knowing how to fill and read a volumetric flask, a volumetric pipette, and a buret. Theory: determining the density of a liquid or any substance requires the mass of the substance and its volume. The mass of the substance can be weighed on a scale subtracting the mass of the container holding it. The volume however, can be determined a number of ways in this experiment. We used a volumetric flask, volumetric pipette, and burette to collect a volume of 10 ml from each. To properly measure these instruments, one must read from the bottom of the meniscus to determine the volume. The meniscus is the curved part at the top of the apparatus. This is due to the fact that the error of adhesion is already accounted for by the instruments.

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Equipment Materials

50.00 ml buret, 250.ml volumetric flask, 1.00 ml volumetric pipet 10.0 mL volumetric pipet, 25.00 mL volumetric pipet, pipettor, 250 mL Erlenmeyer flask, 10.0 mL graduated cylinder, several beakers, several watchglasses, unkown bleach solution, 10% potassium iodide solution, 2M hydrochloric acid solution, 0.150 M sodium thiosulfate solution, 1% starch solution.

Background information regarding this experiment is as follows:

An aqueous solution of sodium hypochlorite (NaOCI) is a clear, slightly yellow liquid, and is commonly known as bleach. Aside from its uses as a bleaching agent, sodium hypochlorite solutions are also used as sterlizing agents and in water treatment. Industrial uses include agricultural, food handling, paper production, and textile production. Sodium hypochlorite is also added to waste water to reduce odors.

The concentration of sodium hypochlorite in bleach solutions can be determined by titration. Therefore, we must use a two-step method to titrate sodium hypochlorite. In the first step, sodium hypochlortie, hydrochloric acid, iodide ion, and starch are combined to form a starch-triiodide complex. In this step there are 3 reactions that take place:

The result of these 3 reactions is that when sodium hypochlorite is present the starch-triiodide complex is produced.

In the second step the starch-triiodide product is titrated by sodium thiosulfate to form a colorless solution of iodide, dithionate.

I do not know how to answer the following on the data sheet: (? means I do not know how to answer)

Table 1:

Mass of 1.00 ml of unknown (by tare): 10.552 g

Density of bleach: (g/ml) : 1.055 g/ml

Volume of diluted bleach used in each titration: 10.00

Concentration of sodium thiosulfate: ? (M)

Titration Data:

Initial buret reading (ml): trial1: 0.000 ml Trial 2: 0.00 ml Trial 3: 0.000ml

Final buret reading (ml): trial 1: 13.50ml Trial 2: 13.30ml Trial 3: 13.40ml

Volume delivered(ml: trial 1: ? Trial 2: ? trial 3:?

Calculations: (show clearly)

For trial 1,2,3 ???

1.Moles of Na₂S₂O₃ in titration: ??? trial 1,2,3

2.Moles of NaOCl: ???trial 1, 2,3

3.Average moles of diluted NaOCl: (one answer) ?

4.Average moles of undiluted NaOCl: (one answer.. mol) ?

5.Standard Deviation: (one answer) (mol)

6.Average mass of NaOCl in 25.00mL of undiluted bleach: ? (g)

7.mass of 25.00 mL of undiluted bleach: ? (g)

8. Mass % of NaOCL from experiment: ? (%)

9.Actual mass % of NaOCL (from prof; student does not make an entry):? (%)

More questions all need to be answered please:

1. Calculate the volume of the reagent thiosulafte solution which would be required if you titrated a 25ml sample of the original commercial bleach instead of 25ml of the diluted solution.

2. Why would we choose a graduated cylinder to measure the HCl and KI solutions instead of a volumetric pipette? When would we use a volumetric pippette?

3. You calculated the mass percent of sodium hypochlorite in the bleach( dilute and undiluted). Now calculate the molarity of the sodium hypochlorite in the diulte and undiluted solution/

4. Use oxidation states to show that equations (2) and (4) in the introduction are redox reactions and that equation 1 is not a redox reaction. :

-(1) NaOCl(aq) + HCl(aq) yields HOCl(aq)+NaCl(aq)

-(2) HOCL (aq) + HCl(aq) + 3I(aq) yields I3(aq) + 2CL(aq) + H₂O(l)

-(4) (I₃) (Starch) + 2S₂O₃ yields 3I + S₄O₆ + starch

5. combine equation 1-3 to show the overall reaction for the products of the starch-triiodide complex.

-(1) NaOCl(aq) + HCl(aq) yields HOCl(aq)+NaCl(aq)

-(2) HOCL (aq) + HCl(aq) + 3I(aq) yields I3(aq) + 2CL(aq) + H₂O(l)

-(3) I₃ + Starch yields (I₃) (Starch)

6. What standard was used in this experiment?

7. Describe the naming of NaClO and HClO. What are the names of the following compounds? NaClO₂ , NaClO_3, NaClO₄ , HClO₂, HClO₃, HClO₄

8 Submit a one paged (typed double spaced) report that discusses the following topics:

a. the goals or objectives of the experiment

b.your results as they relate to the goals and objectives

c. the quality of your results.

1-How many grams of NaCl would be needed to prepare 150.00 L of a 1.402 M NaCl solution?

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2- first a standardized solution of sodium hydroxide (NaOH) will be quantitatively diluted to about 0.1 M but not exactly 0.1M. The molarity of the dilute NaOH will be calculated! A similar quantitative dilution was done in experiment 3 when you diluted 5.0 M HCl to 0.50M HCl using a volumetric flask and pipet.

The second part of the experiment is very similar to the last part of experiment 6 where samples of the unknown were weighed out, dissolved in water, and titrated with the dilute NaOH using phenolphthalein as the indicator to determine the percent by mass of a compound in the unknown. The compound will be different than the compound used in experiment 6. The molecular formula of the compound will be provided during the final. You must know how to weigh by difference (Preweigh, tare sample and small container to zero, transfer sample to flask, and place the small container back on balance to get mass) and titrate the sample using the buret in order to do well.

Be sure to read the instructions for the practical toward the end the CHM151L lab manual and do the practice problem on the next page.

You will have 1.5 hours to do the practical. You may only use a calculator and a pencil on the practical. There is no talking during the practical such that students cannot help each other and the TA may only help you with equipment problems.

It would be a good idea to wash any glassware you might use the lab period before the lab practical. There will also be a help session before the lab practical.

At the end of the lab final you will wash all glassware used or any dirty glassware in your locker, wash your unknown vials and remove the labels, checkin your locker and return your key, and evaluate the lab.

Please put the following statements in the correct order relating to the day of the lab practical:
1 2 3 4 5 6 Wash all your glassware and unknown vials, checkin your locker, evaluate the lab, and check your grades.
1 2 3 4 5 6 Do at least 3 good trials (weigh and titrate sample) as time allows.
1 2 3 4 5 6 Start the lab practical by diluting the NaOH solution.
1 2 3 4 5 6 Before the day of the practical clean glassware, read the practical instructions and do the practice problem in the lab manual and complete the loncapa problems for the final.
1 2 3 4 5 6 Calculate the molarity of the dilute NaOH, the percent by mass of the compound in you unknown for each trial and then the median.
1 2 3 4 5 6 Come to the help session before the lab final.

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A NaOH solution was prepared by diluting 5.00 mL of 2.205 M NaOH to a final total volume of 100.00 mL. What is the exact molarity of the dilute NaOH (use 4-5 significant figures)?

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4-For the problem above, select glassware and size from the list below to conduct the dilution.

A	Amber Bottle
B	Mohr pipet
C	Buret
D	Volumetric Flask
E	Volumetric Pipet or Pipettor
F	Graduated cylinder
G	Erlenmeyer flask
H	Beaker

A B C D E F G H <= Glassware used to transfer the 2.205 M NaOH to be diluted
A B C D E F G H <= Glassware used to measure the final volume of the diluted M NaOH.

5 10 15 20 25 50 100 250 500 1000 <= Volume of the glassware chosen to transfer the concentrated NaOH above
5 10 15 20 25 50 100 250 500 1000 <= Volume of the glassware chosen to contain the final dilute NaOH above.

If you were to over-titrate your calcium solutions in Part B of this lab:a.Would the calculated molarity of EDTA be too high or too low? Explain.

b.Would the calculated molarity of calcium unknown in part C be too high or too low? Explain.

Part B Setup: Complete the following steps, after reading page 6 on how to use volumetric glassware:1.You should have already used a 500 mLvolumetric flaskto prepare an approximately 0.010 M solution of Na2EDTA (Part 1).2.Clean the buret carefully and rinse it two or three times with small amounts (~5mL) of your EDTA solution. Hint; use a clean, dry, labeled beaker to pour solution into the buret. Make sure you rinse through the tip and that no air bubbles are in the tip. Mount the buret on a ring stand using buret clamps. Fill the buret with your EDTA solution nearly to the top mark (to somewhere between the 0 and 5 mL marks for every trialâDO NOT waste time filling the buret to exactly 0.00 mL!). The EDTA is the titrant,the solution added during the titration. Chemistry 161 Lab5Bozlee -Based on S. Critchlow Winter 2018page 4of 11Green River Community College Standardization of the EDTA solution:4.Record the exact reading of the liquid level (bottom of the meniscus) in the buret, recording to the nearest 0.01 mL. This is your initial volume. Note:The burets can be read to a precision of at least +/-0.02 mL. Be sure that all of your readings are precise and consistent.Check with your instructor if you are unclear whether your buret readings are correct.5.In a clean dry beaker, take about 50 mL of standard 0.01000 MCa2+solution; do not take more than this at a time. This is enough to do two trials; if only doing one trial take no more than 30 mL. After proper rinsing, pipet 20.00 mLof this standard Ca2+solution into a 125 mL Erlenmeyer flask. The volumetric pipet tip should NOT be âblown out.â Add about 25 mL of deionized water to the flask.The volume of water is not critical.6.Add a few drops (~6) of indicatorand one full dropperfulof the buffer solutionto the solution in the Erlenmeyer flask.7.Place the stir bar in the flask, place the flask on the stir plate, and set the control for gentle stirring. Or, if you have a good swirling technique with the Erlenmeyer flask, the stir bar and plate is unnecessary. It is essential that the solutions be continually stirred or swirled while titrating.8.What net volume of titrant should be required for the standard trials? You should be able to predict this by calculation!Slowly add your EDTA solution from the buret until the endpoint is reached. The endpointin this titration is the point at which the solution in the Erlenmeyer flask first turns a distinct blue. The color change of the indicatorat the endpoint signals that the equivalence pointhas been reached, where the reactants are in the correct stoichiometric ratio to completely react. As you near the endpoint, add EDTA drop by drop to avoid âovershooting the endpoint.â Record to the nearest 0.01 mL the exact liquid level of EDTA in the buret (your final volume), and calculate the net volume of EDTA used in the titration by subtracting the initial volume from the final volume of EDTA.9.Discard your waste in the appropriate container, using only a very small amount of DI water as the first rinse. Then rinse out your Erlenmeyer flask thoroughlywith several portions of DI water at your sink. Refill the buret (always to between 0 and 5 mL) if you will do another trial. 10.Repeat steps 4-9 two more times, using a fresh aliquot(measured sample) of standard Ca+2solutioneach time. Ideally your replicate titrations should agree within 0.2 mL

CHM 114 Study Guide - Final Guide: Volumetric Flask, Pipette, Burette

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