A. TITLE Acidi -Alkalimetry B. DATE OF EXPERIMENT Tuesday, 22nd November 2011, at 07.30 am C.

FINISH OF EXPERIMENT Tuesday, 22nd November 2011, at 11.30 am D. OBJECTIVES 1. Making and determine standarization of base solution. 2. Determine precentage of H2SO4 in accu zuur. E. BASIC THEORY Titration is a procedure used to determine the amount of reactant present in a chemical solution; it is used to cause a reaction in such a way that the reactant is not in excess. The kinds of titration : 1. Acid base titration 2. Redox titration 3. Complex formation titration 4. Precipitation titration Use an indicators in titration This method relies on observing a color change in the solution. Indicators are weak organic acids or bases that are different colors in their dissociated and undissociated states. Because they are used in low concentrations, indicators do not appreciably alter the equivalence point of a titration. The point at which the indicator changes color is called the end point. Table of Commen Acid-Basa Indicators Indicator Thymol Blue Pentamethoxy red pH range 1.2-2.8 1.2-2.3 Quantity per 10 mL 1-2 drops 0.1% soln. in aq 1 drop 0.1% soln. in 70% alc. Tropeolin OO 1.3-3.2 1 drop 1% aq. soln. Acid red redviolet red Base yellow Colorles s Yellow

2,4-Dinitrophenol

2.4-4.0

1-2 drops 0.1% soln. in 50% alc.

colorles s red

Yellow

Methyl yellow

2.9-4.0 1

1 drop 0.1% soln. in 90% alc.

Red

Methyl orange

3.1-4.4

1 drop 0.1% aq. soln. red orange

red

orange

Bromphenol blue

3.0-4.6

1 drop 0.1% aq. soln.

yellow

blueviolet

Tetrabromphenol blue p-Nitrophenol

3.0-4.6

1 drop 0.1% aq. soln.

yellow

blue

5.0-7.0

1-5 drops 0.1% aq. soln.

colorles s

yellow

Azolitmin Phenol red Neutral red

5.0-8.0 6.4-8.0 6.8-8.0

5 drops 0.5% aq. soln. 1 drop 0.1% aq. soln. 1 drop 0.1% soln. in 70% alc

red yellow red

yellow red yellow

Rosolic acid

6.8-8.0

1 drop 0.1% soln. in 90% alc

yellow

red

Cresol red Naphtholphthalein Tropeolin OOO Thymol blue Phenolphthalein -Naphtholbenzein

7.2-8.8 7.3-8.7

1 drop 0.1% aq. soln. 1-5 drops 0.1% soln. in 70% alc.

yellow rose

red Green

7.6-8.9 8.0-9.6 8.0-10.0

1 drop 0.1% aq. soln. 1-5 drops 0.1% aq. soln. 1-5 drops 0.1% soln. in 70% alc.

yellow yellow colorles s yellow

rose-red Blue Red

9.0-11.0

1-5 drops 0.1% soln. in 90% alc.

Blue

Thymolphthalein

9.4-10.6

1 drop 0.1% soln. in 90% alc.

colorles s blue

Blue

Nile blue

10.111.1

1 drop 0.1% aq. soln.

red

Alizarin yellow

10.012.0

1 drop 0.1% aq. soln.

yellow

Lilac

Salicyl yellow

10.012.0

1-5 drops 0.1% soln. in 90% alc. 1 drop 0.1% aq. soln.

yellow

orangebrown

Diazo violet

10.112.0

yellow

Violet

Tropeolin O

11.013.0

1 drop 0.1% aq. soln.

yellow

orangebrown

Nitramine

11.013.0

1-2 drops 0.1% soln in 70% alc. 1 drop 0.1% aq. soln.

colorles s blue

orangebrown violetpink

Poirrier's blue

11.013.0

Trinitrobenzoic acid

12.013.4

1 drop 0.1% aq. soln.

colorles s

orangered

Titrimetric analysis or volumetric analysis is a quantitative analysis by reaction of a substance to be analyzed with standard solution (standard) which has been accurately known concentration, and reaction between the substance being analyzed and the standard solution took place quantitatively. One of the main group in the classification of titrimetric analysis is the neutralization reaction or acidimetry and alkalimetry. Alkalimetri acidi method used to determine the concentration of acid or base number is not known. Acidimetry a titration technique with acid as titrant, while alkalimetry a titration with a base as the titrant (Christian 1994). Experiment of acididi-alkalimetry aims is to determine the concentration of acid or base titrat with previously standardized base or acid used as titrat. Substances used in the titrimetric must have high purity. So before use, reagent concentration and volume must be known precisely by means of standardization (Harjadi 1986). Standardization is the process by which the concentration of a solution is accurately. The solution that can use for standardization process called primary standard. Primary standard should have the following characteristics:

1. It should be readily available in a pure form or in state of known purity at a reasonable cost. In general, the total amount of impurities should not exceed 0,01 to 0.02%, and it should be possible to test for impurities by qualitative tests of known sensitivity. 2. The substance should be stable. It should be easy to dry and should not be so hygroscopic that it takes up water during weighing. It should not lose weight on exposure to air. Salt hydrates are not normally employed as primary standards. 3. It is desirable that the primary standard have a reasonably high equivalent weight in order to minimize the consequences of errors in weighing. (Underwood ) The formula is V1 x N1 = V2 x N2 Where: V1 = Volume of penetration solution (ml) N1 = Normality of penetration solution (gram equivalents / liter) V2 = volume of titrated solution (ml) N2 = Normality of titrated solution (gram equivalents / liter) End Point titration indicated by the color change indicator, equivalent point occurs at the trajectory (range) pH indicator. the stoichiometry, acid or hydrogen ions and base hydroxide ions tepat habis bereaksi at the equivalence point. H+ + OH- H2O Acid equivalence = Base equivalence

Phenolphthalein and Methyl Orange Indicators The well-known indicator phenolphthalein (below) is a diprotic acid and is colorless. It dissociates first to a colorless form and then, on losing the second proton, to an ion with a conjugated system; a red color result.

Methyl orange, another widely used indicator, is a base and is yellow in the molecular form. Addition of a proton gives a cation which is pink in color.

Calculation of Percent Purity To analyze a sample of unknown purity the analyst weighs accurately a portion of the sample, dissolves it appropriately, and titrates it with a standard solution. If the titration reaction is aA + Tt product Where a molecules of the analyte, A, react with t molecules of the titrant, T, then at the equivalence point t mmol A = a mmol T mmol A = x mmol T

If V and M represent the volume (mL) and molarity (mmol/mL), respectively, of the titrant, and MWA is the molecular weight of the analyte, then mmol A = mg A = The precent by weight of A is %A= %A=
( )

xVxM x V x M x MWA

x 100
( ) ( ( ) )

F. CHEMICALS AND EQUIPMENT Chemicals: 1. H2C2O4.2H20 : 0,6008 g 2. Accu Zuur 3. NaOH 4. Phenolphthalein indicators 5. Methyl orange 6. Aquadest Equipment: 1. 2. 3. 4. 5. 6. 7. 8. 9. Volumetric Flask 100 mL Erlenmeyer 100 mL Graduated Cylinder 10 mL Stative Burette Volumetric Pipette Pipette Spatula Funnel

10. Beaker glass

G. PROCEDURE Standardization NaOH Solution 0,1 N With Oxalate Acid as Primary Standard.

0,6008 gram H2C2O4.2H2O Pouring into volumetric flask 100 ml Disolving with aquades and dilute untile boundaries Shaking well

Standard solution Pipettte 10 ml Pouring into conical flask Adding 25 ml aquades Adding 3 drops of PP indicator Titrate with NaOH solution Stop when the changes of indicators color Read and write the number at initial and end titration Determining volume NaOH Repeating until 3 times with the same volume of H2C2O4.2H2O Calculate average concentration of NaOH solution

Indicator change color

Determining percentage of H2SO4 in accu zuur 2 ml accu zuur Pouring into piknometer with volumetric pipette 2 ml Close the piknometer soon Weight again piknometer + accu zuur

Dencity of accu zuur

100 ml aquadest in volumetric flask Indicator change color Pouring accu zuur with the funnel Rinse the remnant Dilute until boundaries Let 1-2 our until reach the room temperature Pippete 10 ml solution Pouring into conical flask Adding drops of metil orange indicator Titrate with NaOH 0,1 M until there is color change Repeating until 3 times and calculate amount of H2SO4 in accu zuur

H. EXPERIMENT DATA Standardization NaOH Solution 0,1 N With Oxalate Acid as Basic Solution. No 1. 2. 3. Scale Initial (mL) End (mL) 0 8,8 8,8 17,8 17,9 26,9 Volume NaOH (ml) 8,8 9 9 N NaOH (eq/L) O,1084 0,1060 O,1060 Titrator Romadhoni Nurhalimah Istiana

Detemining percentage of H2SO4 in accu zuur No 1. 2. 3. Scale Initial (mL) End (mL) 33,3 49,3 31,2 48,9 16 30,8 Volume NaOH (ml) 16 17,7 14,8 % H2SO4 63,90 70,53 58,99 Titrator Nuurhalimah Istiana Romadhoni

I. ANALYSIS Standardization NaOH Solution 0,1 N With Oxalate Acid as Primary Standard. Before doing titration Washing burette with NaOH solution in order to make NaOH concentration is not changed by a drop of water that left. H2C2O4.2H2O solution is used as the primary standard solution because this solution is not hygroscopic, so it takes up water during weighing. And it has high equivalent weight, so minimize the consequences of error in weighing. In the standardization of NaOH solution, the addition of phenolphthalein indicators that serve to know the equivalent point titration. Phenolphthalein indicator is used because this standardization is a weak acid titration (H2C2O4.2H2O) and strong base (NaOH) so the equivalent point above 7 and in trajectory indicator of phenolphthalein is 8.0 to 9.6. Phenolphthalein indicator classified as weak acid, in condition not ionized this indicator is colorless. So when phenolphthalein indicator was added in H2C2O4.2H2O solution, there is no changes color. Phenolphthalein indicator in base condition given light color because of the anion. The reaction is: H2C2O4.2H2O (aq) + 2 NaOH (aq) Na2C2O4 (aq) + 4 H2O (l) In our experiment we get the normality of NaOH when the volume 8,8 mL is O,1084 eq/L. Calculation: m H2C2O4.2H2O = 0,6008 gram V = 0,1 L N= N = 0,0954 eq/L

V NaOH x N NaOH = V H2C2O4.2H2O x N H2C2O4.2H2O 0,0088 L x N NaOH = 0,01 L x 0,0954 eq/L N NaOH = 0,1084 eq/L

The normality of NaOH when the volume 9,0 mL is 0,1060 eq/L. V NaOH x N NaOH = V H2C2O4.2H2O x N H2C2O4.2H2O 0,009 L x N NaOH = 0,01 L x 0,0954 eq/L N NaOH = 0,1060 eq/L The normality of NaOH when the volume 9,0 mL is 0,1060 eq/L. V NaOH x N NaOH = V H2C2O4.2H2O x N H2C2O4.2H2O 0,009 L x N NaOH = 0,01 L x 0,0954 eq/L N NaOH = 0,1060 eq/L So the averege normality of NaOH is Average N NaOH = = 0,1068 eq/L Determining percentage of H2SO4 in accu zuur Determining H2SO4 solution in the accu zuur, addition of methyl orange indicator is to determines the equivalent point in the titration. Methyl orange is used because for titration H2SO4 with NaOH has a pH below 7 at the equivalent point and in trajectory methyl orange indicator is 3.1 to 4.4. Methyl orange is the sodium salt of a sulphonic acid. Anion in alkaline environment gives a yellow color. While in acid condition methyl orange is a weak base and containing H+ ions, there is a changes in the structure and gives the red color of the ions. The reaction is: H2SO4 (aq) + NaOH (aq) Na2SO4 (aq) + H2O (l) The mass of sample of H2SO4 is Dencity = = = 1,3132 g/mL mass of sample = 2 mL x 1,3132 g/mL = 2,6264 g The percentage H2SO4 when volume of NaOH 16 mL is 63,90%. V H2SO4 x N H2SO4 = V NaOH x N NaOH

0,01 L x N H2SO4

= 0,016 L x 0,1068 eq/L

N H2SO4 = 0,1709 eq/L In 100 ml = 2 x 100 x 0,1709 = 34,18 mmol mmol mg = = 34,18 x 49 = 1674,82 = 1,6748 g % H2SO4 = = 63,90 % The percentage H2SO4 when volume of NaOH 17,7 mL is 70,53 %. V H2SO4 x N H2SO4 = V NaOH x N NaOH 0,01 L x N H2SO4 N H2SO4 = 0,0177 L x 0,1068 eq/L = 0,1890 eq/L

In 100 ml = 2 x 100 x 0,1890 N = 37,80 mmol mmol = mg = 37,80 = 1852,2 = 1,8522 g

% H2SO4 = = 70,53 %

The percentage H2SO4 when volume of NaOH 14,8 mL is 58,99 %. V H2SO4 x N H2SO4 = V NaOH x N NaOH 0,01 L x N H2SO4 N H2SO4 = 0,0148 L x 0,1068 eq/L = 0,1581 eq/L

In 100 ml = 2 x 100 x 0,1581 N = 31,62 mmol mmol = mg = 31,62 = 1549,38 = 1,5494 g

% H2SO4 =

= 58,99 % So the averege percentage of H2SO4 is Average % H2SO4 = = 64,47 % The percentage of H2SO4 in accu zuur is 64,47%, but we dont know the percentage of H2SO4 certain. Because in our accu zuur that we use there is no label of compotition of accu zuur. J. DISCUSSION Application: Determining percentage of H2SO4 in Accu Zuur In the determining percentage of H2SO4 there is a factor that influence the data experiment: There are differences between volume of NaOH that use. In the first experiment we need NaOH 16 mL. In the second experiment we need NaOH 17,7 mL and in the third experiment, we need NaOH 14,8 mL. It caused by in the second

experiment, when we add NaOH solution in the analyte the volume is pass the equivalent point. In the first and second experiment we use NaOH in the bottle 2, but when we want to continue in the last titration, NaOH solution in bottle 2 is fresh out. So in a pinch we use NaOH solution in the bottle 3. K. CONCLUSION Based on our experiment normality average NaOH solution is 0,1068 eq/L Based on our experiment percentage of H2SO4 in accu zuur is 64,47% L. ANSWER OF QUESTION 1. Why in the manufacture of NaOH solution had to use hot water? Answer: The aim that have been boiling the water used is to avoid an explosion, because the reaction of alkali metal (Na) is exothermic and alkali metals are also easily react with water. 2. What's the difference between: Answer: a. Standard solution and primary solution?

Primary solution: where the solution concentration is known from the results of the weighing and dilution, the concentration is determined from the calculation Standard solution: where the solution concentration was determined with accuracy. b. Acidimetry and alkalimetri Acidimetry is a neutralization titration technique with acid as titrant. Alkalimetri is a neutralization titration with a base as the titrant. 3. Give reasons for the use of indicators in the titration of the above! Answer: Phenolphthalein indicator is used because this standardization is a weak acid titration (H2C2O4.2H2O) and strong base (NaOH) so the equivalent point above 7 and in trajectory indicator of phenolphthalein is 8.0 to 9.6. Methyl orange is used because for titration H2SO4 with NaOH has a pH below 7 at the equivalent point and in trajectory methyl orange indicator is 3.1 to 4.4. 4. 1.2 grams NaOH and Na2CO3 dissolve in sample and titrated with 0.5 N HCl with indicator pp. After addition of 30 mL of HCl solution became colorless. Then methyl orange indicator was added and titrated again with HCl. After addition of 5 mL of HCl solution became colorless. How much the percentage of Na2CO3 and NaOH in the sample? Answer: Known : Mass of NaOH Mass of Na2Co3 N of HCl V1 HCl V2 HCl Asked : % Na2CO3? % NaOH? Solution % Na2CO3 : 1,2 grams
: 1,2

grams

: 0,5 N : 30 mL : 5 mL

N Na2CO3 =

mgNa 2 CO3 1200mg x1 = = 2,8 N 84 BENa 2 CO3 .Vol x10 2

Equivalence of Na2CO3 = Equivalence HCl Equivalence of Na2CO3 = NHCl x VHCl = 2,8 N x 60 mL = 168 miliequivalence gram Na2CO3= equivalence x Equivalence Weight x 10 = 168 x 84 / 2 x 10 = 70560 mg Ratio of Na2CO3 =
70560 100 % 1,2 x10 3

= 58,8 %NaOH : NNaOH =

mgNaOH 1200mg x1 = =3N 40 BENaOH.Vol

1 x10

Equivalence NaOH = Equivalence HCl Equivalence NaOH = N x V = 3 N x 60 mL = 180 miliequivalence gram NaOH = Equivalence x equivalence Weight x 10 = 180 x 40 / 1 x 10 = 72000 mg

Ratio NaOH =

72000 100 % 1,2 x10 3

= 60 % 4. At which pH can color changes of pp indicators? At Ph of 8,0-9,6 M. REFERENCES Day,R.A.,Underwood,A.L.(1991).Quantitative Analysis (Sixth ed).New York: Prentice Hall. Tim Penyusun.(2011).Panduan Praktikum Kimia Analitik 1 Dasar-dasar Kimia Analitik.Surabaya:Jurusan Kimia FMIPA UNESA. http://chemistry.about.com/od/acidsbases/a/aa082304a.htm.Access November 2011, at 06.30 pm http://chemistry.about.com/od/acidsbases/a/Acid-Base-Indicators.htm.Access 25nd November 2011, at 06.30 pm at at 25nd

ATTACHMENT Standardization NaOH Solution 0,1 N With Oxalate Acid as Primary Standard Picture Before titration H2C2O4.2H2O + Phenolphthalein Indicator After Titration Result experiment 1 NaOH + H2C2O4.2H2O + Phenolphthalein Indicator Titarator Rhomadhoni

Result experiment 2 NaOH + H2C2O4.2H2O + Phenolphthalein Indicator

Nurhalimah

Result experiment 3 NaOH + H2C2O4.2H2O + Phenolphthalein Indicator

Istiana Yuli Purwati

Determining Percentage of H2SO4 in Accu Zuur Picture Before titration After Titration Result experiment 1 H2SO4 + Methyl Orange Indicator + NaOH Titarator Nurhalima h

H2SO4 + Methyl Orange Indicator

Result experiment 2 H2SO4 + Methyl Orange Indicator + NaOH

Istiana Yuli Purwati

Result experiment 3 H2SO4 + Methyl Orange Indicator + NaOH

Rhomadhoni