Experiment

“Volumetric Determination of an Unknown Chloride”

Abstract:

An unknown chloride will be analyzed volumetrically quantitatively in this experiment. It is

basically a method for measuring the volume of solutions and determining the Cl− percent by

weight of in a soluble salt. In this experiment, we use volumetric determination, a method of

quantitative analysis that is very important. this analysis is also known as titration. It is a very

common method used in the laboratory for the measurement of unknown analyte . This type

of analysis requires very simple instruments and offers other advantages, including

convenience, speed, and accuracy (within 0.1%), which makes it particularly suitable for

routine analysis and determining a large number of samples at once. Titrations include

complexometric, acid-base, precipitation, and redox tests. Mohr's Method is used to titrate by

precipitation in this experiment.

Introduction:

A volumetric analysis is typically faster and easier than a weight analysis. There are, however,

several conditions that must be met for them to be liable. There must be a single known reaction

when the solution is mixed in order to determine the quantitative relationship between the

reactants.  The second requirement is that the reaction must be fast. In the case of chemical

analysis, the reaction must essentially be completed during mixing two solutions. The last

requirement is that there must be a way to determine when the reactants are finished

reacting. Identifying the end point of a reaction is what we call determining the end point.

Titration is the mostly used procedure for the volumetric quantitative analysis. The titration

technique involves dispensing a reagent, called the titrant, into a flask that has contain a fixed
quantity of the second reagent from a burette. The addition of titrant is constant until the

second reagent is completely reacted with the titrant.

A solution's end point is usually visible as a distinct change in color. Indicators are typically

added to the titrated solution to cause color changes. Chemical substances that satisfy two

requirements can be used as indicators. In order to observe a color change, the reaction must

come to an end. The colour changes are sharp, any extra drop of titrant solution can be used

to detect the change in color.

Titration end points can be determined by measuring the volume of titrant used for reaching

the reaction end point along with the balanced reaction. From this, the amount of unknown

sample can be determined.    

An example of a typical titration analysis is shown in this experiment. By titrating a

chloride sample with silver nitrate, AgNO3, the Mohr method determines the percent

of Cl- in a salt.  A very low-solubility silver chloride is formed when the titrant and

sample react.    

                                                Ag+ (aq) + Cl-(aq) →  AgCl(s)

Due to its less solubility, the AgCl is assumed to undergo complete reaction. A rapid removal

of Ag+ from solution occurs during the titration process. The solution appears cloudy because

of the formation of AgCl, a white solid. A large amount of AgCl precipitates at the end of the

reaction.  As AgNO3 is added further, the solution becomes oversaturated with Ag+.  The

first excess of Ag+ indicates the end of the reaction. An excess of Ag+ is indicated by the red

precipitate Ag CrO (s), which forms when excess Ag+ is present.

2 Ag+ (aq) + CrO  2- (aq) → Ag2CrO4(s)
During titration, K2CrO4 is added as the chromate ion. When Ag2CrO4 is dissolved in

water at 25°C, it is ten times more soluble than AgCl. A solution of Ag2CrO4 contains

about the same solubility as AgCl at 0.0018 and 0.014 grams/liter, respectively. The

calculation of AgNO3 to a solution containing CrO42- and Cl- results in the precipitation of

AgCl.  Until Cl- is removed from the solution, the concentration of Ag+ cannot reach the

level that produces Ag2CrO4 precipitation. With further addition of titrant, the Ag+

concentration rises sharply with the chloride completely re-routed as AgCl. As the

concentration of Ag+ and CrO2-4 in the solution increases towards the end of the titration,

Ag2CrO4 precipitates.

A local excess of Ag+ can often lead to the formation of reddish Ag2CrO4 during

titration. Mixing the solution thoroughly re-dissolves it. As the precipitate begins to develop

a definite faint red color that does not fade with time, it indicates that the titration has

reached its end point.

In order to calculate the moles of AgNO3, it is necessary to know the molarity and volume of

AgNO3. As shown by equation (1), when Ag+ is reacted with Cl-, one mole of Ag+ is

generated. The moles, weight, and percentage of Cl- are calculated using the chloride atomic

weight and the sample's original weight.

Experiment

Our first step will be to prepare a 50mL burette and a solid chloride sample that is unknown.

In addition to the paper itself, the analytical balance should weigh a weighing paper

containing 0.1g of sample. The actual mass of the sample can be determined based on these

readings. It should be around 0.1g. After that, the sample will be transferred to an Erlenmeyer

flask. It is necessary to make three samples, which will be labeled as #1, #2, and #3, by
following the above steps. In each flask, add 50mL of distilled water to dissolve the samples

in water. A solution of 1M K2CrO4 should be added. A 250 mL beaker should be clean, dry,

and contain about 0.05M AgNO3. Next, it will be filled with the burette of AgNO3 after

thoroughly rinsing it twice in distilled water and once with AgNO3. Once the samples have

turned red, we will keep adding AgNO3 and swirling them until they have a creamy

consistency. Using the difference between the initial and final burette readings, we can calculate

the amount of AgNO3 used. in the last step measure the moles of AgNO3 that are used against

the moles of CL-.

Results:

Sample #1 Sample #2 Sample

#3

Weight of weighing paper + sample 0.516 g 0.507 g 0.511 g

Weight of weighing paper 0.909 g 0.405 g 0.404 g

Weight of sample to be titrated 0.107 g 0.108 g 0.107 g

Final burette reading 48 mL 40.20 mL 37.80 mL

Initial burette reading 0.50 mL 0.20 mL 0.80 mL

Volume of AgNO3 used 47.50 mL 90 mL 37 mL

Molarity of AgNO3 0.05 M

Moles of AgNO3 used 2.38 × 10-3 mol 1.00× 10-3 mol 1.50× 10-3 mol

Moles of Cl- titrated 2.380× 10-3 mol 2.00× 10-3 mol 1.85× 10-3 mol

Grams of Cl- titrated 0.084g 0.0704g 0.0656g

%Cl in unknown 66.2% 69.5% 66.5%

Average % Cl- 67.3%

Discussion and conclusion

The weights of 3 samples of unknown chloride salt are 0.107g, 0.108g, 0.107g. The volume

of AgNO3 solution used to titrated into 3 sample unknown sample are 47.5ml, 90ml and

37ml. The molarity of AgNO3 solution is 0.05M. So the moles of AgNO3 used to titrated

into 3 samples of unknown chloride salt solutions are 2.38 × 10-3mol, 1.00× 10-3mol and

1.50× 10-3 mol. The moles of Cl- in 3 samples of unknown chloride salt solutions are 2.380×

10-3 mol, 2.00× 10-3 mol and 1.85× 10-3 mol. The grams of Cl- in 3 samples of unknown

chloride salt solutions are 0.084g, 0.0704g and 0.0656g. The percentage of Cl- in 3 samples

of unknown chloride salt solutions are 66.2%, 69.5% and 66.5%, the average percentage of

chlorine is 67.3%

Titration end points are vital in the laboratory. A missed endpoint will result in incorrect

computations. In this case, pink is the right colour to use in order to obtain accurate results.

The indicator dichlorofluorescein facilitates the identification of the endpoint by providing

colour. In the lab, a few mistakes were made. As a first cause of inaccuracy, samples often

lose their mass while being recorded and removed from the analytical balance. As a result of

the sample being taken out of the balance, more sample was lost.

If the mass of the sample is incorrect, Ag+ and Cl- levels will change. To avoid making this

mistake, weigh the sample twice before starting the experiment. Secondly, some of the

solution leaked out of the flask after the distilled water was added. It appears that a

significant amount of solution was lost because the solutions became stuck in the beaker and

refused to transfer to the flask. In addition to having an impact on the moles of Ag+ and Cl-

in the sample, it affects the mass of the solution as well.