CHEMISTRY FINALS Ultra micro <1 mg 0

Sources & Nature of Errors Classification of Analytes

o Accuracy – closeness of a result to its true or o Major constituents
accepted value o Minor constituents
o Precision – closeness of data to other data obtained o Trace constituents
the same way o Ultratrace constituents
o Replicates – samples of about the same size that are Steps in Quantitative Analysis
carried through an analysis in exactly the same way 1. Selection of a method
o Absolute error – difference between the measured - Cost, efficiency, and sensibility; sample and
value and the true value inference
o Relative error – absolute error divided by the true 2. Acquiring the sample
value - Sampling – process of acquiring a small amount
Types of Errors: of material whose composition accurately
o Random or indeterminate error – errors that affect represents the whole material
the precision of measurement 3. Processing the sample
o Systematic or determinate error – errors that affect - Sample preparation and replication
the accuracy of the result 4. Eliminating interference
Sources of Systematic Errors: - Interference - species that affect the
o Instrument errors – calibration eliminates most measurement of the analyte
instrument errors - Matrix – Species that does not affect the
o Method errors – most difficult to identify and correct measurement of the analyte
o Personal errors – based on personal judgment - Masking – to convert into non-interfering form
Classification of Method Analysis Acc. to Final 5. Measurement of the physical/ chemical property of
Measurement the analyte
o Gravimetric – how much of analyte is present in a 6. Calculation of the data
sample 7. Estimation of reliability of results
o Volumetric – volume Volumetric Method
o Instrumental – could vary o Types of titrimetric analysis
Ex. a. Volumetric
a. Electroanalytical (potential difference, voltage, b. Gravimetric
multimeter) c. Coulometric
b. Chromatography o Volumetric analysis – refers to any procedure in
c. Spectroscopic (electromagnetic radiation) which the volume of reagent needed to react with
Classification of Quantitative Analysis Acc. to Number of the analyte is measured
Analyte or Extent of Analysis Titration
o Complete/ ultimate o Process in which standard solution (titrant) is added
o Partial to a solution of an analyte until the reaction is
o Constituent judged to be complete
Acc. to Nature of Analyte o Analyte – the component of the sample that is to be
o Elemental determined
o Molecular o Titrant – added to the analyte until reaction is
Acc. to Concentration of Analyte complete; quantity of analyte based on quantity of
o Macro – major constituent (mostly present) titrant
o Trace – small amount present o Equivalence point – when amount of added titrant is
Acc. to Sample Size chemically equivalent to the amount of analyte in
Mass Volume the sample
Macro >100 mg >100 mL o End point – marked by a sudden change in the
Semi micro 10 – 100 mg 50 – 100 mL physical property of the solution
o Indicator – added to the analyte solution to give an
Micro 1 – 10 mg <50 mL
observable physical change
 o Over-step or over-run – amount of added titrant
exceeds the necessary amount for the end point
o Titrant error – difference in volume or mass of the
equivalence point and end point
o Direct titration – the titrant is added to the analyte
until the reaction is complete
o Back titration – known excess of standerd reagent is
added to the analyte
o Blank titration – same titration procedure is carried
out without the analyte Useful Formulas
Standardization
o Standard solution – reagent of exactly known
concentration
o Standardization – concentration of the titrant is
determined using a weighed amount of primary
standard
o Primary standard – highly purified compound that Indicators
serves as a reference material in titrimetric methods
o Important properties:
a. High purity
b. Stability towards air
c. Absence of hydrate water
d. Readily available at modest cost
e. Reasonable solubility at titration medium
f. Reasonably large molar mass
o Secondary standard – standard solution whose
purity has been established by standardization
Titration Technique
o Burette
a. Joseph Louis Gay-Lussac
b. Karl Friedrich Mohr
o Parallax error - occurs if the eye is either above or
below the level of the meniscus
Weighing Technique
o Triple-beam balance
o Analytical balance – analytical instrument of high Solubility Equilibrium
accuracy (up to 0.1 mg)
o Tare – resets the reading to zero
o Care for analytical balance:
1. Always keep weighing pan clean Factors that affect solubility
2. Use cloth or brush to remove spilled chemicals
3. Do not weigh more than capacity of balance
o Weighing by addition – sample is added carefully
into a container over tha pan of balance till desired
amount
o Weighing by difference – weighing bottle containing
the sample on a balance, sample then removed and
transferred to another container until desires
amount has been removed
Acid-Base Titration
o Titration based on neutralization reaction
o Alkalimetry - use of acid to determine the
concentration of a basic substance
o Acidimetry – use of base to determine the
concentration of an acidic substance
o At equivalence point, amount of acid is
stoichiometrically equivalent to amount of base
# of moles = # of moles base x RR
o RR – reaction ratio of acid and base from balanced
equation
o Dilution
- C1V1 = C2V2
o Molarity
- (M x VL)1 = (M x VL)2 x RR
o Normality
- (N x VL)1 = (N x VL)2
o Changes color at a certain pH range
o Weak acids and bases
o In acidic condition, the color of the acid form (HIn)
predominates.
o In alkaline condition, the color of the conjugate
base (In-) predominates
o Phenolphthalein
- Suitable for the titration of a strong acid with a
strong base whose end point is slightly above pH 7
and vice versa
a. Acid – colorless
b. Base – pink
o Bromothymol blue
a. Acid – yellow
b. Base – blue
o To choose the proper indicator, must change color at
a pH of the expected end point based on titration
curve
o Heterogeneous equilibrium
o Solid (precipitate) in equilibrium with ions in solution
(aqueous)
o Complex ion effect – increases solubility
o Common ion effect – decreases solubility
o Effect of pH:
1. Basic oxides more soluble in acidic solution
2. Acidic oxides more soluble in basic solution