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TABLE OF CONTENT

CONTENT Abstract / summary Introduction Aims / objectives Theory Apparatus Experimental procedure Result Sample error calculation Discussion Conclusion Recommendation References

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ABSTRACT / SUMMARY
By doing this experiment we can determine the concentration of acetic acid in vinegar. Vinegar is a dilute solution of acetic acid. The molarity and the percent by mass of acetic acid in a vinegar solution can be determined by using by titration process.

INTRODUCTION

Vinegar is a dilute solution of acetic acid. Since vinegar is an acid, it can be titrate with a base such as NaOH. A titration is a technique where a solution of known concentration is used to determine the concentration of an unknown solution. Some chemicals can be purchased in a pure form and remain pure over a long period of time other chemicals can be easily contaminated by the absorption of carbon dioxide or water from the air. Sodium hydroxide absorbs wetness from the air and usually appears wet. So that if a solution of sodium hydroxide is prepared by weighing the sodium hydroxide, the concentration of the solution may not be exactly the intended concentration. Besides that, potassium hydrogen phthalate has a lesser tendency to absorb water from the air and when dried will remain dry for a period of time. This means that carefully prepared solutions of known concentration of potassium hydrogen phthalate can be determined by using titration. The equation for the reaction of potassium hydrogen phthalate with sodium hydrogen is:

KCO2C6H4CO2H + NaOH KCO2C6H4CO2Na + H2O

The equivalence point of a titration occurs when chemically equivalent amounts of acid and base are present. At this point the pH changes rapidly with a small addition of acid or base. Once the equivalence point of the titration is known, the concentration of the sodium hydroxide can be determined. The sodium hydroxide is then used to titrate vinegar, and the concentration of the vinegar is determined. The percent acetic acid can be determined from the concentration of the vinegar.

AIM / OBJECTIVES

The purpose of this experiment is to determine the percentage of acetic acid in a vinegar sample by the method of standardization of a sodium hydroxide solution. The concentration of acetic acid also can be determined.

THEORY

In this experiment, the concentration of acetic acid in vinegar can be determined by using titration. A titration is a technique where a solution of known concentration is used to determine the concentration of an unknown solution. Typically, the titrant (the know solution) is added from a burette to a known quantity of the analyte (the unknown solution) until the reaction is complete. Knowing the volume of titrate added allows the determination of the concentration of the unknown. Usually, the indicator is used to give the signal for the end of the reaction, which is known as end point.

The method used to measure the total acidity of the vinegar by using an acid-base titration. For an acid-base titration, the chemical reaction in generally known as :

acid + base water + salt

and for the titration of the vinegar in this experiment the following reaction will be used to determine the acetic acid satisfied of the vinegar sample:

HC2H3O2(aq) + NaOH(aq) H2O(l) + NaC2H3O2(aq)

the sodium hydroxide will be the standard reactant solution for this titration, and acetic acid the calculated unknown reactant.

The other important concept in this experiment is concentration. Concentration is meant that the composition of a solution and can be expressed as the ratio of solute/solvent or solute/solution. The two unit of concentration expressing the ratio are :

Molarity(M) = moles of solute/volume of solution in litre and The percentage by mass = (mass of solute/mass of solution) x 100%

In this experiment, in order to standardize the NaOH solution, potassium hydrogen phthalate, KHP solution will be titrate with 0.6M NaOH solution. While the KHP stock solution must be prepared by dissolving 1.5 grams of KHP in 30mL of distilled water.

APPARATUS

1. pH metre 2. 0.6 M NaOH solution 3. Droppers 4. Buffer pH 7 and 10 5. Vinegar 6. Stirrer and Stir bar 7. Burette 8. Beaker(100mL, 250mL) 9. Funnel 10. Scoopula 11. Burette clamp 12. Pipette 10mL 13. Analytical balance 14. Potassium hydrogen phthalate, KHP

PROCEDURE

Calibration Of pH Probe

1. The pH metre was plugged in and allows it to warm up for about 10 minutes. 2. The temperature knob should be set between 20C and 25C. 3. The electrode was placed in pH 7 buffer, turned the knob to pH, and the pH was adjusted to 7.00 with the standardization knob. 4. The instrument was placed on standby. The electrode was rinsed and blotted. 5. The electrode was placed in pH 10.00 buffer, turned the knob to pH and the pH was adjusted to 10.00 with the slobe knob. 6. The instrument was placed on standby. The electrode was rinsed and blotted.

Titration

1. The burette was rinsed with 5mL of NaOH solution. 2. The burette was rinsed and filled past the 0mL mark with NaOH solution. 3. Some of the NaOH was drained through the tip into a waste beaker to fill the tip and bring the level of NaOH to exactly 0.00mL. If the 0.00mL mark is passed, a dropper was used to bring the meniscus to 0.00mL. 4. About 1.5 grams of potassium hydrogen phthalate was weighed. The exact mass of the potassium hydrogen phthalate was recorded. 5. The potassium hydrogen phthalate was placed in a beaker. 6. 30mL of distilled water was added and the potassium hydrogen phthalate was dissolved. 7. The magnetic stirrer was placed so that the burette and pH electrode may both be placed in the 250mL beaker when it is on the stirrer. 8. The beaker was placed on the stirrer and the stirring bar. The electrode was placed so that the bulb is in the solution but above the stirrer bar. More distilled water was added if necessary. 9. The initial pH for 0.00mL of NaOH added was recorded. 10. NaOH was added until the pH has increased by 0.2 pH units. 11. The pH and the burette reading were recorded to two decimal places.

12. The step 10-11 was repeated until a pH of 12 is obtained. 13. The procedure for other trials as instructed was repeated. 14. The graph pH (y-axis) vs. volume of NaOH (x-axis) was plotted.

Determination The Percentage Acetic Acid in Vinegar

1. A clean 250mL beaker was placed on the balance and tare. 2. 10mL of vinegar was placed exactly by using a pipette in 250mL beaker. The mass of vinegar was recorded. 3. 75mL to 100mL of distilled water was added. 4. The burette was refilled to 0.00mL. 5. The magnetic stirrer was placed so that the burette and pH electrode may both be placed in the 250mL beaker when it is on the stirrer. 6. The beaker was placed on the stirrer and the stirring bar was added. The electrode was placed so that the bulb is in the solution but above the stir bar. 7. The initial pH for 0.00mL of NaOH added was placed. 8. NaOH was added until the pH has increased by 0.2 pH units. 9. The pH and the burette reading were recorded to two decimal places. 10. The step 7-8 was repeated until pH 12 is obtained. 11. The procedure was repeated. 12. The graph pH (y-axis) vs. volume of NaOH (x-axis) was plotted.

Data Table:
Part 1:

Mass of potassium acid phthalate used: 1.503 g Trial number: 1

Vol. NaOH 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18

pH 3.98 4.16 4.32 4.47 4.61 4.75 4.86 5.01 5.14 5.31 5.48 5.76 6.39 11.56 11.96 12.14 12.26 12.36 12.39

Mass of potassium acid phthalate use: 1.470 g

Trial number 2 Vol. NaOH 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 pH 4.00 4.22 4.41 4.56 4.69 4.82 4.95 5.08 5.21 5.37 5.56 5.88 6.86 11.80 12.10 12.24 12.33 12.39 12.45

Data Table:

Part 2:

Mass of vinegar: 10 g Trial number 1 Vol. NaOH 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 PH 2.660 3.220 3.530 3.770 3.920 3.160 4.190 4.280 4.390 4.490 4.590 4.690 4.780 4.850 4.950 5.010 5.120 5.210 5.320 5.410 Vol. NaOH 20 21 22 23 24 25 26 27 pH 5.520 5.650 6.800 7.020 11.040 11.440 11.650 11.760

Mass in vinegar : 10 g

Trial num 2

Vol. NaOH 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19

PH 2.740 3.250 3.520 3.730 3.870 3.980 4.080 4.190 4.280 4.350 4.420 4.500 4.570 4.630 4.690 4.750 4.890 4.990 5.100 5.210

Vol. NaOH 20 21 22 23 24 25 26 27

pH 5.360 5.560 5.900 7.010 11.210 11.440 11.61 11.72

1) Graph of pH(y) vs volume Of NaOH(x) [standardization of NaOH] TRIAL 1

14

12

10

8
Ph Value

0 0 2 4 6 8 10 12 14 16

2) Graph of pH(y) vs volume of NaOH(x) [standardization of NaOH] TRIAL 2

14

12

10

8
Ph Value

0 0 2 4 6 8 10 12 14 16

3) Graph of pH(y) vs volume of NaOH(x) [determination of concentration of acetic acid in vinegar] TRIAL 1
14

12

10

8
pH

0 0 5 10 15 20 25 30

4) Graph of pH(y) vs volume of NaOH(x) [determination of concentration of acetic acid in vinegar] TRIAL 2

14

12

10

8
pH

0 0 5 10 15 20 25 30

SAMPLE CALCULATIONS
PART 1 1) The volume of NaOH required to neutralize the KHP : M1V1 =M2V2

(1M) V1 = (0.6M) (150mL) V1 1L = 90mL = 40g

1000mL= 40g 90mL = ? Therefore, 3.6g of NaOH is required to prepare 0.6M NaOH stock solution.

2) From the graph 1 and 2 for experiment standardization of NaoH, 11.125mL of NaOH is required to neutralize the KHP solution.

3) The molarity of KHP for the titrations (TRIAL 1) : number of moles of KHP= 1.503g / 204.2 g per mole = 7.3604 x 10 -3 mole KHP molarity of KHP = number of moles / volume of solution = 7.3604 x 10 -3 mole KHP / 0.03L = 0.2453 M KHP

4) The molarity of KHP for the titrations (TRIAL 2) : number of moles of KHP= 1.470g / 204.2g per mole = 7.1988 x 10 -3 mole KHP molarity of KHP = number of moles / volume of solution = 7.1988 x 10 -3 mole KHP / 0.03L = 0.2310 M KHP

5) Average molarity of sodium hydroxide solution : TRIAL 1; 1.503g of KHP was weighted out and titrated to an end point with 11.56mL of NaOH solution that was approximately 0.6M. The exactly concentration of NaOH titrate is = 1.503g / 204.2 g per mole = 7.3604 x 10 -3 mole KHP At the end point: 7.3604 x 10 -3 mole KHP = 7.3604 x 10 -3 mole NaOH titrated. 7.3604 x 10 -3 mole NaOH / 0.01156L NaOH titrated = 0.6367 M NaOH

TRIAL 2; 1.470g of KHP was weighted out and titrated to an end point with 11.80mL of NaOH solution that was approximately 0.6M. The exactly concentration of NaOH titrate is = 1.470 g / 204.2 g per mole = 7.1988 x 10 -3 mole KHP At the end point : 7.1988 x 10 -3 mole KHP = 7.1988 x 10 -3 mole NaOH titrated. 7.1988 x 10 -3 mole NaOH / 0.01180L NaOH titrated = 0.6101 M NaOH AVERAGE; (0.6367 M NaOH + 0.6101 M NaOH ) / 2 = 0.6234 M NaOH

PART 2 1) From the graph of pH versus NaOH added, there are 13.00mL of NaOH required to neutralize the vinegar in trial 1, and 13.00mL of naOH required to neutralize the vinegar in trial 2. 2) For trial 1, 10mL aliquot of vinegar requires 13.00mL of 0.6234 M standardized NaOH solution to reach the equivalence point of the titration. Assumes the density of the vinegar solution is 1.00g/mL HC2H3O2(aq) + NaOH(aq) H2O(l) + NaC2H3O2(aq)

The moles of NaOH that reacted; = Molarity x Volume(L) = 0.6234M x 0.0130L = 8.1042 x 10 -3 mol of NaOH 3) The moles of acetic acid neutralized by the moles of NaOH; At the end point, 8.1042 x 10 moles of acetic acid. 4) The molarity of acetic acid concentration 10mL acetic acid x (1L / 1000mL) = 0.010 L acetic acid concentration. Molarity = mole of acetic acid/ volume of solution =8.1042 x 10 -3 mole/0.010L =0.81042M acetic acid
-3

moles of NaOH is equal to 8.1042 x 10

-3

5) Mass of acetic acid : Moles of acetic acid x molecular mass of acetic acid = 8.1042 x 10 -3 mole x 60.06g/mole = 0.4867g of acetic acid 6) Mass of acetic acid solution : 10mL acetic acid solution x (1g acetic acid solution / 1mL acetic acid) 10.00 g acetic acid solution

DISCUSSION

In this experiment, the concentration of acetic acid in vinegar can be determined by using titration process. A titration is a method for determining the concentration of a solution and the purpose of the titration is to determine the equivalence point of the reaction. The equivalence point is reach when the added quantity of one reactant is the exact amount necessary for the stoichiometric reaction with the other reactant. Thus the concentration of an acid could be determined. The concentration of a base could be determined. The concentration of a sodium hydroxide solution will be determined (it will be standardized). The standardized sodium hydroxide solution will be used to titrate vinegar for determination of the concentration of acetic acid. In this experiment, we can learn the basic concept related with titration. Other than that, we also can learn all the techniques used in titration process. By doing this experiment, we also can obtain the titration data thus to perform the titration calculation. Besides, we can standardize a base, in this experiment which is NaOH. Other than that, we can determine the molarity of the acetc acid in vinegar.

As we know, potassium hydrogen phthalate, KHP is a weak acid. In order to standardize the potassium hydrogen phthalate, it will simply react with NaOH which is a base as shown below :

Next, in order to determine the acetic acid in vinegar, acetic acid will be reacted with sodium bydroxide as shown in the equation below : CH3COOH (aq) + NaOH (aq) --> CH3COONa (aq) + H2O (l) The mole ratio of acetic acid to sodium hydroxide is one-to-one. The standardized base will be added to a measured volume of vinegar. The moles of base can be determined using the volume of sodium hydroxide delivered to reach the endpoint and the molarity of the sodium hydroxide. The moles of acetic acid can be determined from the moles of sodium hydroxide and the balanced chemical reaction. The molarity of acetic acid can be determined from the moles of acid and the volume of vinegar.

volume and molarity of NaOH -> moles NaOH -> moles acetic acid -> molarity acetic acid. To determine the molarity of a solution and the percentage by mass of the acetic acid in vinegar by titration of a vinegar sample with a standardize sodium hydroxide solution, we are required to prepare 150mL with 0.6M NaOH stock solution. But in order to get the standardize sodium hydroxide solution, we have to prepare the potassium hydrogen phthalate,KHP by titration with 0.6M NaOH solution that had been prepared before. And the KHP stock solution can be prepared by dissolving 1.5grams of KHP in 30mL of distilled water. In this experiment, we have to do the titration at many times in order to get the most accurate reading to perform the best result needed. So that, while doing the titration, we have to concern about the precaution steps of titration. We have to handle those laboratory equipments carefully. The reading must be recorded with the meniscus reading to prevent the parallax error. Sometimes, theyre some misreading the volume which at any moment, and due to whatever reason. This can be for example a parallax problem, when someone reads the volume looking at an angle, or error in counting unmarked graduation marks. When reading the volume on the burette scale is not uncommon to read both upper and lower value in different lighting conditions, which can make a difference. Other than that, we also have to use much kind of chemical reagents like acid and base. As we know, all the laboratory activity must be handled carefully so that we are required to obey all the rules in laboratory area such as wear the laboratory coat, suitable

goggles, glove, and more. Theyre too important because to protect our body from any incidence that might be happen in the laboratory area. Other than that, problem sometimes occurred when using the unrinsed apparatus. So that, those apparatus will not ready to use thus give the slightly different result with the suppose one. Besides, misreading of the volume of NaOH used when the titration process. So that it will affect the result.

CONCLUSION
At the end of this experiment, we can determine the concentration of acetic acid in vinegar and the percentage by mass of the acetic acid that contain in the vinegar. From the sample of calculation above, we know that the concentration of acetic acid in vinegar is

RECOMMENDATIONS
In this experiment, in order to get the accurate value the titration must be done at least two times. So that, the data we get from the observation can be compared thus the exact value can be determine and calculate. Other than that, to improve the result of the experiments, we can also use indicators such as phenolphthalein to know the end points besides than using the pH probe.

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