LABORATORY REPORT

LAB 7: Chloride and Conductivity

SUBMITTED BY:
MR. BISHAL BHARI (115461)




SUBMITTED TO:
DR. OLEG SHIPIN
MISS SALAYA PHUNSIRI



ED 78.01: ENVIRONMENTAL CHEMISTRY AND LABORATORY
ENVIRONMENTAL ENGINEERING AND MANAGEMENT
SCHOOL OF ENVIRONMENT, RESOURCES AND DEVELOPMENT
ASIAN INSTITUTE OF TECHNOLOGY
Chloride and Conductivity November 6, 2013

1

1. Introduction
The chloride ion is formed when the element chlorine (a halogen) gains an electron to form
an anion (negatively charged ion) Cl. Chlorides occur in natural water in widely varying
concentration. The Chloride content increases as the mineral content increases. Upland and
mountain supplies usually are quite low in chloride, whereas river and ground water usually have
a considerable amount. Sea and ocean water represent the residues resulting from partial
evaporation of natural water that flow into them, and chloride levels are very high. Human
excreta, particularly the urine, contain chloride in an amount about equal to the chloride
consumed with food and water. This amount averages about 6 g of chloride per person per day
and increases the amount of Cl
-
in municipal wastewater about 15 mg/L above that of the
carriage water. Thus, wastewater effluents add considerable chloride to receiving streams. A
high chloride content exerts a deleterious effect on metallic pipes and structures, as well as on
agricultural plants.
Conductivity is a measure of the ability of an aqueous solution to carry an electric current. This
ability depends on the presence of ions ; on their total concentration, mobility, and valence ; and
on the temperature of measurement. Solutions of most inorganic compounds are relatively good
conductors. Conversely, molecules of organic compounds that do not dissociate in aqueous
solution conduct a current very poorly, if at all.
2. Objective
a) To determine the chloride of the sample by using both the Argentometric Method and
Mercuric Nitrate Method.
b) To determine electrical conductivity of the sample.
3. Methodology
3.1 Chloride Determination
3.1.1 Argentometric or Mohr Method
Principle: In a neutral or slightly alkaline solution, potassium chromate can indicate the end point
of the silver nitrate titration of chloride. Silver chloride is precipitated quantitatively before red
silver chromate is formed.
Procedure :
Pipette 50 - 100 mL of sample (pH 7-10) and put it in 250 mL-flask.

Add 1 mL of K
2
CrO
4
indicator and mix them thoroughly.

Titrate with 0.0141 N AgNO
3
.
Then we will get pinkish yellow at the end point.
Chloride and Conductivity November 6, 2013

2

Calculation :
Chloride, mg/L = (A-B) * 0.0141 N AgNO
3
* 35450
mL of sample

NaCl, mg/L = (mg Cl
-
/L) * 1.65
Where,
A = mL titration for sample
B = mL titration for blank

3.1.2 Mercuric Nitrate Method
Principle : Chloride can be titrated with mercuric nitrate, Hg(NO
3
)
2
, because of the formation of
soluble, slightly dissociated mercuric chloride. In the pH range 2.3 - 2.8, diphenylcarbazone
indicates the titration end point by formation of a puple complex with the excess mercuric ions.
Xylene cyanol FF serves as a pH indicator and end point enhancer. Increasing the strength of the
titrant and modifying the indicator mixtures extend the range of measurable chloride
concentrations.
Procedure :
Titration of chloride concentrations less than 100 mg/L.
Titration of chloride concentrations less than 100 mg/L.
Pipette 50 ml of sample and put it in 250 mL-flask.
Adjust pH to 8 with 1 N NaOH.
Add 1 mL indicator - acidifier reagent. (green-blue)
Titrate with 0.0141 N Hg(NO
3
)
2.
.
Then we will get purple color at the end point.
(green-blue blue purple)
Calculation:
Chloride, mg/L = (A-B) * 0.0141 N Hg(NO
3
)
2
* 35450
mL of sample

NaCl, mg/L = (mg Cl
-
/L) * 1.65

Chloride and Conductivity November 6, 2013

3

Where,
A = mL titration for sample
B = mL titration for blank

3.2 Conductivity Determination

Conductivity of the sample was measured using conductivity meter Model Knick 703
Procedure:
Rinse the electrode with distilled water.
Blot-dry by clean tissue paper.
Immerse the electrode to the water sample until the level of the water stay in between the
marks.
Measure the EC of water sample.
Note the temperature of the water sample.
Rinse electrode again with distilled water.
4. Presentation of Results
4.1 Determine of Chloride:

Table 1: Determination of Chloride concentration of Sample CC39
Sample No. Agentometric or Mohr Mercuric nitrate
Vol. of titrate
for sample,
(ml)
Vol. of titrate
blank,
(ml)
Vol. of titrate
for sample
(ml)
Vol. of titrate
blank,
(ml)
1 2.4 0.5 2.0 0.1
2 2.45 0.5 2.1 0.1
Average 2.425 0.5 2.05 0.1
Chloride conc., (mg/l) 19.24 19.49
NaCl conc., (mg/l) 31.75 32.16


Chloride and Conductivity November 6, 2013

4

Calculation
Argentometric or Mohr Method
Chloride, mg/L = (A-B) x 0.0141 N AgNO
3
x 35450
mL of sample
Where,
A = mL titration for sample
B = mL titration for blank

= (2.425 0.5) x 0.0141 N AgNO
3
x 35450
50 ml of sample
= 19.24 mg/L
NaCl, mg/L = (mg Cl
-
/L) * 1.65
= 19.24 (mg Cl
-
/L) * 1.65
= 31.75 mg/L

Mercuric Nitrate Method
Chloride, mg/L = (A-B) * 0.0141 N Hg(NO
3
)
2
* 35450
mL of sample
Where,
A = mL titration for sample
B = mL titration for blank

= (2.05 0.1) x 0.0141 N Hg(NO
3
)
2
x 35450
50 mL of sample
= 19.49mg/L
NaCl, mg/L = (mg Cl
-
/L) * 1.65
= 19.49 mg Cl
-
/L * 1.65
= 32.16 mg/L
Chloride and Conductivity November 6, 2013

5

4.2. Determine of Conductivity
Sample CC39
The conductivity was carried out using Conductivity meter
Table 2: Determination of Conductivity of sample CC39
Parameter Value
Conductivity of Sample (mS/m) 11.59
Temperature (
o
C) 24.5

5. Discussion of Result

Chloride concentration from the Argentometric and Mecuric Nitrate methods was found to be
19.24 and 19.49 mg/L respectively. These two concentration obtained slight vary in
concentration however in most of the cases these two concentration can vary significantly. The
Mercuric Nitrate Method is more precise and accurate than the Argentometric Method. The
reasons are as follows:
The end point of Mohr method is very difficult to be observed.
Mohr method has a lot of interfering factor and several precaution must be taken to
obtain accurate result, the precaution to be taken are as follow:
A uniform sample size must be used.
The pH must be in the range 7-10 because Ag
+
is precipitate as AgOH(s) at high pH
levels and the CrO
4
2-
is converted to Cr
2
O
7
2-
at low pH levels.
A definition amount of indicator must be used to provide a certain concentration of
CrO
4
2-
; otherwise Ag
2
CrO
4
(s) may from too soon or not soon enough.

The Mercuric Nitrate Method is much less subject to interference than the Argentometric
Method because the titration is performed in a sample that pH is adjusted to a value of
about 2.5. Under these condition Hg
2+
ion combines with Cl
-
to form HgCl
2
complex
which is soluble,

Hg
2+
+ 2 Cl
-
HgCl
2
(soluble)
therefore making end point detection easier than the Argentometric Method. As the Cl
-

concentration is reach zero, the Hg
2+
concentration will increase to a level where it
becomes significant as the mercuric nitrate is added.
Chloride and Conductivity November 6, 2013

6

Between these two methods, end point of Mercuric nitrate method is easy to determine
than Mohr method because (1) the changing color of indicator is strong and easy to
recognize and (2) there is no presence of other precipitation that does not made by Cl
-

ion. Thus, Mercuric nitrate method needs lower volume of titrant but more precise than
the rest. However, two times of pH adjustment in the solution will cause trouble of
inaccuracy.
Argentometric method is suitable for sample which has very little turbidity as it can easily
interfere with the color change and the water that has little of chloride (0.15 to 10 mg/l). The
color change of this method is already difficult to see, thus require skill and experience but this
method is easy to do and use less of chemical substance.
For mercuric nitrate method, color change is easier to see than the argentometric method, and it
has less interference. However, this method can only be done after the chloride concentration is
roughly known, because it is suitable for only less than 100 mg/L of chloride. Larger
concentration of chloride must be diluted to less than the above figure.
Conductivity value for sample CC39 is 11.59 mS/m. at 24.5
o
c. The instrument was already
calibrated, so the calibration is not included here. Conductivity can be used as a rough estimate
for dissolved solid, particularly applied in a water supply field. The dissolved solid can be
approximated by multiplying conductivity figure by a specific empirical factor which is around
0.55 to 0.9. Conductivity is temperature dependent, and therefore temperature should also be
noted.


References
AIT, SERD, EEM, Course ED 78.01-Environmental Chemistry and Laboratory,
Laboratory Instruction Sheet 7: Chloride and Conductivity;2013
Sawyer C.N et.al, Chemistry for Environmental Engineering: 5
th
edition Mc.Graw-
Hill;2002
Problem November 6, 2013

1

Problem
6.1 Sodium chloride has considerable as a tracer for pollution of wells. Give the reasons for
this purpose.
Sodium Chloride is used as tracer of pollution because of the following reasons:
1. Its presence is not visually detectable as it easily dilutes in water.
2. It is a normal constituent of water and has not toxic effects.
3. The chloride ion is not absorbed by soil formations.
4. It does not alter or change in amount by biological processes.
5. The chloride ion can be easily measured.

6.2 Explain why a blank correction must be applied to the titration value in both the
Argentometic and Mercuric Nitrate Methods in the calculations of chloride content.
Argentometric Method
Ag
+
+ Cl
-
AgCl
In this method when Ag
+
excess, it will combine with CrO
2
4
-
that decompose from K
2
CrO
4

indicator. Ag
2
CrO
4
begin to form a reddish - brow principitate. If indicator or distilled water is
not pure and have some chloride it will interfere the desired reaction. Hence the determination of
the blank is required.
Mercuric Nitrate Method
Hg
2+
+ Cl
-
HgCl
2

The excess of Hg
2+
can combine with OH
-
to form Hg(OH)
2
like Argentometric method. We
have to do a blank sample to recheck an error in experiment.

6.3 What purpose is served by the nitric acid added to the indicator in the mercuric nitrate
method for chlorides ?
Nitric acid (HNO
3
) is added to adjust the pH of sample near 2.5. Because Hg
2+
ion can combine
with Cl
-
and become HgCl
2
complex under the condition of pH value ~ 2.5. And the color
change of the indicator can only be obtained at the pH 2.5 adjusted by adding nitric acid.