Professional Documents
Culture Documents
ANNEX 5
Pipette 5 Ml 3
Funnel glass 2
Disposable gloves 24
Permanent markers 2
Precautions
1) SAFETY CONSIDERATIONS
Eye protection is required when collecting the samples to prevent the inadvertent contact of methanol
with eyes during sample collection. Gloves should be worn to prevent the absorption of methanol
through skin. Disposable plastic gloves are worn to prevent contamination of sample during collection
process (Sufficient amount of chlorides can be absorbed from the skin to cause the sample to fail the
chloride analysis). Also all sampling equipment including bottles, funnels and other apparatus must
be thoroughly rinsed with methanol prior use as chlorides are abundant in environment. Personal
collecting the samples must be aware samples or sampling equipment must not in any way contact
bare skin or perspiration.
2) TEST SITES
A minimum of four (4) sites, approximately 1 square metre each, must be chosen in each tank, any
area that appears to have crystalline deposits must definitely be tested.
3) COLLECTION PROCEDURE
Dispense methanol on the test sections at the highest practical point (about 1.5 to 2 metres) above
the tank bottom in a stream of about 10 cms wide. Allow the methanol to run down the wall
approximately 15 cms and begin collecting it with a half cut funnel pressed against the bulkhead.
Collect about 200 ml of sample of wall wash methanol in the sample bottle from four sites. This
methanol sample collected is to be used for analysis.
COLOUR TEST
Certain impurities result in discoloration of the wall wash sample. The colour of the wall wash liquid is
compared standard solution. Mostly APHA colour is measured.
CHLORIDE TEST
The principal of the test is that chloride together with silver nitrate solution forms silver chloride (AgCl)
which makes the solution turbid. This solution is compared with various standard solutions to
establish the ppm chlorides in the sample.
Prepare the Nessler tubes as indicated in the below diagrams. Insert the stopper and invert the
tubes. Compare the turbidity of the sample solution with standard .25-PPM, .5-PPM and 2PPM
solutions by looking through the liquid against a black background. Comparison should be done in a
dark room by looking through the tube using a beam flashlight.
If the turbidity of the sample is more than .25-PPM solution, the sample should be compared with .5-
PPM standard solution and so on until the turbidity of the sample matches the higher standard
solution.
46 ml of 45 ml of 44 ml of 38 ml of
DI Water DI Water DI Water DI Water
1 ml of 10 2 ml of 10 8 ml of 10
PPM stand PPM stand PPM stand
Chloride Chloride Chloride
2 ml of 2 ml of 2 ml of 2 ml of
20% HNO3 20% HNO3 20% HNO3 20% HNO3
2 ml of 2% 2 ml of 2% 2 ml of 2% 2 ml of 2%
AgNO3 AgNO3
AgNO3 AgNO3
50 ml of 50 ml of 50 ml of 50 ml of
Wall Pure Pure Pure
wash methanol methanol methanol
sample
HYDROCARBON TEST
The purpose of this test is the qualitative detection of non-water soluble contaminants. It works on the
basis that many impurities are soluble in the wall wash liquid but not in water. Therefore this test is
also called Water Miscibility test. The wall wash sample is poured into clear DI water. The Wall wash
sample is soluble in water but not the impurities. This leads to cloudiness or turbidity of water. The
water with wall wash liquid is compared with a standard solution of pure methanol and DI water.
Prepare the Nessler tubes as indicated in the below diagrams. Insert the stopper and invert the tubes
to mix the contents. Allow it to stand for 5 minutes. Compare the cloudiness / turbidity of the sample
solution with standard solution of pure methanol / DI water by looking through the liquid against a
black background. Comparison should be done in a dark room by looking through the tube using a
beam flashlight. If the sample solution is same in transparency as the standard than wall wash
hydrocarbon content is zero. Similarly if the sample solution is milkier than standard than there is a
presence of hydrocarbon in the wall wash test. If a bluish tint is present, there are moderate to heavy
hydrocarbons.
50 ml of
50 ml of
DI Water
DI Water
50 ml of 50 ml of
Wall Pure
wash methanol
sample
Sample standard
2 ml of 2 ml of
KMnO4 KMnO4
sol sol
50 ml of 50 ml of
Wall Pure
wash Methanol
sample
Sample standard