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Volumetric Analysis

This document outlines the principles and procedures of volumetric analysis and titration. It discusses key concepts like primary and secondary standards, standardization, and determining sample purity through titration. Titration involves completely reacting an analyte with a titrant. The endpoint and equivalence point indicate when the reaction is complete. Volumetric analysis allows calculating analyte concentration from the reaction stoichiometry and titrant volume. Dilution and standardization are also explained. Sample problems demonstrate calculating concentrations and percent purity from titration data.

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267 views31 pages

Volumetric Analysis

This document outlines the principles and procedures of volumetric analysis and titration. It discusses key concepts like primary and secondary standards, standardization, and determining sample purity through titration. Titration involves completely reacting an analyte with a titrant. The endpoint and equivalence point indicate when the reaction is complete. Volumetric analysis allows calculating analyte concentration from the reaction stoichiometry and titrant volume. Dilution and standardization are also explained. Sample problems demonstrate calculating concentrations and percent purity from titration data.

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VOLUMETRIC ANALYSIS

D.F.P
LESSON OUTLINE

 Volumetric Analysis
 Titration

 Dilution and Mixing of Solutions

 Primary and Secondary Standards

 Standardization

 Determination of Sample Purity


VOLUMETRIC ANALYSIS
 A technique in which the volume of
material needed to react with the
analyte is measured
 The analyte concentration is calculated
from the reaction stoichiometry and the
amount of reagent that was required to
react with all of the analyte.
 quantitative
TITRATION measurement of an
analyte in solution by
completely reacting with
a reagent
 ENDPOINT- the point at which all of the
analyte is consumed

 INDICATOR- indicates the endpoint; also


present in the solution.

 EQUIVALENCE POINT- reached when


the quantity of titrant added is the exact
amount necessary for stoichiometric
reaction with the analyte
METHODS OF DETERMINING WHEN ANALYTE
HAS BEEN CONSUMED INCLUDE:

 detectinga sudden change in voltage or


current between a pair of electrodes

 Observing an indicator color change

 Monitoring the absorbance of light by


species in the reaction
SEVERAL REACTIONS USED IN TITRIMETRIC
ANALYSIS, DEPENDING ON THE TYPES OF REACTANTS
INVOLVED:

 Acid-Base
 H+ + OH- H2O strong acid – strong base
 HA + OH- A- + H2O weak acid- strong base
 BOH + H3O+ B+ + 2 H2O weak base-
strong acid
 Redox Reaction
 Fe2+ + Ce4+ Fe3+ + Ce3+
 5 Fe2+ + MnO4- + 8H+ 5 Fe3+ + Mn2+ + 4 H2O
 For acid- base reactions , indicators are
available that change color when the pH
changes.

 When all of the analyte is neutralized,


further addition of the titrant causes the
pH of the solution to change causing the
color of the indicator to change.
 Precipitation
 Ag+ + X- AgX(s) where X- = Cl-,
Br-. I-, SCN-
 Complex Formation
 Ag+ + 2 CN- Ag(CN)2
(basis for the Liebig method for the
determination of CN-)
DILUTION AND MIXING OF SOLUTIONS
 Dilution is the process whereby the concentration
of a solution is lessened by the addition of
solvent.

 For example, we might say that a glass of iced


tea becomes increasingly diluted as the ice melts.
The water from the melting ice increases the
volume of the solvent (water) and the overall
volume of the solution (iced tea), thereby
reducing the relative concentrations of the
solutes that give the beverage its taste
Both solutions contain the same mass of copper
nitrate. The solution on the right is more dilute
because the copper nitrate is dissolved in more
solvent.
 Dilution is also a common
means of preparing
solutions of a desired
concentration. By adding
solvent to a measured
portion of a more
concentrated stock
solution, we can achieve a
particular concentration.

 Aliquots (carefully
measured volumes) of the
stock solution can then be
diluted to any desired
volume.
Watch this video about : How to dilute a solution
https://youtu.be/MG86IFZi_XM
 Dilution equation:
 C1𝑉1 = 𝐶2𝑉2
 𝑀1𝑉1 = 𝑀2𝑉2

 Where:
 C1 = concentration of stock solution
 V1 = volume of stock solution
 C2 = concentration of dilute solution
 V2 = volume of dilute solution
SAMPLE PROBLEMS
 If 0.850 L of a 5.00-M solution of copper nitrate,
Cu(NO3)2, is diluted to a volume of 1.80 L by the
addition of water, what is the molarity of the
diluted solution?
 What volume of 0.12 M HBr can be prepared
from 11 mL (0.011 L) of 0.45 M HBr?
STANDARDIZATION
 process of determining the exact concentration
(molarity) of a solution.

 the concentration of the titrant that is unknown


and the moles of the analyte (primary standard)
are known
 Primary standard
 Substance in pure form or in a state of
known purity at reasonable cost and
stable at ambient temperatures
 KHP, NaC2O4 , K2Cr2O7
 Secondary Standards
 reagents that do not meet the criteria of the
primary standards
 The concentration of a secondary standard
must be determined relative to a primary
standard.
 Commercially available NaOH contains
impurities of NaCl, Na2CO3, and
Na2SO4, and readily absorbs H2O from
the atmosphere
STANDARDIZATION AND TITRATION
CALCULATIONS
𝑚𝑔 𝑠𝑡𝑎𝑛𝑑𝑎𝑟𝑑
 𝑚𝑚𝑜𝑙 𝑠𝑡𝑎𝑛𝑑𝑎𝑟𝑑 = 𝑚𝑔
𝐹𝑊 𝑠𝑡𝑎𝑛𝑑𝑎𝑟𝑑 (𝑚𝑚𝑜𝑙)
𝑚𝑚𝑜𝑙
 𝑚𝑚𝑜𝑙 𝑡𝑖𝑡𝑟𝑎𝑛𝑡 = 𝑀𝑡𝑖𝑡𝑟𝑎𝑛𝑡 𝑚𝑙
𝑥 𝑚𝑙𝑡𝑖𝑡𝑟𝑎𝑛𝑡
𝑡
= 𝑚𝑚𝑜𝑙𝑠𝑡𝑎𝑛𝑑𝑎𝑟𝑑 𝑥 𝑎 (𝑚𝑚𝑜𝑙𝑡𝑖𝑡𝑟𝑎𝑛𝑡 𝑥 𝑚𝑚𝑜𝑙𝑠𝑡𝑎𝑛𝑑𝑎𝑟𝑑)
𝑡 𝑚𝑚𝑜𝑙𝑡𝑖𝑡
𝑚𝑚𝑜𝑙 𝑚𝑚𝑜𝑙 𝑠𝑡𝑑
𝑥 (
𝑎 𝑚𝑚𝑜𝑙𝑠𝑡𝑑
)
 𝑀𝑡𝑖𝑡𝑟𝑎𝑛𝑡 =
𝑚𝑙 𝑚𝐿𝑡𝑖𝑡𝑟𝑎𝑛𝑡

 Combining all the steps at once,


𝑚𝑔 𝑡 𝑚𝑚𝑜𝑙𝑡𝑖𝑡
𝑚𝑚𝑜𝑙 𝑚𝑚𝑜𝑙𝑠𝑡𝑑 𝑥 𝐹𝑊 𝑥 (
𝑚𝑚𝑜𝑙 𝑎 𝑚𝑚𝑜𝑙𝑠𝑠𝑡𝑑)
 𝑀𝑡𝑖𝑡𝑟𝑎𝑛𝑡 =
𝑚𝑙 𝑚𝐿𝑡𝑖𝑡𝑟𝑎𝑛𝑡
 t/a= mole ratio between the titrant and analyte
found in the balance equation
SAMPLE PROBLEMS:
 An approximate 0.1M HCl solution is prepared by
120-fold dilution of concentrated HCl. It is
standardized by titrating 0.1876 g dried primary
standard sodium carbonate:
− +
𝐶𝑂32 + 2𝐻 𝐻2𝑂 + 𝐶𝑂2
The titration required 35.86 ml acid. Calculate
the molar concentration of the HCl.

Given: 0.1 M HCl, 0.1876 g Na2CO3; 35.86 ml acid


Unknown: MHCl = ?
 Solution:
𝑚𝑔𝑁𝑎2𝐶𝑂3
 MHCl= 𝐹𝑊𝑁𝑎2𝐶𝑂3
𝑥2𝑚𝑚𝑜𝑙𝐻𝐶𝑙/1𝑚𝑚𝑜𝑙𝑁𝑎2𝐶𝑂3
VHCl
mg
= (187.6 105.99mg x2 mmolHCl/mmol Na2CO3
mmol

35.86 ml
= 0.09872 mmol/ml
SAMPLE PROBLEMS
 A 50.00 ml volume of HCl solution required
29.71ml of 0.01963M Ba(OH)2 to reach an
endpoint with bromocresol green indicator.
Calculate the M of the acid.
 BaOH2 + 2 HCl BaCl2 + 2H2O

 Given:
 50.00 ml HCl; 29.71 ml of 0.01963M Ba(OH)2

 Unknown: M of HCl
 Solution:
𝐵𝑎 𝑂𝐻 2 2𝑚𝑚𝑜𝑙𝐻𝐶𝑙
 = 29.71𝑚𝑙 𝐵𝑎 𝑂𝐻 2 𝑥 0.01963 𝑚𝑚𝑜𝑙 𝑚𝑙 𝐵𝑎 𝑥
𝑂𝐻 2 1mmolBa OH 2

50.00 ml
= 0.0233 M
 A sample of pure sodium carbonate, Na2CO3 ,
weighing 0.3542 g is dissolved in water and
titrated with a solution of HCl. A volume of
30.23 ml is required to reach the methyl orange
endpoint, the reaction being
 Na2CO3 + 2HCl 2NaCl + H2O + CO2
 Calculate the N of the acid.

 Given:
 0.3542 g Na2CO3 ; 30.23ml HCl

 Unknown: NHCl
 Solution:
 From the given reaction above, there are 2
equivalents of Na2CO3 used in the neutralization
Therefore, the equivalent weight of Na2CO3 is
Na2CO3/2. The number of milliequivalents of
Na2CO3 is equal to the number of
milliequivalents of the acid used in the
neutralization.
wt Na2CO3 354.2 𝑚𝑔
= =NVHCl= 106𝑚𝑔
EW Na2CO3 2𝑚𝑒𝑞

30.23 ml
Ans: 0.2211 meq/ml
DETERMINATION OF SAMPLE PURITY
 Another application of titrimetric analysis is the
calculation of percent purity of a particular
sample.
 To analyze a sample of unknown purity, a
portion of the sample weighed, dissolved
appropriately and titrated with a standard
solution.
𝑚𝑔 𝑜𝑓 𝑎𝑛𝑎𝑙𝑦𝑡𝑒
 % 𝑝𝑢𝑟𝑖𝑡𝑦 = 𝑥 100%
𝑚𝑔 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒
SAMPLE PROBLEMS
Calculate the percent purity of a sample of

Mg(OH)2 if titration of 2.568 g of the sample
required 38.45 mL of 0.6695 M H3PO4.
Mg(OH)2 + H3PO4 Mg3(PO4)2 + H2O
 A sample of impure potassium acid phthalate
(KHP) weighing 2.1283g required 42.58ml of a
0.1084N base solution for titration to the
phenolphthalein endpoint. Calculate the % KHP
(EW=204.2) in the sample.
 Given:
 2.1283g KHP
 42.58ml of a 0.1084N base solution
 KHP: (EW=204.2)

 Unknown:
 %KHP
𝑚𝑒𝑞 𝑚𝑔
𝑉𝑚𝑙 𝑥𝑁 𝑚𝑙 𝑠𝑡𝑑𝑥 𝐸𝑊(𝑚𝑒𝑞)
 %KHP = 𝑥100
𝑤𝑡.𝑠𝑎𝑚𝑝𝑙𝑒(𝑚𝑔)
𝑚𝑒𝑞 𝑚𝑔
42.58𝑚𝑙 𝑥 0.1084 𝑚𝑙 𝑠𝑡𝑑𝑥 204.2(𝑚𝑒𝑞)
 = 𝑥100
2.1283(𝑚𝑔)
 = 44.29%
REFERENCE:
 Introduction to Analytical Chemistry by Skoog
 pp. 181- 195

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