Chemical analysis Flashcards
(25 cards)
Gravimetric analysis steps
🔹 Weighing sample to be analysed
🔹 Stirring sample into solvent
🔹 Filtering off undissolved solids
🔹 Adding excess reagent to precipitate with part of substance
🔹 Filtering, drying and weighing the precipitate
What does gravimetric analysis assume
🔹 Complete dissolving of all the substance being analysed for
🔹 None of the substance remains with the filtered undissolved solids
🔹 All of the substance that can precipitate, does so
🔹 Nothing else in the solution precipitates with the excess reagent
🔹 The precipitate is pure and completely dry before weighing
Error: if BaCl2 is not added in excess to precipitate the Sulfur in the fertiliser
🔹 Not all sulfate ions in the solution will precipitate to form ba2So4
🔹 Mass of BaSo4 in the crucible is lower, lower mole ratio
🔹 Mole of Sulfur is too low
🔹 Percentage of sulphur is too low
Errors leading to high mass of precipitate
1) Did not dry the precipitate completely.
2) Did not wash the precipitate with water to remove water soluble species such as those used to cause the precipitation.
3) Incorrectly weighed sample (e.g. fertilizer) and recorded a lower mass value than the real value - leads to a higher %w/w.
Errors leading to lower mass of precipitate and percentage of Sulfur
1) Incomplete precipitation reaction due to reasons such as not adding enough precipitating agent, not waiting long enough for reaction completion, precipitation performed at a low temperature (slow rate of reaction).
2) Not cooling reaction before filtration of precipitate as at higher temperature the precipitate will give better solubility.
3) Incomplete collection of precipitate due to reasons such as spilling precipitate or not completely collecting precipitate.
4) Incorrectly weighed sample (e.g. fertilizer) and recorded a higher mass value than the real value - leads to a lower %w/w.
Standard solution
Solution of accurately known concentration
Primary standard
A substance for which an accurately known amount can be dissolved to make an accurately known volume of solution to determine an accurate concentration
What must a primary standard be
🔹 Pure and have a known formula (with high relative mass)
🔹 Be soluble, inexpensive and have a high relative mass
🔹 Not change composition during storage
Why are NaOH and HCl not suitable primary standards
🔹 NaOH reacts with Co2 and absorbs water from the atmosphere
🔹 Pure HCl is a gas, difficult to completely dissolve a known mass
These substances would need to be made to an approximate concentration and then standardised using a titration (secondary standard solutions)
Aliquot
Accurate volume of a solution delivered by a pipette
Equivalence point
The point in a titration where there is no excess of either reactant according to the stoichiometry of the equation
Endpoint
The point in a titration when there is a permanent colour change
Burette
Delivers an accurate volume (titre)
Rinse with solution it is to deliver
Volumetric flask
Makes up standard solutions
Rinse with deionised water
Pipette
Delivers an accurate volume called an aliquot
Rinse with solution it is to deliver
Conical flask
Holds aliquot during titration
Rinse with deionised water
What happens if burette is not rinsed with solution it is to deliver?
The water would dilute the added HCl and the volume of titre would be too high. Calculated concentration of HCl is too low
What happens if conical flask is rinsed with na2co3 solution
Extra Na2Co3 is not present in addition to the known amount of sodium carbonate that came from the pipette.
Extra amount of na2co3 means extra volume of titres. Titres too big so concentration of HCl calculated is too low
Why is volumetric flask rinsed with water
Amount of Na2Co3 is the same as water will be added regardless to the calibration line to produce the standard solution
What happens if pipette is not rinsed with sodium carbonate solution
This dilutes the Na2Co3 so the amount of sodium carbonate in the aliquot is less than it should be. Titres are too small.
Calculated concentration of HCl too high
What happens if endpoint was overshot
Too much HCl added from burette. Titres too big and amount of HCl too high so,ethics
What happens if sodium carbonate was partially hydrated
For a given mass of powder there will be less actual na2Co3 as some of the mass is h2o. So titres of HCl a lower volume than they should be.
Calculated concentration of HCl too high
Why is so and so a good indicator for this titration?
So and so changes colour between 1-3. The ph at the equivalence point is 3. This indicator captures the equivalence point and so end point will be a good approximation of equivalence point
What happens if an indicator who changes colour at a lower ph was used
Methyl orange changes colour between so and so, as such the colour change will be well before the equivalence point and the volume of the titre will be too low