Chapter 9C - Volumetric Analysis
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What is volumetric analysis?
• quantitative technique • involves measuring volume of a solution of known concentration to determine the concentration of the analyte • titration process
What are the steps to volumetric analysis?
• Preperation of a standard solution using a primary standard • Titration b/w standard solution & solution to be standardised • Titration b/w standardised solution & solution being analysed • Stochiometric calculations to determine the concentration of the solution being analysed
Volumetric flask
• used for measuring a fixed volume (commonly 100 or 250mL) • used to prepare a standard solution (known concentration) • rinse with distilled water
Pipette
• used for measuring a fixed volume (aliquot) • commonly 20 or 25mL • used to transfer a known volume of the solution being analysed to the conical flask • rinse with the solution it is to contain
Burette
• measure a variable volume (titre) • holds up to 50mL • usually contains the standard solution (known concentration) • rinse w/ the solution it is to contain
Concentration
• amount of solute in a specified volume of solvent/solution
Conical flask
• used for holding the aliquot delivered from the pipette • rinse w/ distilled water
Molarity
• amount of substance (mol) per volume of solution (L)
Percentage by mass
• %m/m • mass of component (g) per 100g sample/solution
Percentage by volume
• %v/v • volume of solute (mL) per 100mL solution
Percentage mass/volume
• %m/v • mass of solute (g) per 100mL solution
Parts per million (ppm)
• mass of solute (mg) per kg of solution • mass of solute (mg) per L of solution
What is a standard solution?
• solution w/ accurately known concentration • prepared in volumetric flask • prepared using a primary standard
What is a primary standard?
• available in pure form • has a known formula • is stable enough to not react w/ atmosphere or decompose over time • reasonably high molar mass to minimise weighting errors • inexpensive
Standardisation
A standard solution is used to standardise another solution
What is a titration?
Involves adding one solution (oxidant/reductant) to another solution (oxidant/reductant) until the reaction b/w them is complete
Equivalence Point
Point at which the ratio of oxidising agent to reducing agent present is equivalent to the stochiometric mole ratios in the equation
End point
When the reaction solution changes colour (due to the indicator or one of the chemicals involved in the redox reaction)
What are steps of the titration process?
• Rinse & fill a pipette w/ the analyte. Transfer aliquot to a conical flask • Add several drops of a suitable indicator to the conical flask if the reaction is not self indicating • Rinse & fill a burette w/ standard solution. Record initial burette reading • Titrate analyte w/ known solution until endpoint reached. Record final burette reading and titre • Repeat until 3 concordant titres obtained
What are concordant titres?
• 0.1mL b/w lowest & highest titre • increases reliability/precision • minimises effect of random errors
What type of experimental errors are associated with volumetric analysis?
• rinsing errors • indicator errors
Why do rinsing errors need to be considered?
• lead to overestimations or underestimations of the final analyte concentration
What happens if the pipette is rinsed with water?
• decrease reactant amount (in mol) in the aliquot delivered to the conical flask • decreases size of titre • underestimated concentration
What happens if the pipette is rinsed with a more concentrated solution?
• increase reactant amount (in mol) in the aliquot delivered to the conical flask • increases size of titre • overestimated concentration