Experiment No.

6
“Determination of Carbonates in a Mixture: Double Indicator Titration”

I. Objectives

 To determine the percent composition and molar concentration of each constituents

present in the unknown sample of carbonate mixtures
 To analyze the volume relationships used between the two endpoints: conversion from
carbonate to hydrogen carbonate and formation of carbonic acid and carbon dioxide
 To standardized the hydrochloric acid against sodium carbonate which will be used as a
titrant

II. MSDS

Chemical/Reagent Safety Precautions First-Aid Disposal

12 M HCl Toxic and corrosive; For any contact, wash Inorganic Waste
Wear PPE when with water Container
handling
NaCl Not suitable for food; Use water for first Solid waste
very soluble. aid/emergency purposes container

Na2CO3 standard Not for food, drug or Rinse with water in any Dispose in its
household use, can contact appropriate
cause some irritation container
Methyl orange May cause irritation, Rinse with water for Dispose in its
indicator non-hazardous, use emergency purposes appropriate
PPE when handling container
Phenolphthalein Avoid strong oxidizers Rinse with water for any Dispose in
indicator and exposure to light contact inorganic waste
container

III. Materials and Equipment

 Beaker, 200-mL
 Volumetric flasks, 500-mL & 250-mL
 Erlenmeyer flasks, 250-mL
 Calibrated burette, 25-mL
 Wash Bottle
 Stirring rod
  Tripod and Bunsen Burner

Reagents

 Distilled Water
 12 M HCl
 NaCl
 Na2CO3 standard
 Methyl orange indicator
 Phenolphthalein indicator

IV. Procedure / Schematic Diagram

A. Preparation of reagents

 Standard HCl Solution

≈ 9.115g HCl

-Weigh
-Dilute to 500mL
Store in a
reagent bottle

 NaCl Solution

≈ 0.7305g NaCl

-Weigh
-Dilute to 250mL
Store in a
reagent bottle
B. Standardization of HCl titrant

1.5 to 2.0 g pure Na2CO3

-Dry at 150 to 160°C (2hours)

- Cool at desiccator

0.15g of dried Na2CO3

- weigh triplicates
- +50mL H2O; swirl
- +4d methyl orange
- Titrate with HCl
Orange Solution

-boil solution (2minutes)

- Cool @ room temp
-wash the walls
- continue titration
Record burette reading

- Do blank correction
- Repeat 3x

Compute for Molarity

C. Analysis of unknown sample (Single vessel only)
*Sample may contain NaOH only, Na2CO3 only and NaHCO3 only or any two components
combination in these 3 constituents.

Unknown sample
- Dry at 110°C (2hours)
- cool at desiccator

Dried sample

- dilute in 100mL
10 mL aliquot (triplicates)
- +50 mL H2O; swirl
- +2d phenolphthalein
- immerse sol’n in ice bath
- titrate; swirl until pink color disappears
- *Omit this step if sol’n doesn’t turn pink when
phtp is added

Record Volume of phtp

endpoint
- Remove sol’n in ice bath
- titrate (follow steps 4-6)
-Record volume for methyl orange endpoint
Compute for %Comp of
NaOH, Na2CO3 and NaHCO3
V. Data and Results
Table 1. Preparation of the Sample
T1 T2 T3
Unknown sample A A A
Volume of the original stock, mL 10.00 10.00 10.00
Volume of the water added, mL 90.00 90.00 90.00
Final volume of the solution, mL 100.00 100.00 100.00

Table 2. Analysis of Components of the Mixture

2.1 Methyl orange indicator T1 T2 T3
Volume of sample titrated, mL 50.00 50.00 50.00
Concentration of HCl, M 0.1000 0.1000 0.1000
Initial volume of HCl, mL 2.50 1.80 0
Final volume of HCl, mL 20.75 19.60 18.50
Volume of HCl used in titration, mL 18.25 17.80 18.50

2.2 Phenolphthalein indicator T1 T2 T3

Volume of sample titrated, mL 50.00 50.00 50.00
Concentration of HCl, M 0.1000 0.1000 0.1000
Initial volume of HCl, mL 38.90 1.50 0
Final volume of HCl, mL 44.80 8.30 6.30
Volume of HCl used in titration, mL 5.90 6.80 6.30

Determination of Components T1 T2 T3
Mass NaOH, g 0.024 0.027 0.025
Mass NaHCO3, g 0.15 0.15 0.16
Mass Na2CO3, g 0.13 0.13 0.13
% NaOH 0.048% 0.054% 0.050%
% NaHCO3 0.3% 0.3% 0.3%
% Na2CO3 0.26% 0.26% 0.26
Components present in the sample NaHCO3 and NaHCO3 and NaHCO3 and
Na2CO3 Na2CO3 Na2CO3
Calculations:
C. Analysis of Unknown Sample
39.997 g of NaOH
 g NaOH=(V phth ( L ))(M of HCl)
1mol of NaOH
39.997 g of NaOH
T1: g NaOH=( 0.00590 L ) ( 0.1000 M of HCl ) =0.024 g of NaOH
1 mol of NaOH
39.997 g of NaOH
T2: g NaOH=( 0.00680 L ) ( 0.1000 M of HCl ) =0.027 g of NaOH
1 mol of NaOH
 39.997 g of NaOH
T3: g NaOH=( 0.00630 L ) ( 0.1000 M of HCl ) =0.025 g of NaOH
1 mol of NaOH
84.007 g of NaHCO3
 g NaHCO3 =(V mto ( L )) ( 0.1000 M of HCl )
1 mol of NaHCO 3
84.007 g of NaHCO 3
T1: g NaHCO3 =( 0.01825 L )( 0.1000 M of HCl )
1 mol of NaHCO3
¿ 0.15 g of NaHCO 3

84.007 g of NaHCO 3
T2: g NaHCO3 =( 0.01780 L )( 0.1000 M of HCl )
1 mol of NaHCO3
¿ 0.15 g of NaHCO 3

84.007 g of NaHCO 3
T3: g NaHCO3 =( 0.01850 L )( 0.1000 M of HCl )
1 mol of NaHCO3
¿ 0.16 g of NaHCO3

V mto + V phth 105.9888 g of Na 2 CO3

 g Na2 CO 3=( ) ( 0.1000 M of HCl )
2 1 mol of Na 2 CO 3
105.9888 g of Na2 CO 3
T1: g Na 2 CO 3= ( 0.01825 L+0.00590
2
L
)( 0.1000 M of HCl ) 1 mol of Na 2 CO 3
¿ 0.13 g of Na2 CO3

0.01780 L+0.00680 L 105.9888 g of Na2 CO 3

T2: g Na 2 CO 3= ( 2 )
( 0.1000 M of HCl )
1 mol of Na 2 CO 3
¿ 0.13 g of Na2 CO3

0.01850 L+0.00630 L 105.9888 g of Na2 CO 3

T3: g Na 2 CO 3= ( 2 )
( 0.1000 M of HCl )
1 mol of Na 2 CO 3
¿ 0.13 g of Na2 CO3

 % NaOH =
( vol. ofgsolution
NaOH
( mL ) )
×100

T1:% NaOH =( 0.024 g NaOH

50.00 mL )
×100=0.048 % NaOH

0.027 g NaOH
T2:% NaOH =(
50.00 mL )
×100=0.054 % NaOH
 T3:% NaOH = ( 0.025 g NaOH
50.00 mL )
×100=0.050 % NaOH

g NaHCO 3
 % NaHCO 3= ( vol . of solution ( mL ) ) ×100

( 0.1550.00
T1:% NaHCO 3=
g NaHCO
mL )
3
×100=0.3 % NaHCO 3

0.15 g NaHCO
T2:% NaHCO =(
50.00 mL )
3
3 ×100=0.3 % NaHCO 3

0.16 g NaHCO
T3:% NaHCO =(
50.00 mL )
3
3 ×100=0.32 % NaHCO 3

g Na 2 CO 3
 % Na2 CO3= ( vol . of solution ( mL ) ) ×100

0.13 g Na2 CO3

(
T1:% Na2 CO3= )
50.00 mL
×100=0.26 % Na2 CO 3

0.13 g Na CO
T2:% Na CO =(
50.00 mL )
2 3
2 3 ×100=0.26 % Na CO 2 3

0.13 g Na CO
T3:% Na CO =(
50.00 mL )
2 3
2 3 ×100=0.26 % Na CO 2 3

VI. Discussion

A double indicator titration is the process used in chemistry experiments to determine and
analyze the amount of concentration of acids and bass in a solution at two end points. In this
specific experiment however, the indicators that are used are phenolphthalein and methyl orange.
Phenolphthalein is pH indicator commonly used for titrations that changes to pink in alkaline
solutions and bright magenta at a pH level of 10 and above. Methyl orange on the other hand is
an indicator used in titration due to its distinct color variance at different pH values. it is color
orange in a neutral medium, yellow in an alkaline medium and reddish orange in an acidic
medium. Phenolphthalein is used in this experiment to measure the first end point of the solution,
when NaHCO3 is formed. However, methyl orange changes its color at the second end point only
and the first end point remains unknown.
Sodium Hydroxide (NaOH) and NaHCO3 is a pair that cannot exist together in a mixture.
Since NaOH is a strong base and NaHCO 3 is an amphoteric salt, the reaction of the two will
produce a carbonate ion. After the reaction, there will be less hydroxide left and therefore the
components of the solution will not be distinguishable. Though NaHCO 3 is an acid salt in terms
of its composition, it is also a basic salt as its aqueous solution is slightly, tough distinctly, basic
due to hydrolysis.
 In titrating the solution, it produces carbon dioxide as a by-product that is trapped within
the solution. Since carbon dioxide in the solution can be converted to carbonic acid, it might act
as a buffer that infer with the accuracy of the data that is gathered in the experiment. Through the
process of boiling, the carbon dioxide will be removed thus increasing the accuracy of the
volumes as well as the endpoints while titrating.
The primary standard that is used to standardize the HCl titrant is sodium carbonate
(Na2CO3). To know if a primary standard is best to be used, the six desired properties for a
primary standard must be considered, ranked from importance (first to fourth is more important
the last two): has high purity, stability (low reactivity), low hygroscopicity, high equivalent
weight, non-toxic, and ready and cheap availability. With respect to the given criteria, sodium
carbonate satisfies all except having high equivalent weight. Its molecular weight is 105.9885
g/mol, however its equivalent weight is only 52.9942 g/mol. Therefore,
tris(hydroxymethyl)aminomethane is a better choice since its molecular weight is the same of its
equivalent weight (121.12 g/mol).
One of the possible errors that can be encountered during the analysis is the carbonate in
the solution while titrating. It happens when the solution reacts with the carbon dioxide in the
atmosphere and while titrating. It acts as a buffer and increases the pH level of the solution
resulting to a less accurate data gathering. Volumetric glasswares that are used to store basic
solutions can also disrupt the accuracy of the glassware through OH - slowly reacting with the
silicon in the glasswares. In addition to this, the reaction that takes place can destroy the insides
of the glassware. Also, not measuring on where the titrant on the burette was, might lead on not
analyzing the data accurately and the correct amount of titrant cannot be determined.

Conclusion
In the experiment, the constituents containing Na2CO3, NaHCO3 and NaOH alone or in a
solution are determined by using titrimetry in the form of percent composition. Determinations if
the constituents in a solution containing Na2CO3, NaHCO3 and NaOH on its own or in a solution
gives an interesting example for neutralization titration. It is also known that only two of these
constituents can exist with each other since any of them eliminates the third constituent. In this
case, NaOH that is mixed with NaHCO 3 produces Na2CO3 until both or one of the original
reactants is used up.
In determining the constituents that are present in the mixture, these are analyzed with the
help of two indicators, specifically, methyl orange and phenolphthalein. Both of these indicators
show how the reaction goes by their colors. Phenolphthalein has a transition range in the pH
range of 8 to 10, thus, this is used to detect the first endpoint, for when NaHCO 3 is formed.
Methyl orange on the other hand, is used to indicate the second end point of the reaction in the
solution. Titration can be done with both indicators used and successive addition of an acid
solution after every color change. In this experiment, two samples that contain the same amount
of the mixture, but the indicators that were used are added separately.
 Analyzing the sample, the titrant was first prepared with HCl, diluted to 500 mL. In
standardizing the solution, a primary standard is used, specifically Na2CO3. The titrations are
done in triplicates and calculated for HCl molarity. The calculated g of NaOH of the triplicates
are: 0.0024 g, 0.0027 g, and 0.0025 g. For NaHCO 3, the mass of each trial is: 0.15 g, 0.15 g, and
0.16 g. And g Na2CO3 in all triplicates is 0.13 g. In calculating for the constituents’’ percent
composition, the calculated mass of each constituent will be divided by the volume of the
solution, and multiplied by 100. The % NaOH are as follow: 0.048%, 0.052%, and 0.050%. For
the %NaHCO3, the calculated data are: 0.3%, 0.3% and 0.32%. And %Na 2CO3, all triplicates
calculating to 0.26%. From the data stated above, we can conclude that the solution contains both
NaHCO3 and Na2CO3, as the NaOH that was present initially was used up to yield another
compound, which is Na2CO3.