CBB 4032 CHEMICAL ANALYSIS GRAVIMETRIC ANALYSIS OF A CHLORIDE SALT

Group E3
Rosli bin Mhm Said Yanisa Klinsamorn Zaza Syamimi binti Zahari Zulhafeez bin Zapar 14680 12937 13435 13439

Date of experiment: 14 June 2013

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OBJECTIVE

Gravimetric analysis is another method in analytical chemistry that uses to determine the amount of constituent in a sample. In general, Gravimetric analysis is a measurement of mass. In this experiment, we use a precipitation method in order to analyze the constituent. The precipitation involves isolation of an ion in solution by a precipitation reaction, filtering, washing the precipitate free of contaminants, conversion of the precipitate to a product of known composition. In this experiment, the solution sample containing chloride ions is given to every group. To determine the amount of chloride ion, the solution is reacted with silver ion in which it will form silver chloride precipitate in the sample. The silver chloride precipitate is then removed from the solution by filtration process. The expected outcome from this experiment is student should be able to: 1. Calculate the percentage yield of a product 2. Calculate the standard deviation for the percentage yield of a product 3. Carry out the gravimetric experiment confidently

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STEP-BY-STEP PROCEDURE A. Mass by subtraction: 1. An unknown sample is weighed on a top loading balance by using a weighing paper. The mass is recorded. 2. An empty paper is weighed .The mass is recorded. 3. The sample is transferred from the weighing paper into the beaker for further reaction. B. Precipitation: 1. 75 mL of distilled water and 1 mL of 6 M HNO3 are added to the beaker. The beaker is labeled as #1. 2. The steps above are repeated with sample numbers 2 and 3 with the beaker labeled as #2 and #3 respectively. 3. Each of the solutions is stirred with three different glass stirring rods until the entire sample has dissolved. The stirring rods are left in respective beakers. 4. While stirring the solution, 30 mL of 0.125 M AgNO3 solution is added slowly in drops into the solution. Step 4 is repeated with sample 2 and 3. 5. Watch glasses are placed on the beakers and the beakers together with the watch glass are covered with foil to protect them from sunlight. 6. The solutions are warmed gently on the hot plate. The solutions are kept warm for approximately 30 minutes. C. Filtration: 1. Three of filter papers are obtained and folded. The papers folded as per appendix and then torn before it weighed accurately. 2. The paper is fitted into a glass funnel with one side has one piece and the other side has three pieces. 3. The paper is wet with distilled water to hold it in place in the funnel. 4. The precipitate and all the warm solution are transferred completely and quantitatively from the beaker onto the filter and the last traces of precipitate are washed out. 5. The level of solution in the filter funnel is observed to be below the top edge of the filter paper. 6. Finally, three 5 mL portions of acetone are carefully poured through the filter. 7. The filter papers are removed and placed on a numbered watch glass. Then, it is stored in locker until the next period. 8. The above processes are repeated with the other two samples. 9. Next, when the AgCl is thoroughly dried, the filter papers with the AgCl are weighed and the mass of AgCl is calculated. From these data, the parameters below are calculated:

i. ii. iii.

Mass of chloride in original sample, Percentage of chloride in the original sample, Average percent chloride, standard deviation and relative standard deviation.

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SCHEMATIC DIAGRAM OF APPARATUS / EQUIPMENT SETUP

The apparatus involve in this experiment are a weighing scale, beaker, stirring rod, a hot plate and filter papers. The equipment setup for this experiment, begin with the weighing the unknown compound in which contains chloride ions. Put the weighed unknown compound in the beaker and add silver nitrate and nitric acid to dissolved compound. Next, aluminium foil is used to cover the whole beaker and put the beaker on the hot plate in order to heat the solution. Finally, the precipitate is filtered through filter paper. Below are the schematic diagram and the apparatus for this experiment.

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APPARATUS

Below are the list of apparatus used and their functions. No. Apparatus Functions To measure the weight of unknown compound and the weight of 1. Weighing Scale precipitation obtained in the filter paper after the reaction takes place. 2. 250 mL Beaker The unknown compound, solvent and silver nitrate are stirred and mixed well in the beaker. A stirring rod is needed to help dissolve the compound in the solvent quicker. To heat the chemical reaction using beaker. After silver chloride precipitation has been formed, the filter paper 5. Filter Paper is used to separate the precipitate from the solution to be measured. 6. Glass Funnel The filter paper is placed in the glass funnel to make the separation easier. The aluminium foil is used to wrap the whole beaker during the 7. Aluminium Foil reaction as the reaction itself is photosensitive and the Cl- ions might separate if it is exposed if the light existed. 8. Weighing Paper The weight of the compound is initially measured on a weighing paper. List of apparatus used and their functions 5.0 REAGENT AND CHEMICAL

3. 4.

Stirring Rod Hot Plate

These are the chemicals that have been used for this experiment: 1. 2. 3. 4. Unknown salt with ClSilver nitrate Nitric Acid Acetone (XCl) (AgNO3) (HNO3) (C3H6O)

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RESULTS AND CALCULATION

Mass of sample (g) Mass of filter paper (g) Mass of filter paper +AgCl (g) Mass of AgCl (g) Moles of ClMass of Cl- (g) % of Cl- (%) Average % of ClStandard Deviation Calculation for Trial 1: Ag+ + ClAgCl(s)

Trial 1 0.2 1.48 1.94 0.46 0.0032 0.1134 56.7

Trial 2 0.2 1.58 1.98 0.4 0.0028 0.0989 49.47 53.71 3.772

Trial 3 0.2 1.58 2.02 0.44 0.0031 0.1099 54.95

100 mL of distilled water was used to dissolve 0.17g of unknown and 0.46g of AgCl was formed after drying. Given that molecular mass for AgCl = 143.32 g/mol Thus, no of moles AgCl = (0.46g) / (143.32 g/mol) = 0.0032 mol From the stoichiometric equation, it showed that 1 mol of Cl- reacts will 1 mol Ag+ to form 1 mol of AgCl. In order to form 0.0032 mol of AgCl, the same amount of mole is required. Thus, 0.0032 mol Cl- is required for the reaction. Formula mass of Cl- = 35.45 g/mol Mass of Cl- = 0.0032 mol x 35.45 g/mol = 0.1134 g Percentage of Cl- = (0.1134 g Cl-) / (0.2 g unknown sample) x 100% = 56.7% The same procedure is repeated for Trial 2 and 3.

Average of Cl- :

Calculation of standard deviation: Xi 56.7 49.47 54.95 53.71 (Xi - X) 2.99 -4.24 1.24 Sum (Xi - X)^2 8.9401 17.9776 1.5376 28.4553

Trial 1 Trial 2 Trial 3 Mean

= 28.4553

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DISCUSSION

Gravimetric analysis is one of the most accurate and precise methods of macro-quantitative analysis. In this experiment, a chloride salt that is silver chloride, AgCl, is produced through several steps in the gravimetry analysis. The salt is obtained through the reaction between a chloride solution mixed with silver nitrate, AgNO3 solution. The steps needed in a gravimetric analysis are preparation of the solution, precipitation, filtration and washing, drying, weighing, and calculation. Three solutions of chloride were prepared during the experiment. This was needed in order to make the averaging of the calculations later and reduce the percentage error while weighing the final amount of the salt, thus increasing the results accuracy. The chloride solution was then added with AgNO3 solution and the precipitation occurred. However, the solution was heated to aid increase the solubility of AgNO3 in the chloride solution and providing an even precipitation with high rate of precipitate formed. In addition, great care was taken in handling

the mixture of chloride and AgNO3 since AgCl produced easily decomposes in the presence of light due to its photosensitive nature. Hence, the beaker containing the solution was wrapped with the aluminium foil while it was being heated. The solution was then filtrated for the precipitate to be collected for weighing. Washing was also needed to retrieve any remaining precipitate in the beaker holding the precipitate. A test was conducted to determine whether the washing was complete or not using several drops of the AgNO3 solution. The solution was added into the clear filtrate and if the filtrate turned cloudy, it had to be re-filtered. Acetone was used to wash the filter in the final step of washing. Next, the wet precipitate would be dried using the oven to remove the remaining water and absorbed electrolyte from the wash liquid. The final step would be calculation of the weight of the target analyte that was AgCl. From the calculation, the average amount of chloride ions in the chloride solution was 53.71 %. Using the three trials conducted during the experiment, the standard deviation for the experiment was calculated, giving the value of 3.772. The small value of standard deviation proved that the experiment was nearly accurate but the accuracy could be improved by improving the errors involved in the steps, either in random or systematic error.

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ERROR ANALYSIS AND RECOMMENDATION

Random error involved the unforeseen errors that could happen during an experiment, involving the mistakes caused by the person conducting the experiment or human error. In this experiment, random error might have happened when measuring the volume of AgNO3 solution and preparing the chloride solution in the form of parallax error. Thus, averaging had been done to minimize the effect of this type of error. The systematic error might happen during the measuring of the weight of the precipitate due to the fluctuating value of the weighing scale. In this experiment, the time given for the precipitate to form crystals of AgCl was short and it will be better for the mixture of chloride solution and AgNO3 solution to be heated for a longer time in order for larger crystals of AgCl precipitate to form, resulting in more accurate weighing as more AgCl can be collected. In addition, the stirring process before the mixture is heated needs to be done thoroughly to facilitate the solubility and increase the reaction rate between the two solutions.

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CONCLUSION

Through this experiment, the constituents present in a sample of material are determined through analytical chemistry method specifically gravimetric analysis. For a given solution sample containing chloride ions, the method of determining the amount of chloride ion is through reaction with silver ion forming silver chloride precipitate in the sample. The silver chloride is then removed through filtration process. The main purpose of conducting this experiment is to get familiarize with the typical techniques that are used in gravimetric analysis by quantitatively determining the amount of chloride in an unknown solution.