1.

Karl Fischer:
Karl Fischer titration is a widely used analytical method for quantifying water content
in a variety of products. The fundamental principle behind it is based on the Bunsen
reaction between iodine and sulfur dioxide in an aqueous medium. Karl Fischer
discovered that this reaction could be modified to be used for the determination of
water in a non-aqueous system containing an excess of sulfur dioxide. He used a
primary alcohol (methanol) as the solvent, and a base (pyridine) as the buffering
agent.
How does it work?
Water and iodine are consumed in a 1:1 ratio in the above reaction. Once all of the
water present is consumed, the presence of excess iodine is detected voltametrically
by the titrator's indicator electrode. That signals the end-point of the titration.
The amount of water present in the sample is calculated based on the concentration of
iodine in the Karl Fischer titrating reagent (i.e. titre) and the amount of Karl Fischer
reagent consumed in the titration.
http://www.monash.edu/science/research-groups/chemistry/ionicliquids/equipment/kf
Gas Chromatography:
Principle of gas chromatography: The sample solution injected into the instrument
enters a gas stream which transports the sample into a separation tube known as the
"column." (Helium or nitrogen is used as the so-called carrier gas.) The various
components are separated inside the column. The detector measures the quantity of
the components that exit the column. To measure a sample with an unknown
concentration, a standard sample with known concentration is injected into the
instrument. The standard sample peak retention time (appearance time) and area are
compared to the test sample to calculate the concentration.
http://www.shimadzu.eu/gas-chromatography
High Performance Liquid Chromatography:
High performance liquid chromatography (HPLC) is a separation technique utilizing
differences in distribution of compounds to two phases, called stationary phase and
mobile phase. The stationary phase designates a thin layer created on the surface of
fine particles and the mobile phase designates the liquid flowing over the particles.
Under a certain dynamic condition, each component in a sample has a different
distribution equilibrium depending on solubility in the phases and/or molecular size.
As a result, the components move at different speeds over the stationary phase and are
thereby separated from each other. This is the principle behind HPLC. The column is
a stainless steel (or resin) tube which is packed with spherical solid particles. Mobile
phase is constantly fed into the column inlet at a constant rate by a liquid pump. A
sample is injected from a sample injector, located near the column inlet. The injected
sample enters the column with the mobile phase and the components in the sample
migrate through it, passing between the stationary and mobile phases. Compounds
move in the column only when is in the mobile phase. Compounds that tend to be
distributed in the mobile phase therefore migrate faster through the column while
compounds that tend to be distributed in the stationary phase migrate slower. In this
way, each component is separated on the column and sequentially elutes from the

outlet. Each compound eluting from the column is detected by a detector connected to
the outlet of the column.
When the separation process is monitored by the recorder starting at the time the
sample is injected, a graph is obtained. This graph is called a chromatogram. The time
required for a compound to elute (called retention time) and the relationship between
compound concentration (amount) and peak area depend on the characteristics of the
compound. Retention time is therefore used as an index for qualitative determination
and peak surface area (or height) as an index for quantitative determination. The
retention time of the target compounds and the concentration for each unit of peak
area are based on data obtained in advance by analyzing a sample with known
quantities of the reference standards. Normally, the reference standards are highly
purified target compounds.
A HPLC system is basically composed of 1) a pump, 2) an injector, 3) a column, 4) a
column oven and 5) detector, as shown in Fig.4.1.10.
http://nett21.gec.jp/CTT_DATA/WMON/CHAP_4/html/Wmon-085.html
2. In liquid chromatography (LC), the flowing or mobile phase is a liquid, whereas in
gas chromatography (GC) is a gas.
The GC-MS system is equipped to allow for either Electron Ionization (EI), or
Chemical Ionization (CI) both in either positive or negative ion mode. In addition the
GC can be run as a stand-alone component, with detection using a Flame Ionization
Detector (FID).
The HPLC system can also be run coupled to the MS or with its own internal UV
detector.HPLC offers the ability to analyse compounds which do not lend themselves
to GC methods, and can cope with compounds that are less thermally stable, that have
a high molecular mass, or that are highly polar. The LC-MS can be equipped with
APCI or electrospray sources.
Ideal solvents for GC methods are volatile solvents such as hexane, diethyl ether or
dicholromethane.
For HPLC methods more polar solvents such as water and water mixtures, methanol
and acetonitrile maybe used.
http://www.jcu.edu.au/aac/facilities/instruments/JCUTST_056353.html
What are the main differences between High Performance Liquid
Chromatography and Gas Chromatography?
In HPLC the mobile phase is a liquid whereas in GC the mobile phase or
carrier is a gas.
HPLC is useful for analysis of samples which are liable to decompose at
higher temperatures. GC involves high temperatures so compounds are stable
at such temperatures.
GC is applied for analysis of volatile compounds whereas non volatile
compounds can be easily analyzed on HPLC.
GC cannot be used for analysis of high molecular weight molecules whereas
HPLC has applications for separation and identification of very high
molecular weight compounds.

HPLC requires higher operating pressures than GC because liquids require

higher pressures than gases for transport through the system.
HPLC columns are short and wide in comparison to GC columns
http://lab-training.com/landing/free-hplc-training-programme-11/
3. 1. MS/MX/MF/ML is a heating and drying method analyzer that compares weight
before and after heating and drying, while a Karl Fischer type analyzer titrates KF
reagent that contains iodine to sample electric-chemically.
2. Karl Fischer method enables a measurement from some ppm to 100% (water), but
operation is complicated and the unit is expensive. MS/MX/MF/ML is very easy to
handle, needs short time to measure and is reasonably priced.
3. Where required resolution is under 0.01% MS/MX is more suitable in terms of
handling, accuracy and running cost. There is no difference between data obtained
with the Karl Fischer method and heating and drying method; however MS/MX is
more likely to have better repeatability than a Karl Fischer type.
http://www.aandd.jp/support/moisturefaq.html#q1