ANALYTICAL METHODS IN CHEMISTRY Objective :

1. To determine weight of water in a hydrated salt. 2. To determine end point in an acid-base titration. Part A : Use of Analytical Balance In Determining The Water Content Of A Given Hydrated Salt Introduction :

Balances are important laboratory equipments as they are used to determine the mass of materials. There are two types of balances used in laboratory which are two-decimal place balances and analytical balances. High accuracy is needed in certain experimental work such as material analysis or those involving small change in material mass. Unknown masses of materials are normally estimated with the use of two-decimal place balances, before they are determined accurately with analytical balances. As the analytical balance is very expensive and sensitive, adequate training has to be acquired by users so that they can use it correctly. Besides, the correct use and interpretation of measurements made with the balance is dependent on an understanding of the absolute precision with which samples can be weighed. In this experiment we will learn to use the balance properly and to evaluate the magnitude of various common errors encountered in weighing. Apparatus 1. 2. 3. 4. 5. 6. :

Evaporating dish Analytical balance Small test tubes Desiccators Thermometer Electrical heater :

Material

1. Sand 2. CuSO4 xH2O salt Procedure :

1. The pencil was weighted with two-decimal balance. Then, the pencil was reweighed using analytic balance. 2. A piece of 6cm2 size area was weighed accurately. Signature was put down on the paper and reweighed. 3. An electrical evaporating dish was filled with sand to about half-full. The electric heater was turned on and sand was heated slowly until the temperature reached 120 125 . 4. Small test tubes were heated in the hot sand for 10 minutes to dry them and then cooled down to room temperature.

5. When the test tube were cooled, they were weighed first with two-decimal balance and then with an analytical balance. The weights were recorded. 6. A test tube was filled with CuSO4 xH2O salt to about 0.5 cm depth. The weight was determined. 7. The test tube with CuSO4 xH2O salt was heated in the sand at 120 125 for about 30 minutes. Then, it was cooled in the desiccator to avoid the salt reabsorbing the moisture. 8. When it is cooled, the test tube was weighed. 9. Reheated for another 10 minutes, cooled it and reweighed when cooled. 10. The procedure was repeated until the weight was constant (less than 3/1000 for two readings). All the weights were recorded. Results : Materials 1. Pencil 2. 6 cm2 paper 3. 6 cm2 paper + Signature 4. Test tube 5. Test tube + CuSO4.xH2O. 6. Test tube + CuSO4.xH2O. after heat for 30 minutes. 7. Test tube + CuSO4.xH2O. reheat for another 10 minutes 8. Test tube + CuSO4.xH2O reheat for another 10 minutes 9. Test tube + CuSO4.xH2O. reheat for another 10 minutes 10. Test tube + CuSO4.xH2O. reheat for another 10 minutes 15.99g 15.9916g 16.01g 16.0127g 16.03g 16.0296g 16.09g 16.1037g 2 decimal balance 9.12 0.04 0.05 15.50g 16.30g 16.14g Analytical balance 9.1451 0.0434 0.0452 15.5180g 16.2613g 16.1475g

Discussion

The 2 types of the balances used in laboratory such as two-decimal place balances which digitally display a mass reading, in grams, to 2 decimal places as they are used to determine masses to 0.01 g while the analytical balances digitally display a mass reading, in grams, to 4 decimal places which are sensitive to 0.0001 g. Analytical balances is much more sensitive than the two-decimal place balances. This sensitivity of the laboratory balances makes it necessary to adhere to some strict rules or precaution steps to minimize the error when making measurements.

Water is present in many compounds especially inorganic salts. Hydrate is a chemical compound that contains a specific number of moles of water relative to each mole of the primary ionic solid. The number of moles of water present in the hydrate is a definite percent by mass. The water molecules are usually held loosely within the crystal. Since the water in a hydrated salt is loosely bound, therefore the water is easily removed by heating moderately of the hydrate. Hydrate salt + Heat Anhydrous Salt + Water

When water molecules are removed from the hydrate to yield the anhydrous form of the compound, a color change also occurs. In this experiment CuSO4.xH2O was used. Upon heating, dark blue CuSO4.xH2O is converted to a bluish white CuSO4 residue and water vapor. CuSO4.xH2O(s) + Heat CuSO4 (s) + xH2O (g) blue blunish white The percent by mass of water or the amount of water in an unknown hydrated salt can be determined in this experiment. The hydrated salt was weighed at first before heating, then the sample was heated to allow the water to volatilize. After heating, the dried sample was reweighed. The loss in weight corresponds to the water content. Certain anhydrous salts will gain waters of hydration easily by simple exposure to the atmosphere. In order to remove water completely and get the accurate result, the residues are then cooled in a desiccator. The desiccator is a metal container with a tight fitting lid and small amount of drying agent or desiccant inside to remove traces of water from an almost-dry sample. A desiccant is a compound that rapidly absorbs water from surrounding. Precaution steps : All balances are affected by vibrations of the bench top and by movement of air currents around the balance pan. These effects increase as the sensitivity of the balance increases. The balance pan of an analytical balance is housed in a closed chamber with doors. When using analytical balance to determine mass, it is necessary to close the balance doors to prevent external drafts from moving the balance pan. Besides, another source of error is vibration caused when objects are placed on the table on which the balance is located. Therefore do not lean on, rest hands or arms on or write lab reports on the balance table. Be sure the balance pan is clean. Do not place the chemical directly on the pan, use a weighing bottle, beaker, watch glass, etc. Corrosive liquids and solids are always placed in a vapor tight, pre-weighed container before weighing on an analytical balance. Conclusion :

Analytical balance is much more sensitive than the two-decimal place balances. The percent by mass of water or the amount of water in an unknown hydrated salt can be determined in this experiment by using the analytical balance. The weight of dried CuSO4 is 0.4736g and the weight of water in CuSO4.xH2O salt is 0.2697g. The ratio of no. of mole of H2O/no. of mole of CuSO4 = 5, hence the empirical formula of the salt is CuSO4.5H2O.

Reference

1. Introduction to the Analytical Measurements. Retrieved from http://www.chem.sc.edu/analytical/chem321L/labs/Expt1.pdf 2. Weighing with an Analytical Balance. Retrieved from

http://personal.monm.edu/asostarecz/CHEM225_S09/BalancesExpt1.pdf 3. Use of top-loading and Analytical balances: determination of the water of hydration of an ionic solid. Retrieved from http://www.usna.edu/ChemDept/plebeChem/manual/Ex2.pdf Questions :

1. Determine the weight of water in the salt and calculate the value x for the salt (CuSO4 xH2O). Weight of CuSO4 xH2O = 16.2613g - 15.5180g = 0.7433g Weight of CuSO4 = 15.9916g 15.5180g = 0.4736g Weight of water = 0.7433g 0.4736g = 0.2697g Number of mole CuSO4 = = = 2.9587 Number of mole H2O = = = 0.01498 mol mol

Mole ratio of CuSO4

= =1

Mole ratio of H2O

= = 5.06

The value of x

=5

2. A 15.00 g sample of an unstable hydrated salt Na2SO4 xH2O, was found to contain 7.05 g of water. Determine the empirical formula of the salt. Elements present (X)
Mass (X) Molar mass of (X) Number of mole of (X)

Na2SO4
7.95 g 142.1g

H2O
7.05 g 18.0g

= = 0.05596 mol

= = 0.3917 mol

Simplest mole ratio

= =1

= =6.999

The value of x

=7

The empirical formula Na2SO4.7 H2O Part B : The Use of Volumetric Flask, Burette And Pipette In Determining The Concentration Of NaOH Soluiton. Introduction :

Basic experimental work in sciences requires accurate and consistent data. Accurate data can only be obtained if you are able to use apparatus correctly. For example, volumetric analysis is a method of quantitative chemical analysis that always used in titration. In titration, the apparatus required are volumetric flask, burette and pipette. These apparatus have been calibrated to measure specific volume. Measuring cylinders are only used to measure rough volume of fluids. In this experiment you are trained to use apparatus for titration. Titrations are used to determine the concentration of acids or bases in solution. For example, a given volume of a solution of unknown acidity may be titrated with a base of known concentration until complete neutralization has occurred. Within the acid-base titration, there are four types of reactions, such as titration involving a strong acid and a strong base, titration involving a weak acid and a strong base, titration involving a strong acid and a weak base and titration involving a weak acid and a weak base. In titration, indicators are used to indicate the end point of the titration. Apparatus 1. 2. 3. 4. 5. 6. 7. :

500 cm3 Beaker 50 cm 3 Burette 20 cm3 or 25cm3 Pipette 200 cm3 volumetric flask Funnel Watch glass Erlenmeyer flask

Material

1. 0.5 M NaOH solution 2. 1.000 10-2 M HCl 3. Phenolphthalein solution Procedure :

1. Volumetric flask was cleaned and rinsed with distilled water. 2. 5 ml NaOH solution was transferred into volumetric flask using funnel and the remaining NaOH solution was washed into flask several times using distilled water. 3. The NaOH solution was topped up to 250 cm 3 with distilled water, the cap was closed and the flask was rotated several times to get a homogenous solution. 4. This solution was poured into a clean and dry beaker, labeled it, covered with a watch glass and put aside. The volumetric flask was cleaned. 5. The burette was cleaned with distilled water and rinsed with 5cm3 NaOH solution a few times. The burette was filled with NaOH solution using funnel. 6. The pipette was cleaned and rinsed a few times with acid to be used in titration. 7. Pipetted 20cm3 acid solution into three clean Erlenmeyer flask. 8. Two drops of phenolphthalein were added to the acid solution. 9. The initial burette reading was recorded and the acid was titrated with NaOH solution in the burette until end pointed was reached. The end reading to obtain the volume of acid used was recorded. 10. The titration was repeated several times until the acid volumes remained constant with 3/1000for three titrations, i.e.

Results

: Titration 1 1.10 20.70 19.60 Titration 2 20.70 40.20 19.50 Titration 3 11.20 30.80 19.60

Burette reading (cm3) Initial reading Final reading Volume of NaOH solution used

Average volume reading of NaOH solution used =

cm3

Volume of NaOH solution used (cm3) Titration 1 Titration 2 Titration 3 19.60 19.50 19.60 (within the range) (within the range) (within the range)

Discussion

An acid base titration is a procedure used quantitative chemical analysis to determine the concentration of either an acid or base. Strong acid- strong base titration was carried out in this experiment since strong acid, HCl and strong base, NaOH were used to for titration in this experiment.

The graph shown above is the pH against volume of the titration curve for the HCl-NaOH titration. Based on the graph, the pH has a low value at the beginning of the titration which shows the concentration of the HCl in conical flask. Near the equivalent point, the pH of the solution jumps from around 4.0 to 10.0 and the equivalent point is 7.0 because the NaCl formed is not hydrolysed. In titration, indicators are used to indicate the end point of the titration. The colour of the indicators change sharply at the end point and it happens on the addition of just one drop of acids and bases. At the end-point of the titration, all the acid has been neutralized by the alkali to produce only salts and water in the conical flask. A suitable indicator must be chosen so that the end-point coincides with the equivalence point of the two reacting solution. According to the graph, any acid-base indicator whose colour changes in the pH range from about 4.0 to 10.0 is suitable for HCl-NaOH titration. Phenolphthalein was the suitable acidbase indicator in this experiment as it is situated within the pH range of 8.3 to 10.0. Phenolphthalein is a weak acid.

colourless

pink

According to the Le Chteliers principle, in the presence of an acid, the eqilibrium is pushed to the left and the solution turns colourless. While decrease in acid in a solution shifts the equilibrium to the right, increasing the amount of In- and hence displaying pink colour. In general, if 90% or more of an indicator is in the form HIn, the solution will show the acid colour. If 90% or more is in the form In-, the solution takes on the base colour. If the concentrations of HIn and In- are about equal, the indicator is in the process of changing from one form to the other and has an intermediate colour which is the mixture of acid and base colour. Based on the result, the 3 titration carried out in this experiment were within the range ( Precaution steps : Firstly, for preparation a standard solution of the NaOH solution, the standard solution is prepared in a 250mL volumetric flask by adding 5mL of NaOH and distilled water should be added to the graduated line in the flask. During the adding of distilled water, water could have overshoot the line and cause the concentration of the standard solution to be different from the expected concentration. Thus, use dropper to fill the water into flask when the meniscus level approaches to the graduated line of the flask to avoid the overshooting of distilled water during the preparation of standard solution. After that, the NaOH is poured out to a beaker. Since NaOH solution will react quickly with the carbon dioxide in the air, therefore, NaOH should be covered by watch glass. Next for titration, make sure no air bubble is presented in the nozzle of the burette, Remove it if it is presented before taking the initial reading. Do not blow or shake the last remaining bit of liquid out of the pipette. Check to see that the water flows freely and that there are no leaks at the stopcock to prevent not leakage from the burette during titration. When reading a burette or pipette, the viewer's eyes must be at the level with the liquid surface to avoid parallax error. Always read lower meniscus in case of colourless solution and upper meniscus in case of coloured solutions. Often it is helpful to hold a white card or paper on it behind the burette to see the meniscus more clearly.Shaking of the titration flask should be continous during adding the solution from the burette. White tile should be placed at the bottom of the conical flask so that the changes of colour can be easily seen.Through careful control of the stopcock and rinsing, even partial drops of liquid can be added to the receiving flask. Always wear safety glasses and protective gloves and clothing while handling reagents as concentrated hydrochloric acid is corrosive and poison and avoid direct contact with NaOH as it is corrosive. Conclusion : The acid-base indicator that is used for the titration of HCl-NaOH is phenolphthalein which is situated within the pH range of 8.3 to 10.0 as the pH range of the titration of HCl-NaOH in this experiment is from 4.0 to 10.0. Titrations are used to determine the concentration of acids or bases in solution. By acid-base titration of HCl with NaOH, the initial concentration of NaOH solution is determined as 0.051M.

References : 1. How to use a Burette and Volumetric. Retrieved from Pipetteshttp://www.instruction.greenriver.edu/kmarr/Chem%20162/Chem162%20Lab s/How%20to%20use%20Volumetric%20Pipettes%20and%20Burets.htm 2. What is the precaution step of acid base titration? Retrieved from http://wiki.answers.com/Q/What_is_the_precaution_step_of_acid_base_titration 3. Acid- base indicators. Retrieved from http://www.chemguide.co.uk/physical/acidbaseeqia/indicators.html 4. Bobby Stanton, Lin Zhu, & Charles H. Atwood (2nd ed.). (2010). Experiments in General Chemistry Featuring MeasureNet. Belmont, CA: Brooks/Cole, Cengage Learning. Questions : 1. Calculate the concentration of NaOH solution. NaOH (aq) + HCl (aq) Volume of NaOH used Volume of HCl used Concentration of HCl No of moles HCl = = = 0.01 mole dm3 = Molarity Volume = 0.01 mole dm3 0.020 dm3 = 0.0002 mole NaCl (aq) + H2O (aq)

Based on equation, 1 mole of NaOH reacted with 1 mole of HCl. Hence, 0.0002 mole of NaOH reacted with 0.0002 mole of HCl. Molarity = = = 0.0102 M For dilution, M1V1 = M2V2 M1 (5) = (0.0102)(250) M1 = = 0.051M (Initial concentration of NaOH) (Concentration of diluted NaOH)

2. Distinguish between acid strength and acid concentration The strength of acids can be defined as the degree of dissociation and the dissociation constant. However, the degree of dissociation of an acid varies with concentration but the dissociation constant does not vary with concentration. Strength is how strong the bonds between the elements in the acid are. The stronger the bonds the harder it is for the hydrogen ions to dissociate from the acid which means strong acid dissociates completely in solution while weak acid dissociates only partly or not at all. For concentration of an acid, this is a measure of the moles of an acid that is dissolved in a litre of solution or concentration is a ratio of the amount of solute dissolved in a unit volume of solvent or solution. 3. Distinguish between a week base and an insoluble base. Weak base is a base which dissociates partially in aqueous solution. Weak base do not ionize completely in water. The compound which water insoluble and its acts as base is called as insoluble base such as various aromatic bases, metal oxide and metal hydroxide such as magnesium hydroxide, Mg(OH)2. Consider the solubility equilibrium of magnesium hydroxide: Mg(OH)2 (s) Mg2+ (aq) + 2OH- (aq) By adding H+ ions (decreasing the pH) shifts the equilibrium from left to right, and the solubility of Mg(OH)2 increases. Thus, insoluble bases tend to dissolve in acidic solutions. Similarly, insoluble acids dissolve in basic solutions.