Bringas, XyzaMarize D.

2 ChE A

February 23, 2011 Maam Susana D. Torres

Experiment 05 VOLUMETRIC ANALYSIS OF A CARBONATE BICARBONATE MIXTURE

I. Abstract Volumetric analysis is quantitative analytical techniques which employ a titration in comparing an unknown with a standard. In a titration, a volume of a standardized solution containing a known concentration of reactant "A" is added incrementally to a sample containing an unknown concentration of reactant "B". The titration proceeds until reactant "B" is just consumed (stoichiometric completion). This is known as the equivalence point. At this point the number of equivalents of "A" added to the unknown equals the number of equivalents of "B" originally present in the unknown. Volumetric methods have the potential for a precision of up to 0.1%. For volumetric methods to be useful, the reaction must reach 99%+ completion in a short period of time. In almost all cases, a buret is used to meter out the titrant. When a titrant reacts directly with an analyte, the procedure is termed a direct titration. The alternative technique is called a back titration. Here, an intermediate reactant is added in excess of that required to exhaust the analyte, then the exact degree of excess is determined by subsequent titration of the unreacted intermediate with the titrant. Regardless of the type of titration, an indicator is always used to detect the equivalence point. Most common are the internal indicators, compounds added to the reacting solutions that undergo an abrupt change in a physical at or near the equivalence point. Sometimes the analyte or titrant will serve this function. External indicators, electrochemical devices such as pH meters, may also be used. Ideally, titrations should be stopped precisely at the equivalence point. However, the everpresent random and systematic error, often results in a titration endpoint, the point at which a titration is stopped, that is not quite the same as the equivalence point. Fortunately, the systematic error, or bias may be estimated by conducting a blank titration. In many cases the titrant is not available in a stable form of well-defined composition. If this is true, the titrant must be standardized against a compound that is available in a stable, highly pure form, a primary standard is an example. II. Introduction This experiment entails first standardizing a sodium hydroxide with a primary standard and standardizing hydrochloric acid solution using standardized sodium hydroxide as a secondary standard. The objective of this experiment is to have the percentage of Na2CO3 and NaHCO3 that is present in the sample.

III. Review of Related Literature In chemistry, a carbonate is a salt of carbonic acid, characterized by the presence of the carbonate ion, CO32-. The name may also mean an ester of carbonic acid, an organic compound containing the carbonate group C(=O)(O)2. The term is also used as a verb, to describe carbonation: the process of raising the concentrations of carbonate and bicarbonate ions in water to produce carbonated water and other carbonated beverages either by the addition of carbon dioxide gas under pressure, or by dissolving carbonate or bicarbonate salts into the water. In geology and mineralogy, the term "carbonate" can refer both to carbonate minerals and carbonate rock (which is made of chiefly carbonate minerals), and both are dominated by the carbonate ion, CO32-. Carbonate minerals are extremely varied and ubiquitous in chemicallyprecipitated sedimentary rock. The most common are calcite or calcium carbonate, CaCO3, the chief constituent of limestone, dolomite, a calcium-magnesium carbonate CaMg(CO3)2, and siderite, or iron (II) carbonate, FeCO3, an important iron ore. Sodium carbonate and potassium carbonate have been used since antiquity for cleaning and preservation, as well as for the manufacture of glass. Carbonates are widely used in industry, e.g. in iron smelting, as a raw material for Portland cement and lime manufacture, in the composition of ceramic glazes, and more. In inorganic chemistry, bicarbonate (IUPAC-recommended nomenclature: hydrogen carbonate) is an intermediate form in the deprotonation of carbonic acid. Its chemical formula is HCO3. Bicarbonate serves a crucial biochemical role in the physiological pH buffering system.

IV. Methodology y Preparing the sample

We dissolved 2.0 grams of the solid sample in 100 milliliters of distilled water, and then transferred it to a 250 milliliters volumetric flask. We diluted the solution until it reached the blue line of the flask and inverted the flask for several times for uniform mixing. y Classical Method

In classical method, we measured 50 milliliters of the sample and put it on a flask or a beaker, and then we added 3 drops of indicator which is phenolphthalein and titrated it with HCl. After recording the volume of HCl used when a pink-colored

solution is obtained weve added 3 drops of methyl orange as in indicator, then recorded the volume used when an orange-colored solution appeared. y Using the pH meter

Here, we measured 15 milliliters of the sample and added 10 milliliters of distilled water. Using a pH meter which already has a buffers standardized in it, we immersed the electrode into the solution and the burette with HCl. In every 0.5 milliliters of HCl used weve recorded its pH until we reached its constant value.

V. Discussion of Data and/or Results

Classical Method Volume (1st end point) Volume (2nd end point) Trial 1 14.5 mL 48.5 mL Trial 2 14.5 mL 48.0 mL

In the classical method, the volume of the first end point for trial 1 and trial 2 are just the same. And for the volume of the second end point Using pH meter mL 0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 pH 9.81 9.75 9.65 9.50 9.40 9.21 9.03 8.75 8.30 7.58 7.28 mL 5.5 6.0 6.5 7.0 7.5 8.0 8.5 9.0 9.5 10.0 10.5 pH 7.17 6.99 6.86 6.73 6.62 6.59 6.52 6.45 6.38 6.29 6.23 mL 11.0 11.5 12.0 12.5 13.0 13.5 14.0 14.5 15.0 15.5 16.0 pH 6.14 6.04 5.90 5.74 5.61 5.38 5.14 3.12 2.72 2.50 2.36 mL 16.5 17.0 17.5 18.0 18.5 19.0 19.5 20.0 20.5 21.0 21.5 pH 2.27 2.22 2.16 2.11 2.07 2.04 2.01 1.99 1.96 1.94 1.91 mL 22.0 22.5 23.0 23.5 24.0 24.5 25.0 25.5 pH 1.89 1.87 1.86 1.83 1.82 1.80 1.79 1.78

Computations: Classical Method: Trial 1 massNaHCO3 =[48.5 - (14.5 x 2)] mL HCl

       

= 865.68 mg NaHCO3
 

% NaHCO3 = = 39.35% NaHCO3

100%

mass Na2CO3 = (14.5 x 2) mL HCl

= 812.30 mg Na2CO3 % Na2CO3 = = 36.92% Na2CO3 Trial 2 massNaHCO3 = [48.0 - (14.5 x 2)] mL HCl
           

100%

= 843.49 mg NaHCO3
 

% NaHCO3 = = 38.34% NaHCO3

100%

mass Na2CO3 = (14.5 x 2) mL HCl

= 812.30 mg Na2CO3 % Na2CO3 = = 36.92% Na2CO3 Potentiometry: massNaHCO3 = [14.5 - (3.5 x 2)] mL HCl
           

100%

= 665.91 mg NaHCO3
 

% NaHCO3 = = 30.27% NaHCO3

100%

mass Na2CO3 = (3.5 x 2) mL HCl

= 392.15 mg Na2CO3 % Na2CO3 = = 17.82% Na2CO3

   

100%

Questions and Answers: 1. Prepare a titration curve from the data obtained in the experiment.

Titration Curve 12 10 8
pH 6

4 2 0 0.10 2.60 5.10 7.60 10.10

Volume of HCl

12.60

15.10

17.60

20.10

2. Why is the phenolphthalein chosen to be the indicator? Phenolphthalein is chosen to be the indicator because it is the most commonly used indicator and it is easy to see when it changes if the solution is clear. And sometimes it is the only indicator available in the school lab. 3. What is the role of buffers when a pH meter is standardized? Accurate pH measurements cannot be accomplished with a pH meter unless the meter has been calibrated against standardized buffer. Without a proper calibration the meter has no way to determine the pH value of the solution you are testing. 4. Illustrate and label the parts of a standard pH meter.

VI. Conclusion and Recommendations In this experiment, the amounts of carbonate and bicarbonate present in an unknown solid were calculated. A significant error in this experiment caused uncertainties to be yielded. This could have occurred during the procedure part of the experiment or by misreading the measurements taken in this experiment.

VII. Bibliography y y y y y y y y http://www.docstoc.com/docs/2375050/Analysis-of-a-Mixture-of-Carbonate-andBicarbonate http://www.ecs.umass.edu/cee/reckhow/courses/572/572bk16/572BK16.html http://en.wikipedia.org/wiki/Carbonate http://en.wikipedia.org/wiki/Bicarbonate http://answers.yahoo.com/question/index?qid=20060725193555AAWNTKR http://www.ehow.com/facts_6180086_important-its-electodes-againstbuffer_.html http://www.carlroth.com/media/_en-de/Graphics/00028942_0.jpg http://www.mcm.edu/~simpsong/Quant3.html