Volhard Method - Determination of Chlorides in Yogurt

Chemical Analysis Laboratory
Jean Carlos Villa Arpi - [email protected]

Hector Ronaldo Lasluisa Morocho - [email protected]
Kenia Michelle Luzuriaga Espinoza - [email protected]
Alexandra Maribel Puruncaja Catota - [email protected]
Andrea Karolina Valarezo Albán - [email protected]
June 6, 2020
Chemical Analysis Laboratory, School of Chemistry and Engineering, Yachay Tech,

Urcuquí. Ecuador.
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San Miguel de Urcuqui | Hacienda San José | www.yachaytech.edu.ec

Laboratory class
Volhard’s Method of precipitation titration: Determination of chlorides
in yogurt
Summary
A sample of yogurt will be diluted in distilled water to form a solution, from which an
aliquot will be isolated in an Erlenmeyer flask with silver nitrate, nitric acid and ferric
sulfate ammonia as the indicator with a proper stirring to coagulate silver chloride. Then,
the resultant content will be titrated with potassium thiocyanate until obtain a light orange
color in the sample analyzed. This entire procedure is suggested to repeat around of two or
three times to compare results and obtain the deviations of each one in order to determine
the amount of chlorides in the original sample.
Introduction
Titration is a process by which the concentration of an unknown substance in solution is
determined by adding measured amounts of a standard solution that reacts with the
unknown. Then the concentration of the unknown can be calculated using the stoichiometry
of the reaction and the number of moles of standard solution needed to reach the so-called
end point.
 Precipitation titrations
Precipitation is the term used to describe the process whereby a substance leaves
solution rapidly, forming either a crystalline solid or amorphous solid (the precipitate).
In the case of a precipitation titration, this process occurs when the analyte forms a
precipitate with the titrant. The most common types of precipitation titrations use silver
nitrate as the titrant. They are often referred to as argentometric titrations.
 Argentometric titrations
In analytical chemistry, it is a type of titration involving the silver(I) ion. Typically, it is
used to determine the amount of chloride present in a sample. The sample solution is
titrated against a solution of silver nitrate of known concentration. Chloride ions react
with silver(I) ions to give the insoluble silver chloride:
Ag+ (aq) + Cl− (aq) → AgCl (s)
 Volhard’s method
The Volhard’s method was first descried by Jacob Volhard, a German chemist, in 1874.
This is an indirect titration procedure used for determining the anions that precipitate
with silver.
This method uses a back titration with potassium thiocyanate to determine the
concentration of chloride ions in a solution. Before the titration an excess volume of a
silver nitrate solution is added to the solution containing chloride ions, forming a
precipitate of silver chloride. The term ‘excess’ is used as the moles of silver nitrate
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added are known to exceed the moles of sodium chloride present in the sample so that
all the chloride ions present will react.
Ag+ (aq) + Cl− (aq) → AgCl (s)
The indicator Fe3+ (ferric ion) is then added and the solution is titrated with the potassium
thiocyanate solution. The titrate remains light yellow as the excess silver ions react with the
thiocyanate ions to form a silver thiocyanate precipitate.
Ag+ (aq) + SCN- (aq) → AgSCN(s)

Once all the silver ions have reacted, the slightest excess of thiocyanate reacts with Fe3+ to
form a dark red complex.
Fe3+ (aq) + SCN- (aq) → [FeSCN]2+ (aq)
The concentration of chloride ions is determined by subtracting the titration findings of the
moles of silver ions that reacted with the thiocyanate from the total moles of silver nitrate
added to the solution. This method is used when the pH of the solution, after the sample has
been prepared, is acidic.
Figure 1. Volhard’ method: titration between silver ion with thiocyanate ion, and determination of the end point.
Objectives
 Determine the concentration of chlorides in an aqueous sample using the Volhard’s

method.
 Apply the theoretical principles of precipitation volumes using the Volhard’s
method.
Materials
 Erlenmeyer flask (250 mL)
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 Graduated pipette (10 mL)
 Graduated pipette (5 mL)
 Suction pear
 Burrete clamps
 Burette (25mL)
 Wash bottle
 Volumetric flask (100mL)
 Beaker (150mL)
Reactives
 Natural yogurt sample

 Silver Nitrate 0.1N
 Concentrated Nitric Acid
 Ferric Ammonium Sulfate (saturated)
 Potassium thiocyanate 0.1N
 Distilled Water
Experimental Procedure
 Measure 10 mL of the natural yogurt sample using the suction pear and graduated
pipette of 10 mL.
 Transport the measured sample to the 100 ml volumetric flask.
 Add distilled water to the volumetric flask until it reaches 100 mL, shake until
obtaining a homogeneous mixture and transport it to a 150 mL beaker.
 Take 10 ml of the sample, again with the help of the suction pear and graduated
pipette, and transfer it to the 250 ml Erlenmeyer flask.
 Add 10 ml of Silver Nitrate, 1 ml of nitric acid, 1 ml of the indicator (Ferric sulfate
ammonia) and shake vigorously to coagulate the precipitate forming AgCl.
 Repeat the procedure for at least two or three times, using the same amount of
sample in the other Erlenmeyer flasks.
 Titrate the excess of 0.1 N Silver nitrate with the Potassium Thiocyanate until
obtaining a permanent slight orange coloration.
Final Questions
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 Explain briefly why in the Volhard’s method the precipitate formed must be
removed before the excess silver ion is removed by recoil in the determination of
chloride ions
 What is the role of nitrobenzene added to the solution containing chlorides in the
determination by the Volhard’s method?
 Express the concentration of chlorides in mg / l NaCl.
Recommendations
 For greatest accuracy it is a good idea to standardize your thiocyanate solution by
titrating several samples against your standardized solution.
 Measure the volumetric units very accurately and pay close attention when adding
the solution to avoid deviating our practice from the best results.
 Rinse the burette, pipet and volumetric flask with several portions of distilled water
and put them away. Use a brush and soapy water to wash the Erlenmeyer flasks.
References
[1].Harris, Daniel Charles (2003). Quantitative chemical analysis (6th ed.). San
Francisco: W.H. Freeman. pp. 142–143
[2].https://www.rsc.org/publishing/journals/prospect/ontology.asp?
id=CMO:0002145&MSID=B000901F
[3].https://chem.libretexts.org/Courses/Northeastern_University/09%3A_Titrimetric_M
ethods/9.5%3A_Precipitation_Titrations
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Chemical Analysis Laboratory

Jean Carlos Villa Arpi - [email protected]

Chemical Analysis Laboratory, School of Chemistry and Engineering, Yachay Tech,

San Miguel de Urcuqui | Hacienda San José | www.yachaytech.edu.ec

San Miguel de Urcuqui | Hacienda San José | www.yachaytech.edu.ec

Ag+ (aq) + Cl− (aq) → AgCl (s)

Ag+ (aq) + SCN- (aq) → AgSCN(s)

 Determine the concentration of chlorides in an aqueous sample using the Volhard’s

San Miguel de Urcuqui | Hacienda San José | www.yachaytech.edu.ec

 Natural yogurt sample

San Miguel de Urcuqui | Hacienda San José | www.yachaytech.edu.ec

San Miguel de Urcuqui | Hacienda San José | www.yachaytech.edu.ec

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