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Title: Titration
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TITRATION
CONTENTS
History and etymology 1
Procedure 2
Preparation techniques 2.1
Titration curves 3
Types of titrations 4
Acid–base titration 4.1
Redox titration 4.2
Gas phase titration 4.3
Complexometric titration 4.4
Zeta potential titration 4.5
Assay 4.6
Measuring the endpoint of a titration 5
Endpoint and equivalence point 5.1
Back titration 5.2
Graphical Methods 6
Particular uses 7
HISTORY AND See also 8
ETYMOLOGY References 9
\mathbf{C}_a=\frac{\mathbf{C}_{t}\mathbf{V}_{t}\mathbf{M}}{\mathbf{V}_a}
where Ca is the concentration of the analyte, typically in molarity
(/articles/eng/Molarity); Ct is the concentration of the titrant, typically in molarity; Vt is
the volume of the titrant used, typically in liters; M is the mole ratio of the analyte and
reactant from the balanced chemical equation (/articles/eng/Chemical_equation); and
Va is the volume of the analyte used, typically in liters.[6]
P R E PA R AT I O N T E C H N I Q U E S
Typical titrations require
titrant and analyte to be in
a liquid (solution) form.
Though solids are usually
dissolved into an aqueous
solution, other solvents
such as glacial acetic acid
In instances where two reactants in a sample may react with the titrant and only one is
the desired analyte, a separate masking solution (/articles/eng/Masking_agent) may
be added to the reaction chamber which masks the unwanted ion.[9]
Some redox (/articles/eng/Redox) reactions may require heating the sample solution
and titrating while the solution is still hot to increase the reaction rate
(/articles/eng/Reaction_rate). For instance, the oxidation of some oxalate solutions
requires heating to 60 °C (140 °F) to maintain a reasonable rate of reaction.[10]
TITRATION CURVES
A titration curve is a curve in the plane whose x-coordinate is the volume of titrant
(/articles/eng/Titrant) added since the beginning of the titration, and whose y-
coordinate is the concentration of the analyte at the corresponding stage of the
titration (in an acid-base titration, the y-coordinate is usually the pH of the solution).[11]
In an acid-base titration, the titration curve re ects the strength of the corresponding
acid and base. For a strong acid and a strong base, the curve will be relatively smooth
and very steep near the equivalence point. Because of this, a small change in titrant
volume near the equivalence point results in a large pH change and many indicators
would be appropriate (for instance litmus (/articles/eng/Litmus_test), phenolphthalein
(/articles/eng/Phenolphthalein) or bromothymol blue
(/articles/eng/Bromothymol_blue)).
If one reagent is a weak acid or base and the other is a strong acid or base, the
titration curve is irregular and the pH shifts less with small additions of titrant near the
equivalence point. For example, the titration curve for the titration between oxalic acid
(/articles/eng/Oxalic_acid) (a weak acid) and sodium hydroxide
(/articles/eng/Sodium_hydroxide) (a strong base) is pictured. The equivalence point
occurs between pH 8-10, indicating the solution is basic at the equivalence point and
an indicator such as phenolphthalein (/articles/eng/Phenolphthalein) would be
appropriate. Titration curves corresponding to weak bases and strong acids are
similarly behaved, with the solution being acidic at the equivalence point and
indicators such as methyl orange (/articles/eng/Methyl_orange) and bromothymol
blue (/articles/eng/Bromothymol_blue) being most appropriate.
Titrations between a weak acid and a weak base have titration curves which are highly
irregular. Because of this, no de nite indicator may be appropriate and a pH meter
(/articles/eng/PH_meter) is often used to monitor the reaction.[12]
The type of function that can be used to describe the curve is called a sigmoid
function (/articles/eng/Sigmoid_function).
TYPES OF TITRATIONS
There are many types of titrations with different procedures and goals. The most
common types of qualitative titration are acid-base titrations (/articles/eng/Acid-
base_titration) and redox titrations (/articles/eng/Redox_titration).
AC I D – B A S E T IT R AT I O N
Indicator Color on acidic side Range of color change Color on basic side
For very strong bases, such as metal amides, and hydrides (/articles/eng/Hydride),
water is generally not a suitable solvent and indicators whose pKa (/articles/eng/PKa)
are in the range of aqueous pH changes are of little use. Instead, the titrant and
indicator used are much weaker acids, and anhydrous solvents such as THF
(/articles/eng/THF) are used.[14][15]
R E D OX T IT R AT I O N
Redox titrations are based on a reduction-oxidation reaction (/articles/eng/Redox)
between an oxidizing agent and a reducing agent. A potentiometer
(/articles/eng/Potentiometer) or a redox indicator (/articles/eng/Redox_indicator) is
usually used to determine the endpoint of the titration, as when one of the
constituents is the oxidizing agent potassium dichromate
(/articles/eng/Potassium_dichromate). The color change of the solution from orange
to green is not de nite, therefore an indicator such as sodium diphenylamine is used.
[16] Analysis of wines for sulfur dioxide (/articles/eng/Sulfur_dioxide) requires iodine
as an oxidizing agent. In this case, starch is used as an indicator; a blue starch-iodine
complex is formed in the presence of excess iodine, signalling the endpoint.[17]
Some redox titrations do
not require an indicator,
due to the intense color of
the constituents. For
instance, in
permanganometry
(/articles/eng/File:Iodometric_titration_mixture.jpg)
Color of iodometric
(/articles/eng/Iodometry) titration
mixture before (left) and after (right) the
end point
G A S P H A S E T IT R AT I O N
Gas phase titrations are
titrations done in the gas
phase
O3 + NO → O2 + NO2.[19][20]
After the reaction is complete, the remaining titrant and product are quanti ed (e.g., by
FT-IR (/articles/eng/Fourier_transform_spectroscopy)); this is used to determine the
amount of analyte in the original sample.
C O M P L E XO M E T R I C T IT R AT I O N
Complexometric titrations
rely on the formation of a
complex
Z E TA P OT E NT I A L T IT R AT I O N
Zeta potential titrations are titrations in which the completion is monitored by the zeta
potential (/articles/eng/Zeta_potential), rather than by an indicator
(/articles/eng/PH_indicator), in order to characterize heterogeneous
(/articles/eng/Heterogeneous) systems, such as colloids (/articles/eng/Colloid).[23]
One of the uses is to determine the iso-electric point (/articles/eng/Iso-electric_point)
when surface charge (/articles/eng/Surface_charge) becomes zero, achieved by
changing the pH (/articles/eng/PH) or adding surfactant (/articles/eng/Surfactant).
Another use is to
determine the optimum
dose for occulation
A S S AY
An assay is a form of
biological titration used to
determine the
concentration of a virus
(/articles/eng/Virus) or
bacterium
(/articles/eng/Bacterium).
Serial dilutions are
performed on a sample in
a xed ratio (such as 1:1,
1:2, 1:4, 1:8, etc.) until the
last dilution does not give
a positive test for the
presence of the virus. The
positive or negative value
may be determined by
visually inspecting the
infected cells under a
microscope (/articles/eng/Microscope) or by an immunoenzymetric method such as
enzyme-linked immunosorbent assay (/articles/eng/ELISA) (ELISA). This value is
known as the titer (/articles/eng/Titer).[25]
MEASURING THE ENDPOINT OF A TITRATION
Different methods to determine the endpoint include:[26]
Indicator: A substance that changes color in response to a chemical change. An acid-base indicator
(/articles/eng/PH_indicator) (e.g., phenolphthalein (/articles/eng/Phenolphthalein)) changes color
depending on the pH. Redox indicators (/articles/eng/Redox_indicator) are also used. A drop of
indicator solution is added to the titration at the beginning; the endpoint has been reached when the
color changes.
Potentiometer (/articles/eng/Potentiometer_(measuring_instrument)): An instrument that measures
the electrode potential (/articles/eng/Electrode_potential) of the solution. These are used for redox
titrations; the potential of the working electrode will suddenly change as the endpoint is reached.
pH meter (/articles/eng/PH_meter): A potentiometer with an electrode whose potential depends on
the amount of H+ ion present in the solution. (This is an example of an ion-selective electrode
(/articles/eng/Ion-selective_electrode).) The pH of the solution is measured throughout the titration,
more accurately than with an indicator; at the endpoint there will be a sudden change in the
measured pH.
Conductivity (/articles/eng/Electrical_conductivity): A measurement of ions in a solution. Ion
concentration can change signi cantly in a titration, which changes the conductivity. (For instance,
during an acid-base titration, the H+ and OH− ions react to form neutral H2O.) As total conductance
depends on all ions present in the solution and not all ions contribute equally (due to mobility
(/articles/eng/Electrophoretic_mobility) and ionic strength (/articles/eng/Ionic_strength)), predicting
the change in conductivity is more dif cult than measuring it.
Color change: In some reactions, the solution changes color without any added indicator. This is
often seen in redox titrations when the different oxidation states of the product and reactant produce
different colors.
Precipitation (/articles/eng/Precipitation_(chemistry)): If a reaction produces a solid, a precipitate
will form during the titration. A classic example is the reaction between Ag+ and Cl− to form the
insoluble salt AgCl. Cloudy precipitates usually make it dif cult to determine the endpoint precisely.
To compensate, precipitation titrations often have to be done as "back" titrations (see below).
Isothermal titration calorimeter (/articles/eng/Calorimeter#Isothermal_titration_calorimeter): An
instrument that measures the heat produced or consumed by the reaction to determine the endpoint.
Used in biochemical (/articles/eng/Biochemistry) titrations, such as the determination of how
substrates (/articles/eng/Substrate_(biochemistry)) bind to enzymes (/articles/eng/Enzyme).
Thermometric titrimetry (/articles/eng/Thermometric_Titration): Differentiated from calorimetric
titrimetry because the heat of the reaction (as indicated by temperature rise or fall) is not used to
determine the amount of analyte in the sample solution. Instead, the endpoint is determined by the
rate of temperature change.
Spectroscopy (/articles/eng/Spectroscopy): Used to measure the absorption of light by the solution
during titration if the spectrum (/articles/eng/Spectrum) of the reactant, titrant or product is known.
The concentration of the material can be determined by Beer's Law (/articles/eng/Beer%27s_Law).
Amperometry (/articles/eng/Amperometric_titration): Measures the current produced by the titration
reaction as a result of the oxidation or reduction of the analyte. The endpoint is detected as a change
in the current. This method is most useful when the excess titrant can be reduced, as in the titration
of halides (/articles/eng/Halide) with Ag+.
E N D P O I NT A N D E Q U I VA L E N C E P O I NT
Though equivalence point and endpoint are used interchangeably, they are different
terms. Equivalence point is the theoretical completion of the reaction: the volume of
added titrant at which the number of moles (/articles/eng/Mole_(unit)) of titrant is
equal to the number of moles of analyte, or some multiple thereof (as in polyprotic
(/articles/eng/Polyprotic) acids). Endpoint is what is actually measured, a physical
change in the solution as determined by an indicator (/articles/eng/PH_indicator) or
an instrument mentioned above.[27]
There is a slight difference between the endpoint and the equivalence point of the
titration. This error is referred to as an indicator error, and it is indeterminate.[28]
B AC K T IT R AT I O N
Back titration is a titration done in reverse; instead of titrating the original sample, a
known excess of standard reagent is added to the solution, and the excess is titrated.
A back titration is useful if the endpoint of the reverse titration is easier to identify than
the endpoint of the normal titration, as with precipitation
(/articles/eng/Precipitation_(chemistry)) reactions. Back titrations are also useful if
the reaction between the analyte and the titrant is very slow, or when the analyte is in a
non-soluble (/articles/eng/Solubility) solid.[29]
GRAPHICAL METHODS
The titration process creates solutions with compositions ranging from pure acid to
pure base. Identifying the pH associated with any stage in the titration process is
relatively simple for monoprotic acids and bases. The presence of more than one acid
or base group complicates these computations. Graphical methods,[30] such as the
equiligraph,[31] have long been used to account for the interaction of coupled equilibria.
These graphical solution methods are simple to implement, however they are
infrequently used.
PARTICULAR USES
Speci c examples of titrations include:
Acid-Base Titrations
In biodiesel (/articles/eng/Biodiesel): Waste vegetable oil (/articles/eng/Vegetable_oil_fuel) (WVO)
must be neutralized before a batch may be processed. A portion of WVO is titrated with a base to
determine acidity, so the rest of the batch may be properly neutralized. This removes free fatty acids
(/articles/eng/Fatty_acid#Free_fatty_acids) from the WVO that would normally react to make soap
instead of biodiesel.[32]
ammonia with sulfuric acid (/articles/eng/Sulfuric_acid) and potassium sulfate
(/articles/eng/Potassium_sulfate). Finally, ammonia is back titrated with boric acid
(/articles/eng/Boric_acid) and then sodium carbonate (/articles/eng/Sodium_carbonate).[33]
Acid value (/articles/eng/Acid_value): The mass in milligrams of potassium hydroxide
(/articles/eng/Potassium_hydroxide) (KOH) required to titrate fully an acid in one gram of sample. An
example is the determination of free fatty acid (/articles/eng/Fatty_acid#Free_fatty_acids) content.
Saponi cation value (/articles/eng/Saponi cation_value): The mass in milligrams of KOH required to
saponify a fatty acid (/articles/eng/Fatty_acid) in one gram of sample. Saponi cation is used to
determine average chain length of fatty acids in fat.
Ester value (or ester index): A calculated index. Ester value = Saponi cation value – Acid value.
Amine value: The mass in milligrams of KOH equal to the amine (/articles/eng/Amine) content in one
gram of sample.
Hydroxyl value (/articles/eng/Hydroxyl_value): The mass in milligrams of KOH corresponding to
hydroxyl (/articles/eng/Hydroxyl) groups in one gram of sample. The analyte is acetylated
(/articles/eng/Acetylation) using acetic anhydride (/articles/eng/Acetic_anhydride) then titrated with
KOH.
Redox titrations
Winkler test for dissolved oxygen (/articles/eng/Winkler_test_for_dissolved_oxygen): Used to
determine oxygen concentration in water. Oxygen in water samples is reduced using manganese(II)
sulfate (/articles/eng/Manganese(II)_sulfate), which reacts with potassium iodide
(/articles/eng/Potassium_iodide) to produce iodine (/articles/eng/Iodine). The iodine is released in
proportion to the oxygen in the sample, thus the oxygen concentration is determined with a redox
titration of iodine with thiosulfate (/articles/eng/Thiosulfate) using a starch indicator.[34]
Vitamin C (/articles/eng/Vitamin_C): Also known as ascorbic acid, vitamin C is a powerful reducing
agent. Its concentration can easily be identi ed when titrated with the blue dye
Dichlorophenolindophenol (DCPIP (/articles/eng/Dichlorophenolindophenol)) which turns colorless
when reduced by the vitamin.[35]
Benedict's reagent (/articles/eng/Benedict%27s_reagent): Excess glucose (/articles/eng/Glucose) in
urine may indicate diabetes (/articles/eng/Diabetes) in the patient. Benedict's method is the
conventional method to quantify glucose in urine using a prepared reagent. In this titration, glucose
reduces cupric (/articles/eng/Copper) ions to cuprous ions which react with potassium thiocyanate
(/articles/eng/Potassium_thiocyanate) to produce a white precipitate, indicating the endpoint.[36]
Bromine number (/articles/eng/Bromine_number): A measure of unsaturation
(/articles/eng/Saturation_(chemistry)) in an analyte, expressed in milligrams of bromine absorbed by
100 grams of sample.
Iodine number (/articles/eng/Iodine_number): A measure of unsaturation in an analyte, expressed in
grams of iodine absorbed by 100 grams of sample.
Miscellaneous
Karl Fischer titration (/articles/eng/Karl_Fischer_titration): A potentiometric method to analyze trace
amounts of water in a substance. A sample is dissolved in methanol (/articles/eng/Methanol), and
titrated with Karl Fischer reagent. The reagent contains iodine, which reacts proportionally with
water. Thus, the water content can be determined by monitoring the potential
(/articles/eng/Electric_potential) of excess iodine.[37]
SEE ALSO
Acid (/articles/eng/Acid)
Base (/articles/eng/Base_(chemistry))
Nonaqueous titration (/articles/eng/Nonaqueous_titration)
EXTERNAL LINKS
Wikihow: Perform a Titration
An interactive guide to titration
Science Aid: A simple explanation of titrations including calculation examples
Titration freeware - simulation of any pH vs. volume curve, distribution diagrams and real data
analysis
Graphical method to solve acid-base problems, including titrations
Graphic and numerical solver for general acid-base problems - Software Program for phone and
tablets
Analytical chemistry (/articles/eng/Analytical_chemistry)
Atomic absorption spectrometer
(/articles/eng/Atomic_absorption_spectroscopy) |
Flame emission spectrometer
(/articles/eng/Flame_emission_spectroscopy) |
Gas chromatograph (/articles/eng/Gas_chromatography) |
High-performance liquid chromatograph
(/articles/eng/High-performance_liquid_chromatography)
|
Instrumentation (/articles/eng/Measuring_instrument)
Infrared spectrometer
(/articles/eng/Infrared_spectroscopy) |
Mass spectrometer (/articles/eng/Mass_spectrometry) |
Melting point apparatus
(/articles/eng/Melting_point_apparatus) |
Microscope (/articles/eng/Microscope) |
Spectrometer (/articles/eng/Spectrometer) |
Spectrophotometer (/articles/eng/Spectrophotometry)
Calorimetry (/articles/eng/Calorimetry) |
Chromatography (/articles/eng/Chromatography) |
Electroanalytical methods
Techniques (/articles/eng/Electroanalytical_method) |
Gravimetric analysis (/articles/eng/Gravimetric_analysis) |
Mass spectrometry (/articles/eng/Mass_spectrometry) |
Spectroscopy (/articles/eng/Spectroscopy)
Chemometrics (/articles/eng/Chemometrics) |
Calibration curve (/articles/eng/Calibration_curve) |
Matrix effect (/articles/eng/Matrix_(chemical_analysis)) |
Calibration
Internal standard (/articles/eng/Internal_standard) |
Standard addition (/articles/eng/Standard_addition) |
Isotope dilution (/articles/eng/Isotope_dilution)
Analyst (/articles/eng/Analyst_(journal)) |
Analytica Chimica Acta
(/articles/eng/Analytica_Chimica_Acta) |
Analytical and Bioanalytical Chemistry
Prominent publications
(/articles/eng/Analytical_and_Bioanalytical_Chemistry) |
(/articles/eng/List_of_important_publications_in_chemistry#Analytical_chemistry)
Analytical Chemistry
(/articles/eng/Analytical_Chemistry_(journal)) |
Analytical Biochemistry
(/articles/eng/Analytical_Biochemistry)
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