ADAMSON UNIVERSITY

College of Engineering

Chemical Engineering Department

Manila

FORMAL LABORATORY REPORT

ANALYTICAL CHEMISTRY

Experiment #5

DETERMINATION OF CARBONATES IN A MIXTURE: DOUBLE INDICATOR

TITRATION

Group # 12
Renta, Josef
Rogado, Jomar
Santos, Cherrylen

Wednesday | 7:00am -10:00am | 05028

Date Performed:
March 27, 2019

Engr. Eduardo O. Hernandez

Professor
ABSTRACT

The experiment is conducted to determine the amount of Carbonates formed using the

double indicator titration method. This method is used whenever there are two end points to a

titration. The indicator used here are the Phenolphthalein and the Bromocresol Green Indicator to

detect the end point of the titration, as opposed to the single indicator titration method or the normal

titration method where only Phenolphthalein was used. This form of titration involves a weak base

– strong acid titration. The primary standard used here is Na ₂CO₃ to standardize Hydrochloric

Acid (HCl). Two endpoints are made with the titration of Na ₂CO₃ where the first endpoint is the

conversion of Carbonate to Hydrogen Carbonate, while the second endpoint forms Carbonic Acid

and Carbon dioxide. From the volumes of the titrant in both endpoints, the constituents and its

concentration can be computed for both the Standardization of the HCl titrant in part C and the

analysis of the unknown sample in part D and also computing for the Mean, SD, and %RSD.

INTRODUCTION

Qualitative and quantitative determinations of the constituents in a solution containing

Na2CO3, NaHCO3 and NaOH alone or in a mixture provide an interesting example for

neutralization titrations. It is obvious that no more than two of these constituents can be present in

a solution together since the reaction between some of them eliminates the third one. Mixing of

NaOH with NaHCO3 results in the formation of Na2CO3 until one or the other (or both) of the

original reactants is used up.

NaOH + NaHCO3 → Na2CO3 + H2O

 Analysis of such mixtures requires the use of two indicators in their titrations with standard

acid solutions. An indicator with a transition range in the pH range of 8 to 10, such as

phenolphthalein, is used for detecting the first end point; an acid range indicator such as

bromocresol green is used for the second end point. Titration can be done A) In one sample, using

both indicators by successive addition of acid solution after each color change. B) Using two

samples containing exactly the same amount of mixture solution and applying two indicators

separately. The composition of the solution can be obtained using the volumes of acid used for

reaching each end point (http://users.metu.edu.tr/chem223f, n.d).

Titration is a technique that chemists use to determine the unknown concentration of a

known solution (we know what chemical is dissolved, but not how much in a solution). Because

knowing what the chemical is, how it will react with other chemicals is known and that reaction

can be used to determine the concentration of the solution by measuring the formation of

product(s). In the case of an unknown concentration of acid, a known concentration of hydroxide

base can be used. This type of reaction is a neutralization reaction, where salt and water are

products of the reaction: Acid + Base  Salt + H2O a pH indicator can be used,

a chemical that changes color depending on the pH, to show when the reaction has completely

neutralized. This point, where all acid was consumed and there is no excess of base, is called the

equivalence point. The equivalence point is used to determine the initial concentration of acid

using a series of calculations. The goal of the titration is to get as close as possible to the

equivalence point by careful addition of the base; this will ensure the calculated acid concentration

is as close to the true value as possible (https://www.researchgate.net/, n.d)

OBJECTIVES

The aim of this experiment is to determine the constituent’s presence in a mixture, and the

concentration present for each constituent.

MATERIALS AND EQUIPMENT

 Distilled Water  12M HCl

 NaCl  Na2CO3 standard

 Bromocresol Green Indicator  Erlenmeyer Flask

 Wire gauze  Analytical Balance

 Tripod and Bunsen Burner  Calibrated Burette

Table 1.

EXPERIMENTAL PROCEDURE

This section shows the step-by-step description of the activities that were done in order to

gather the information needed to achieve the purpose of the experiment.

A. PREPARATION OF REAGENTS

1. Standard HCl Solution

 Compute the volume of concentrated HCl needed to prepare 500 mL of 0.1000 M HCl

solution.

2. NaCl Solution

 Compute the weight of NaCl needed to prepare 250 mL of 0.05 M NaCl solution.
B. CORRECTION FACTOR FOR INDICATOR

1. Titrate approximately 100 mL of 0.05 NaCl and 3 drops of indicator.

2. Boil briefly, cool and then complete the Titration.

3. Determine the volume of HCl that react with the indicator. Create one to two replicates

C. STANDARDIZATION OF HCl TITRANT

1. Dry 1.5 to 2.0 g pure Na2CO3 in a glass weighing bottle at 150 to 160°C for at least 2

hours. Cool in the desiccator.

2. Weigh 0.15 g (+-0.3 mg) portions of the dry material into clean Erlenmeyer Flasks. Do

triplicate measurements.

3. Add 5. mL distilled water to each and swirl gently to dissolve the salt.

4. Add 4 drops of bromocresol green indicator and titrate the HCl solution to an

intermediate green color.

5. Stop the titration when the solution turned green and boil the solution gently for a

minute or two.

6. Cool the solution at room temperature, wash the flask walls with distilled water and

then continue the titration.

7. Record the burette reading.

D. ANALYSIS OF UNKWON SAMPLE

1. Pipette two 50 mL aliquot of the liquid sample into two Erlenmeyer flasks.

2. To the first aliquot, add 3 drops of phenolphthalein indicator.

3. To the second aliquot, add 3 drops of methyl orange indicator.

 4. Titrate the first aliquot with standard HCl until the appropriate color change.

5. For the second aliquot, titrate with standard HCl until color changes. Boil for 2-3 mins,

and then cool. Titrate again until the appropriate color change.

6. From the total volume of HCl used for the titration of the second aliquot, subtract the

indicator correction.

7. Compute for the two constituents (Na2CO3 and NaHCO3) molarity, mean molarity,

SD and % RSD of each.

RESULTS AND DISCUSSION

B. CORRECTION FACTOR FOR INDICATOR

TRIAL 1 TRIAL 2

100 mL NaCl 100 mL NaCl

V1= 0 mL V1= 0.1 mL

V2= 0.4 mL V2= 0.3 mL

ΔV= 0.4 mL ΔV= 0.2 mL

MEAN= 0.3 mL

Table 2.

Table 2 shows the difference in volume of the two trials for 100 mL NaCl. Both trials

resulted in a 0.3 mL mean.

C. STANDARDIZATION OF HCL TITRANT

 TRIAL 1 TRIAL 2 TRIAL 3

Weight of Na2CO3 0.1503 g 0.1498 g 0.1501 g

Initial Volume Before Boiling 0 mL 0 mL 0 mL

Final Volume Before Boiling 25 mL 25 mL 25 mL

ΔV Before Boiling 25 mL 25 mL 25 mL

Initial Volume After Boiling 0 mL 0 mL 0 mL

Final Volume After Boiling 15 mL 14 mL 16 mL

ΔV After Boiling 15 mL 14 mL 16 mL

True Volume of HCl 39.7 mL 38.7 mL 40.7 mL

Molarity 0.0714 M 0.0730 M 0.0732 M

Mean 0.0725

SD 9.8658x10^-4

% RSD 0.0136

Table 3.

Table 3 indicates the data for triplicate trials of Na2CO3, the first trials weighed 0.1503 g,

its change in volume before boiling is 25 mL and the change in volume after boiling weighed 15

mL, having the change in volume before and after boiling the compound it resulted to a 39.7 mL

in its true volume with the mentioned data it resulted to a molarity of 0.0714. For the second trial,

Na2CO3 weighed 0.1498 g, the change in volume before boiling is 25 mL and the change in after

boiling is 14 mL, using the said change in volume it resulted to a true volume of 38.7 mL and the

computed molarity with the said data revealed a molarity of 0.0730. The last trial weighed 0.1501

g, its change in volume before boiling is 25 mL and the volume after boiling is 16 mL, through
these volumes it resulted to a true volume of 40.7 mL. Using all the gathered data the computed

molarity for the last trial is 0.0732 M. The molarity for the triplicate trials depicts a mean of 0.0725,

a standard deviation of 9.8658x10^-4 and %RSD (Relative Standard Deviation) of 0.0136.

D. ANALYSIS OF UNKNOWN SAMPLE

1st ALIQUOT TRIAL 1 TRIAL 2 TRIAL 3

Volume of a Sample 50 mL 50 mL 50 mL

Initial Volume of HCl 0 mL 0 mL 0 mL

Final Volume of HCl 4 mL 3 mL 3 mL

ΔV of HCl 4 mL 3 mL 3 mL

MEAN 3.33

Table 4.

Table 4 reveals the data for the 1st Aliquot. Triplicate trials were created each trial has the

same volume weighing 50 mL. However, the change in volume for trial 1 is 4 mL it differs for

trial 3 and 4 weighing 3 mL. It resulted to a mean of 3.33.

2nd ALIQUOT TRIAL 1 TRIAL 2 TRIAL 3

Volume of Sample 50 mL 50 mL 50 mL

Initial Volume of HCl Before 0 mL 0 mL 0 mL

Boiling
Final Volume of HCl Before 6 mL 7 mL 7 mL
Boiling
 ΔV of HCl Before Boiling 6 mL 7 mL 7 mL

Initial Volume of HCl After Boiling 0 mL 0 mL 0 mL

Final Volume of HCl After Boiling 18 mL 13 mL 10 mL

ΔV After Boiling 18 mL 13 mL 10 mL

True Volume 23.7 mL 19.7 mL 16.7 mL

MEAN 20.03

CONSTITUENTS: Na2CO3 NaHCO3

Molarity 2.4143x10^-3 M 0.0242 M

Mean Molarity 0.0133

SD 0.0154

% RSD 1.1579

Table 5.

Table 5 shows the data gathered for the 2nd Aliquot. Each trial weighed the same volume

of sample weighing 50 mL. Before boiling of HCl, trial one has the change in volume weighing 6

mL and for the second and last trial’s change in volume it weighed 7 mL. After boiling the HCl

the change in volume for each trial is different from each other, trial one has a volume of 18 mL,

trial two contains a volume of 13 mL and the last trial has the least volume with 10 mL. Having

the data for before and after boiling volumes of HCl true volume was computed. The true volume

for trial one is 23.7 mL, trial two has a true volume of 19.7 mL and last trial is has a volume of

16.7 mL. The mean for the second aliquot is 20.03. The sample contained Na2CO3 and NaHCO3

constituents. For both the constituent’s molarity it resulted to a mean molarity of 0.0133, a standard

deviation of 0.0154 and %RSD (Relative Standard Deviation) of 1.1579.

ANALYSIS/ CALCULATION

On the first part of the experiment, the table shows that the given data is a grouped data. In

that case, the mean can be computed by using the mean formula of the grouped data:

To determine the value of the Standard Deviation, the Individuals uses the SD formula:

Where:
σ = Lower case sigma is the symbol for standard deviation,
Σ = Upper case sigma is the summation symbol,
X = Each individual value in the data set,
x̅ = The arithmetic mean (known as “x-bar”),
n = The number of data points in the set (the number of X values).
 The manual asks for the percentage Relative Standard Deviation (%RSD) of the given data.

The Individuals computed it by using the % RSD formula which is:

Where:
S = Standard Deviation,
X̅ = Mean.

To find the True Volume of each trial, the change in volume before boiling should be added

to the amount of volume after boiling, its summation minus the mean of the correction indicator.

ΔV Before Boiling + ΔV After Boiling = Ans – Correction Indicator

TRIAL 1 25 mL + 15 mL = 40 mL

40 mL– 0.3 = 39.7 mL

TRIAL 2 25 mL + 14 mL = 39 mL

39 mL – 0.3 = 38.7 mL

TRIAL 3 25 mL + 16 mL = 41 mL

41 mL – 0.3 = 40.7 mL

To compute for the molarity in the third part of the experiment the molar mass of Na2CO3

is needed in which it has 105.99 g/mol. The weight of sample multiplied by its molar mass, true

volume and stoichiometric ratio.

 1 𝑚𝑜𝑙 𝑁𝑎2𝐶𝑂3 2 𝑚𝑜𝑙 𝐻𝐶𝑙 1 1000 𝑚𝐿
Molarity of HCl = g Na2CO3 x 105.99 𝑔 𝑜𝑓 𝑁𝑎2𝐶𝑂3 x 1 𝑚𝑜𝑙 𝑁𝑎2𝐶𝑂3 x 𝑡𝑟𝑢𝑒 𝑣𝑎𝑙𝑢𝑒 x 1𝐿

TRIAL 1 1 𝑚𝑜𝑙 𝑁𝑎2𝐶𝑂3 2 𝑚𝑜𝑙 𝐻𝐶𝑙 1 1000 𝑚𝐿

0.1503 g of Na2Co3 x 105.99 𝑔 𝑜𝑓 𝑁𝑎2𝐶𝑂3 x 1 𝑚𝑜𝑙 𝑁𝑎2𝐶𝑂3 x 39.7 𝑚𝐿 x 1𝐿

= 0.0714 M

TRIAL 2 1 𝑚𝑜𝑙 𝑁𝑎2𝐶𝑂3 2 𝑚𝑜𝑙 𝐻𝐶𝑙 1 1000 𝑚𝐿

0.1498 g of Na2CO3 x 105.99 𝑔 𝑜𝑓 𝑁𝑎2𝐶𝑂3 x 1 𝑚𝑜𝑙 𝑁𝑎2𝐶𝑂3 x 38.7𝑚𝐿 x 1𝐿

= 0.0730 M

TRIAL 3 1 𝑚𝑜𝑙 𝑁𝑎2𝐶𝑂3 2 𝑚𝑜𝑙 𝐻𝐶𝑙 1 1000 𝑚𝐿

0.1501 g of Na2CO3 x 105.99 𝑔 𝑜𝑓 𝑁𝑎2𝐶𝑂3 x 1 𝑚𝑜𝑙 𝑁𝑎2𝐶𝑂3 x 40.7 𝑚𝐿 x 1𝐿

= 0.0732 M

To compute for the molarity of Na2CO3 that is found in the 2nd Aliquot, the mean of change

in volume of the 1st Aliquot is needed. Multiplied by the mean of HCl in standardization titrant,

stoichiometric ratio of Na2CO3 over HCl and the sample volume.

0.0725 𝑚𝑚𝑜𝑙 1 𝑚𝑚𝑜𝑙 𝑁𝑎2𝐶𝑂3 1

Molarity of Na2CO3 = x̄ volume of the 1st aliquot x x x 50 𝑚𝐿
𝑚𝐿 2 𝑚𝑚𝑜𝑙 𝐻𝐶𝑙

[Na2CO3] 0.0725 𝑚𝑚𝑜𝑙 1 𝑚𝑚𝑜𝑙 𝑁𝑎2𝐶𝑂3 1

3.33 mL x x x 50 𝑚𝐿 = 2.4142x10^-3 M
𝑚𝐿 2 𝑚𝑚𝑜𝑙 𝐻𝐶𝑙
 To get the molarity of NaHCO3, first the mean of the change in volume before boiling the

HCl is needed minus the mean of HCl in standardization of titrant. The product is then multiplied

to the stoichiometric ratio of NaHCO3 over HCl and the sample volume.

0.0725 𝑚𝑚𝑜𝑙
Molarity of NaHCO3 = x̄ ΔV Before Boiling - x̄ volume of the 1st aliquot = Ans x x
𝑚𝐿

1 𝑚𝑚𝑜𝑙 𝑁𝑎𝐻𝐶𝑂3 1
x 50 𝑚𝐿
1 𝑚𝑚𝑜𝑙 𝐻𝐶𝑙

[NaHCO3] 20.03 mL – 3.33 = 16.7 mL

0.0725 𝑚𝑚𝑜𝑙 1 𝑚𝑚𝑜𝑙 𝑁𝑎𝐻𝐶𝑂3 1

16.7 mL x x x 50 𝑚𝐿 = 0.0242 M
𝑚𝐿 1 𝑚𝑚𝑜𝑙 𝐻𝐶𝑙

CONCLUSION

Double titrations are necessary specially when there are two similar types of solution, using

one indicator will show you only one chrome effect. Then, if two indicators be used it will show

different colors. Double titrations help a lot and is a figure of merit.

REFERENCES

(n.a), “Analysis of Carbonate Mixtures.pdf”. (n.d). users.metu.edu.tr/chem223/Analysis of

carbonate mixtures.pdf.

(n.a), “Titration of Hydrochloric Acid with Sodium Hydroxide”. (n.d). Microsoft Word - SP12

1011 Titration of Hydrochloric Acid with Sodium Hydroxide,

jupiter.plymouth.edu/~jsduncan/courses/.../4-Titrations.pdf.