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Lab Experiment 1 Acid-Base Titrations with Worksheet, Lab Reports of Chemistry

General Chemistry lab manual on acid base titration is here. First lab experiment in EPL CHEM 153 class.

Typology: Lab Reports

2020/2021

Uploaded on 03/30/2021

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Experiment 1
Acid-Base Titrations
Discussion
Volumetric procedures are among the most common and convenient methods of analysis. The
preparation of a reactive solution of accurately known concentration is fundamental to these
methods, and the exercise serves as an introduction to the techniques of solution preparation and
titration.
The objective of this exercise is to prepare and accurately determine the concentration of a solution
of NaOH, and to use that standardized solution in the determination of the concentration of acid in a
commercially available sample. The first step is the preparation of a sodium hydroxide solution
whose concentration is approximately known. The second step is the determination of the
concentration accurately by titration with a solution containing a known concentration of a primary
standard, in this case potassium hydrogen phthalate. (Primary standards are substances which
may be obtained in a stable form of known purity and which react with other substances quickly in
a definite and known manner.)
Potassium hydrogen phthalate and sodium hydroxide react as follows:
KHC8H4O4 + NaOH KNaC8H4O4 + H2O
or, expressed as an ionic equation:
HC8H4O4+ OH C8H4O42– + H2O
The complete structure of potassium hydrogen phthalate is
This reaction is a representative of an acid-base reaction. In this case the hydrogen phthalate ion is
the acid (proton donor) and the hydroxide ion is the base (proton acceptor). The stoichiometric
ratio between the hydrogen phthalate ion and the hydroxide ion, and therefore between the
potassium hydrogen phthalate and the sodium hydroxide, is obviously one to one.
The equivalent weight of an acid (also called an equivalent) is the weight in grams that
furnishes one mole of H+ ion in an acid-base reaction. Correspondingly, the equivalent weight
of a base is the weight in grams that accepts one mole of H+ ion in an acid-base reaction. (In the
reaction under consideration, what is the equivalent weight of the potassium hydrogen phthalate and
the sodium hydroxide?)
CH
CH
CH
C
C
CH
C
C
O
OH
O
O-K+or
COOH
COO-K+
pf3
pf4
pf5

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Experiment 1

Acid-Base Titrations

Discussion Volumetric procedures are among the most common and convenient methods of analysis. The preparation of a reactive solution of accurately known concentration is fundamental to these methods, and the exercise serves as an introduction to the techniques of solution preparation and titration. The objective of this exercise is to prepare and accurately determine the concentration of a solution of NaOH, and to use that standardized solution in the determination of the concentration of acid in a commercially available sample. The first step is the preparation of a sodium hydroxide solution whose concentration is approximately known. The second step is the determination of the concentration accurately by titration with a solution containing a known concentration of a primary standard , in this case potassium hydrogen phthalate. (Primary standards are substances which may be obtained in a stable form of known purity and which react with other substances quickly in a definite and known manner.) Potassium hydrogen phthalate and sodium hydroxide react as follows: KHC 8 H 4 O 4 + NaOH → KNaC 8 H 4 O 4 + H 2 O or, expressed as an ionic equation: HC 8 H 4 O 4 –^ + OH–^ → C 8 H 4 O 4 2–^ + H 2 O The complete structure of potassium hydrogen phthalate is This reaction is a representative of an acid-base reaction. In this case the hydrogen phthalate ion is the acid (proton donor) and the hydroxide ion is the base (proton acceptor). The stoichiometric ratio between the hydrogen phthalate ion and the hydroxide ion, and therefore between the potassium hydrogen phthalate and the sodium hydroxide, is obviously one to one. The equivalent weight of an acid (also called an equivalent ) is the weight in grams that furnishes one mole of H+^ ion in an acid-base reaction. Correspondingly, the equivalent weight of a base is the weight in grams that accepts one mole of H+^ ion in an acid-base reaction. (In the reaction under consideration, what is the equivalent weight of the potassium hydrogen phthalate and the sodium hydroxide?)

CH

CH

CH

C

C

CH

C

C

O

OH

O

O

  • K + or^

COOH

COO

  • K +

In determining the exact concentration of a solution, a procedure called a titration is commonly used. A titration is a process in which a solution containing a known amount of a substance is allowed to react with a second solution containing an unknown concentration of another substance that will react with the first substance in a known and reproducible manner. The substances are allowed to react until there is some indication that equivalent amounts of the substances have reacted. The solutions are measured from a buret , a long, graduated glass tube with a stopcock at the bottom. In the present case a solution of potassium hydrogen phthalate is prepared in an erlenmeyer flask by dissolving an exactly known weight of pure potassium hydrogen phthalate in water. The sodium hydroxide solution (whose exact concentration is unknown), is delivered from a buret until an amount equivalent to the amount of potassium hydrogen phthalate has been added. This point in the process is called the equivalence point of a titration. We can monitor the progress of acid-base titrations by two means. The first uses a pH meter, and the second uses an acid-base indicator. An indicator is a dye that has the particular property of changing color as a function of pH. You will select an appropriate indicator to use in your titrations based on the data you obtain using a pH meter. The point in the titration when the indicator changes color is called the end point. Ideally the indicator should be selected so that the end point coincides with the equivalence point. Procedure (For instructions on using the pH meters, see below) Using the ~9M NaOH solution provided, make up approximately 500 mL of ~0.1M NaOH in a polyethylene bottle. Cap tightly and shake thoroughly. You will standardize your NaOH solution against potassium hydrogen phthalate. Accurately weigh by difference 4 separate 0.20-0.30 g portions of dry potassium hydrogen phthalate into clean and dry 150 mL or 250 mL beakers. Add approximately 50-100 mL distilled water to each and swirl until the potassium hydrogen phthalate is completely dissolved. Do a rough titration (Titration 1), adding approximately 1 mL of your NaOH solution at a time, recording the pH after each addition (be sure to give the reagents a few seconds to fully react before recording the pH.) In recording data from a titration, record the actual buret readings (estimate to nearest 0.01 mL), not the volume of titrant delivered. This eliminates a possible source of error. Make a rough plot of your titration data. Based on your titration curve, select an appropriate indicator and add a few drops to one of the three remaining flasks. Titrate this sample more carefully (Titration 2) – recording both the pH meter as well as the indicator. You may add approximately 0.5 mL at a time in the "flat" regions of the titration curve, then add 1 drop at a time as the pH begins to change more rapidly close to the equivalence point. You should determine the equivalence point to within a drop of titrant. Record the color change along with the volume of NaOH used and the pH and check that the chosen indicator accurately marks the equivalence point of your titration. If that is the case, add your indicator to the remaining two samples and titrate those (Titration 3 and

  1. without the help of the pH meter, only using the indicator. Again, determine the equivalence point to within a drop of titrant.

Function Slope Temperature Standardize Stir plate Electrode buret Stir bar Figure 1. Set-up for titration using the Acumet pH meter.

Experiment 1 Worksheet — Acid-Base Titrations

Name___________________________ Date of Experiment: ____/____/____ Date of Report: ____/____/____ Standardization of NaOH solution against potassium hydrogen phthalate Molarity of NaOH: _______________ ± _______________ ( ± ____________ %) (average) (std. dev.) (rel. error) Prepare a titration curve (you can use a computer graphing program if you choose) for your careful titration following the guidelines in the introductory pages and turn it in with your worksheet. Mark the equivalence point and its coordinated on both axes. Please attach your analysis: Report your initial data (weight of samples, volume of titrant used). Introduce symbols for your numerical quantities and use those in equations to indicate the mathematical transformations performed for every step in your analysis. Calculate and report the standard deviation (error) along with the average of the molarity. See the sample analysis in the introductory section. Discuss if the indicator you used was appropriate for your sample. Are your results reasonable? Determination of concentration of commercial acid Commercial acid sample: ___________________________ Identity of acid in sample: ___________________________ Concentration of acid according to label: _______________ Molarity of commercial acid: ________________________ ± __________ Concentration of acid in weight %: ____________________ ± __________ Attach a titration curve for the commercial acid and show your results and calculations on a separate sheet. Follow the guidelines given above. For the discussion, you could consider the following questions. Does your result agree with the bottle label? Does your result seem to make sense? Is the manufacturer cheating? Any comments about possible discrepancies?