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CHEMISTRY FINALS

Sources & Nature of Errors


o Accuracy closeness of a result to its true or
accepted value
o Precision closeness of data to other data obtained
the same way
o Replicates samples of about the same size that are
carried through an analysis in exactly the same way
o Absolute error difference between the measured
value and the true value
o Relative error absolute error divided by the true
value
Types of Errors:
o Random or indeterminate error errors that affect
the precision of measurement
o Systematic or determinate error errors that affect
the accuracy of the result
Sources of Systematic Errors:
o Instrument errors calibration eliminates most
instrument errors
o Method errors most difficult to identify and correct
o Personal errors based on personal judgment
Classification of Method Analysis Acc. to Final
Measurement
o Gravimetric how much of analyte is present in a
sample
o Volumetric volume
o Instrumental could vary
Ex.
a. Electroanalytical (potential difference, voltage,
multimeter)
b. Chromatography
c. Spectroscopic (electromagnetic radiation)
Classification of Quantitative Analysis Acc. to Number of
Analyte or Extent of Analysis
o Complete/ ultimate
o Partial
o Constituent
Acc. to Nature of Analyte
o Elemental
o Molecular
Acc. to Concentration of Analyte
o Macro major constituent (mostly present)
o Trace small amount present
Acc. to Sample Size
Mass
Volume
Macro
>100 mg
>100 mL
Semi micro
10 100 mg
50 100 mL
Micro
1 10 mg
<50 mL

Ultra micro

<1 mg

Classification of Analytes
o Major constituents
o Minor constituents
o Trace constituents
o Ultratrace constituents
Steps in Quantitative Analysis
1. Selection of a method
Cost, efficiency, and sensibility; sample and
inference
2. Acquiring the sample
Sampling process of acquiring a small amount
of material whose composition accurately
represents the whole material
3. Processing the sample
Sample preparation and replication
4. Eliminating interference
Interference - species that affect the
measurement of the analyte
Matrix Species that does not affect the
measurement of the analyte
Masking to convert into non-interfering form
5. Measurement of the physical/ chemical property of
the analyte
6. Calculation of the data
7. Estimation of reliability of results
Volumetric Method
o Types of titrimetric analysis
a. Volumetric
b. Gravimetric
c. Coulometric
o Volumetric analysis refers to any procedure in
which the volume of reagent needed to react with
the analyte is measured
Titration
o Process in which standard solution (titrant) is added
to a solution of an analyte until the reaction is
judged to be complete
o Analyte the component of the sample that is to be
determined
o Titrant added to the analyte until reaction is
complete; quantity of analyte based on quantity of
titrant
o Equivalence point when amount of added titrant is
chemically equivalent to the amount of analyte in
the sample
o End point marked by a sudden change in the
physical property of the solution
o Indicator added to the analyte solution to give an
observable physical change

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
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
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
accuracy (up to 0.1 mg)
o Tare resets the reading to zero
o Care for analytical balance:
1. Always keep weighing pan clean
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

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
Useful Formulas
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
Indicators
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
Solubility Equilibrium
o Heterogeneous equilibrium
o Solid (precipitate) in equilibrium with ions in solution
(aqueous)
Factors that affect solubility
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

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