Analysis Schedule,
Procedure for Sampling,
Field test
Rupesh Chandarana
SAMPLING ????
Any Product to compete in the market has
to be economical and should primarily
satisfy the customer qualitatively.
Therefore testing representative samples
is essential for a product to qualify
The Small part tested must be, identical to
the Stream that it represents. Samples,
which are not truly representative, can
mislead operation to serious
consequences
TYPES OF SAMPLES
Two types of samples are used
in controlling the operation
Grab or Spot Samples
Composite Samples
Grab or Spot Samples
In taking a Spot Sample,
Entire Sample is obtained at one
time.
The Sample represents the composition
of the total stream at that time.
The operator uses the results of
Sample tests to make routine
adjustments in operating
conditions, To follow the continuous
operation of the unit, spot samples
are sent to lab at specified intervals
Composite Samples
In the case of Composite Sample,
Equal portions of the stream are put
in a large sample container at regular
intervals over a period of time.
This type of Sample is used by
Technical staff to determine the loss of
valuable products into a less valuable
stream, to evaluate the effects of
changes in operating condition and to
make weight balances around the
unit.
Sampling Methods
It can be varied as determined by the
nature, temp, and pressure of the
sample as well as the type of process
container and sample connection.
General technique for procuring
representative sample safely are as
given below:
Open Container
Sample Bombs
Blader
SAMPLE COLLECTOR
SAMPLE
BOMB
SAMPLE
BOTTLE
SAMPLE
BLADDER
Open Container
Open container sampling is the most
common type of sample taken. It is used
for low vapour pressure samples like
heavy oils, and cooling water The sample
is drawn into an empty bottle A stopper is
placed in the bottle, t and sent to the lab.
The sample point is sometime equipped
with a flexible tubing extension so that the
liquid sample enters the bottle under the
liquid level in order to avoid saturating the
sample with air and to decrease loss of
volatile vapour
Sample Bombs
They are used for taking samples of
gaseous hydrocarbons and certain
hydrocarbon liquids with vapour
pressure above 15 PSI, like fuel gas
and LPG the valves on sample bombs
should only be more than hand tight.
Otherwise valve seats will be
seriously damaged and the valve will
leak.
Sampling Procedure
The procedure for sampling high
pressure sample with this bomb is
as follows.
Open valve, flush the line and close.
Connect valve to the sample line.
Open valve on the sample line.
Open the valve u/s of the sample
line and purge the sample bomb
well with the sample. Be sure to
direct the flow towards the flare.
CLOSED SAMPLE POINT
SAMPLE POINT
Close valve towards the flare and let the
bomb fill with the sample. Open the d/s
valve of the bomb and establish the
circulation through d/s process line.
Close the valve d/s of the bomb and
close u/s valve after filling the bomb with
the sample. Then unscrew the bomb
from sample valve.
Incase of a liquid sample, hold the bomb
in an upright position and then open the
bottom valve and close it quickly so that
a portion of a liquid phase escapes. This
is to provide a vapour space in the
sample bomb. Proper vapour space is
between 5 and 10 percent.
Check the inlet and outlet valves on
sample bomb for leaks and tags the
sample for identification.
Safety precautions to be
followed while taking samples:
Use safety equipment as prescribed in the
specific instructions. This includes gloves, face
shields, goggles, oxygen masks etc.
Check surrounding area for a source of ignition.
Allow a vapour space in the container for
expansion in the case of both bottles and
bombs.
Keep control flow of sample.
Be careful and complete in tagging sample
containers. Wrong labels can cause accidents in
the lab.
Safety Precautions to be
followed while taking samples:
Check the sample container for
cleanliness or foreign material. Water in
the bottle or on the walls of a container
receiving hot oil can flash to steam.
Check sample coolers for water flow.
If necessary to climb ladders or mount
platforms for samples use both hands.
Special sampling equipment should be
provided to allow both hands for
climbing.
Attach grounding devices for static
electricity dissipation where provided.
SAMPLING SCHEDULE & USING
SAMPLE RESULTS
If the sample results indicate that
corrective action to be taken, it is the
duty of the operator to do so. After
corrective action has been taken ,
and unit has lined out , it is equally
important to resample and test the
streams in question to see that the
change in operation was proper and
effective.
FIELD TEST
&
FIELD ACTIVITIES
:: Hydrogen ::
Reformer Visual
Checking
Dragger Analysis
Chlorine Analysis
Visual Inspection
Hot Bands
• Reduction in activity
• Due to Poisoning
• Coating by small ‘C’
layer
• Hot brands may often
be removed by
steaming
• Otherwise catalyst to
be replaced
Visual Inspection
Tiger tailing
• Alternate hot & cold rings
developed at random on
individual tubes
• Indicate voids in the
catalyst packing, as a
result of improper
charging.
• If vibration or careful
hammering does not
remove the voids, the
tube should be
discharged and refilled at
the earliest opportunity.
Visual Inspection
Giraffe necking
• Extensive deactivation
from catalyst poisoning
or a surface deposit.
• Channeling through the
catalyst. This cools the
tube where the gas is still
reacting and overheats
the tube where the flow
of gas is impeded.
• Channeling can be
caused by pockets of
broken catalyst and dust,
or by accumulation of
carbon.
Visual Inspection
Hot tubes
• Where extensive carbon
deposition or catalyst
breakdown restricts the
flow of gas a whole tube
can become overheated.
• It may be possible to
remove carbon in such
tubes by steaming but
this is usually ineffective
because of preferential
flow through the
unaffected tubes.
DRAGER ANALYSIS
For H2S Measurement
Break both ends of the tube and
insert one end of the tube as per
given direction in to the Drager Tube
Pull out the handle of the pump and
give the no. of stroke as per define
Range ::
5 to 100 ppm -- V06 + R01O/L-1stk
0.5 to 10 ppm -- R02A/B – 5 strk
Colour Change ::
White to Brownish
DRAGER TUBE
DRAGER PUMP
MEASUREMENT OF ORGANIC
CHLORIDE
To measure Organic chloride content
using TCE (Tri chloro Ethylene)
Detector Tubes.
To measure inorganic chloride HCL
Detector Tubes.
Color Change :::
Orange to Blue (TCE)
Green to Pink (HCL)
CHLORINE TUBE
For streams containing higher
concentrations of Chloride one stroke
would be enough, for lower concentrations
more strokes can be taken.
Range :
1 to 16 ppm – TCL – 10 strk
2 to 20 ppm – HCL – 10 strk
Divide the reading obtained on the tube
with the number of strokes to get the
correct value of TCE.
Divide the reading obtained on the
tube with the number of strokes to
get the correct value of TCE.
Multiply the TCE value obtained with
3 to get the value of total organic
chloride.
Example ::
Reading on TCE tube: 5ppmv
No. of strokes: 2
Correct TCE value: 5/2 = 2.5 ppmv
Correct Total Chloride reading: 2.5 *
3 = 7.5 ppmv
For Organic Chloride:
Difference between the readings of
Total Chloride and HCL gives the
value of Organic Chloride
Example:
Correct reading of HCL :
1.5ppmv
Correct total chloride reading:
7.5 ppmv
Correct organic chloride reading:
7.5 - 1.5 = 6ppmv
:: Merox ::
SHAKE TEST
WEATHERING &
% OXYGEN
LEAD ACETATE
DOCTOR TEST
SHAKE TEST
It is a simple test which can be
performed in the unit by the
operators to estimate the
effectiveness of Merox caustic
regeneration.
Half fill a small, clear glass bottle
with regenerated Merox caustic
solution taken from the suction of
the Merox Caustic circulation pump .
The color of the solution should change green to
deep blue after one or two minutes of shaking.
If more than two minutes of shaking are required
to make the color change due to any one of the
following may be the reason
a. Insufficient air to Oxidiser,
b. Oxidiser temperature is too low .
c. Insufficient catalyst in caustic.
If less than 30 sec’s of shaking are required to
make the color change any one of the following
may be the reasons;
Excessive air
Oxidiser temperature is too high
[Link] catalyst in the caustic
WEATHERING
This test is Performed to check the
components of the LPG. It is the Only
Approximate Test Developed Based
on the Lab results
The temperature at which 95% of the
liquid LPG evaporate is Known as
WEATHRING TEST .
Weathering Test is a Qualitative Field
Test which indicates the presence of
either C2 or C5.
If Weathering less than -2 C means
C2 content are more that means
lighter components are more.
If Weathering is more than +2 C
means C5 contents are more that
means heavier components are more
Procedure for Weathring Test
Flush the Weathering tube with the
sample
Take 100ml of LPG sample in the
tube
Insert the thermometer in the tube
during test
Thermometer should not be touching
the tube wall
Put the LPG Weathering tube in the
water bath. Do not emerge tube more
than 0.5 ml mark of the tube in the
water bath
Allow the liquid LPG to vaporize
Thermometer Mercury bulb should be
fully emerged in the liquid under test
even when last 6 ml liquid is left over
Take the temperature reading when 6
ml liquid is left over in the tube .
This 6 ml is taken equivalent to 5 ml
as thermometer is dipped inside the
liquid
% OXYGEN
Checking % Oxygen for making Vent
gas as combustible gases for crude
heaters
Range 10 to 12%
% Oxygen to be checked with the
help of O2 meter or O2 Analyser
O2 METER
LEAD ACETATE
It is the simple test to check the
presence of H2S or RSH in LPG
Procedure :
Take a Filter paper & immersed it in
Lead acetate Solution. Then allow
that paper to come in contact with
LPG vapour & monitor the colour of
Lead acetate paper
Note down the colour change in each
vessel
If change of colour is YELLOW &
gradually turns to white, it indicates
the presence of RSH.
If change of colour is BROWN or
BLACK it indicates the presence of
H2S & if Paper remains WHITE it
indicates there is no H2S & RSH
DOCTOR TEST
H2S & RSH to be measured with the help
of this Test
10 ml of Gasoline to be taken in Sample
Measuring Flask.
5 ml Sodium Plumbite ( Doctor’s Solution )
to be added in Measuring Flask
If brown ring appears then RSH present in
Gasoline
Otherwise when it not appears then we
add Sulphur Powder for checking our H2S
presence as same as RSH
Thanks….
UNSAT LPG FEED AND PRODUCT
SPECIFICATION
FEED
(a) Normal condition :
Mercaptan sulfur : 827 [Link]
H2S content :10994 [Link]
(b)Maximum flow condition:
Mercaptan sulfur : 824 [Link]
H2S content : 9618 [Link]
PRODUCT
Total sulphur : 20 [Link]
(max.)
Sodium :1
[Link](max.)
SAT LPG FEED AND PRODUCT
SPECIFICATION
FEED
(a) Normal condition :
Mercaptan sulfur : [Link]
H2S content :1200 [Link]
(b)Maximum flow condition:
Mercaptan sulfur : 916 [Link]
H2S content : 43000 [Link]
PRODUCT
The product specifications are as following for both
the cases.
Total sulfur : 20 [Link] (max.)
Sodium : 1 [Link](max.)
Gasoline FEED SPECIFICATION
Mercaptan = 90 [Link](Max.)
H2S = 1wt ppm (Max.)
PRODUCT SPECIFICATION
Mercaptan = 5 wt. pp
H2S = Ni
Sodium (Na+) = 1wt .ppm
(Max)
Negative by UOP Doctor Test = yes