 Catalyst used in petroleum and

chemical refining is poisoned by trace

amounts of nitrogenous materials are
contained in feedstock’s
 Some nitrogen compounds are also
corrosive.
 Crude oils with nitrogen contents greater
than 0.25wt% requires treatment in
refineries for nitrogen removal.
 To determine bound nitrogen in process
feeds and may also be used to control
nitrogen compounds in finished products
 Prevent gum formation in finished
product.
 Most prominent nitrogen containing
classes in crude oil are pyridine, pyridine
derivatives and pyrrole derivatives,
including porphyrins.
 Hetero-atoms that are identified were
amides, hydroxy-quinolines, pyrrole-
carboxylic acids, imidazoles, caffeines,
etc.
ASTM D 5762 is one of the method in ASTM
to determine Nitrogen content in crude oil
 At high temperature nitrogen presents in
a crude oil converted into nitric oxide
(NO). The NO contacts ozone and is
converted to excited nitrogen dioxide
(NO2). The light emitted as the excited
NO2 decays is detected by a
photomultiplier tube and the resulting
signal is a measure of the nitrogen
contained in the sample.
 Nitrogen analysis begins with high
temperature oxidation of the entire sample.

 The sample is combusted with oxygen at a

temperature of 1050 ºC. The oxidation
products include CO2, H2O, NO, SO2, and
various other oxides.
 The combustion gases are routed through a
membrane drying system to remove moisture
and then to the nitrogen detector module
for quantification.
 NO is contacted with O3 (ozone),
produced by an onboard generator, to
form NO2 (metastable nitrogen dioxide).
 Boat inlet system: Boats are made up from
platinum or quartz. Small piece of quartz
wool is fitted to boat to provide liquid
injection. It should be cleaned by swapping
inert gas.
 Chemiluminescence Detector: It is used to
measure light emitted from the reaction
between nitric oxide and ozone.
 Combustion Tube: It is made up of quartz.
The inlet end of the tube shall be large
enough to accept the sample and have
side arms to introduce oxygen and inert gas
for cleaning.
 Drier tube: To remove water vapour which
can be done by using magnesium per-
chlorate Mg (ClO4)2 or membrane drying or
chilled dehumidifier assembly.
 Electric furnace: To maintain temperature for
pyrolysis of sample for conversion of nitrogen
to NO.
 Temperature controller: For safety purpose to
maintain temperature below 1100 ºC in single
zone tube but in case of two zone tube 1050
ºC has to be maintain in each zone.
 Micro-syringe: Capacity of 5 or 10 µL to
provide sample.
 Ozone detector and Recorder: To supply
ozone to the detector reaction cell and to
display signal.
 Prepare a test specimen solution by dilution of the test
specimen in xylene. The nitrogen concentration in the test
specimen solution shall be less than the concentration of
the highest standard used in calibration and greater than
3 mg nitrogen/ul.
 Record the mass of the test specimen and the total mass
of the test specimen and solvent.
 Record the mass of the test specimen and the total
volume of the test specimen and solvent.
 Sample is placed boat for measurements of
chemiluminescence response. Combustion of sample is
taking place in tube for conversion of N to NO and NO2.
 Check the complete combustion of sample and if some
coke or soot present allow some residence time and
decrease the boat introduction rate.
Measure each test sample three times and calculate
the average chemiluminescence response.
The concentration of nitrogen in the
crude oil is a measure of the
presence of nitrogen containing
compounds