Characterization of Spent Wash

CHARACTERIZATION OF SPENT WASH
A. Ph Determination of pH was done by using the pH meter after all necessary

calibrations all the samples were taken in 3 different clean glass bottles and named
all of them and the pH was analyzed for all the samples.
B. Electrical Conductivity Determination of electrical conductivity was done using an

instrument called a conductivity meter after all necessary calibrations. The clean
glass bottles were used for the purpose of analysis. Thus EC was determined.
C. Dissolved Oxygen The estimation of dissolved oxygen is done by Winkler’s Azide

titrimetric method. Take a clean 300ml BOD for which 300 ml of sample is added,
now add 2ml of manganese sulphate (MnSO4), add 2ml of alkali-azide iodide, and
stop carefully to remove air bubbles, and mix thoroughly by shaking. If there is the
presence of oxygen the brownish precipitation is formed. If the oxygen is absent
white precipitation is formed. To the brown ppt after it is allowed to settle for a few
mins add 2ml of concentrated sulfuric acid. By this, a clear yellow suspension is
formed. Add 203 ml of the sample to a conical flask with a few freshly made starch
solution droplets and the sample was titrated against 0.025N sodium thiosulphate
(Na2S2O3). Titration was done till the blue color disappeared. The Volume of
Na2S2O3 used was noted for the determination of DO.
D. Chlorides Estimation of chlorides is done by Mohr’s titrimetric method Spent wash

sample of 0.1ml was taken and was diluted with 1000ml of RO water and now take
50ml from the diluted sample. Aluminum hydroxide was added to the sample and
was mixed and the solution was allowed to settle. Now to the filtrate add 1ml
potassium chromate indicator and titrate it against silver nitrate solution. Titrate till
the endpoint is yellow in color. Repeat the procedure for the Blank sample. And do
the necessary calculations.
E. Biochemical Oxygen Demand (B.O.D) Biological Oxygen Demand estimation was

done using a BOD bottle and BOD was calculated for 3-Days. A spent wash sample
of 0.1ml was taken and diluted with 1000ml of RO water. The 300 ml of sample was
filled till the neck in an air-tight B.O.D bottle of 300 ml and incubated at 270 degree
Celsius for three days in a B.O.D incubator by adding nutrient solutions such as
magnesium sulphate solution(MgSo4), Calcium chloride solution (CaCl2), Ferric
Chloride solution (FeCl3), Phosphate buffer solution. Dissolved oxygen measure is
done initially. 3 days of analysis is done for both blank and sample. Later BOD
calculations are done with the standard formulas.
F. Chemical Oxygen Demand (C.O.D) Chemical oxygen demand estimation was done
by the “Open reflux method”. 0.1ml of sample is taken and 1000ml of RO water is
added. Take 10 ml of the sample in a cod bottle before adding sample water to wash
thoroughly using soap powder and make sure no soap residue is left now wash it
with distilled water and make sure it is clean and ready to add the sample. Now add
0.4mg of mercuric sulphate (HgSO4) and add 10 ml of potassium dichromate and
add 30ml concentrated sulfuric acid and add some glass beads so that it avoids
bumping.
Switch on the apparatus and make sure that the water is flowing continuously reflux
action should take for around 2 hours and after that, it should be allowed to cool for
one hour. After cooling add 80ml of distilled water and add a few drops of ferroin ion
indicator. It should be titrated with 0.1N ferrous ammonium sulphate (FAS) until the
color turns blue-green. Do the necessary calculations for blank and sample and get
the COD values.
G. Total Phosphorous For this firstly turn on the heating block, hot kit TNT 72 prepare
a series of vial blanks, standard, and others needed. Using a micro pipette add 5ml of
deionized water to the vial marked blank. Add 5 millimeters of standard solution to
the vial marked standard. Add 5 ml collected sample to vial marked sample, add 1ml
potassium persulfate to each vial cap invert the vial two to three times to mix and
insert all the into the block digest for 30 minutes at 150 degrees Celsius. When
finished remove all vials from a heating block using tongs to cool the vials to touch.
Take sodium hydroxide 2ml solution using a micropipette and add to each vial. Now
add 5ml of molybdenite invert two to three times to mix properly and wait for 7
minutes. Choose program on hoc spectrometer 3900 choose method 542 total
phosphorous HR tnt press start place vials one by one and press read. Record the
results.
H. Sodium Potassium & Calcium Are determined by using a Flame Photometer using
the analytical tool microprocessor flame photometer model LT671. LPG is connected
to the instrument. Then LPG is mixed with the aspirated solution and then the
aspirated solution liquid vaporizes and the metallic ion is converted to a gaseous
state, then a neutral state. Neutral ions will now dissociate and the presence of
thermal energy will excite them to a higher energy state after coming to the lower
energy state it will produce the photons and by using these photons it will give out
the concentration in ppm.
I. Total Solids Take the empty weight of the crucible (w1), add 25ml of sample to the
crucible keep the crucible on the hot plate until the moisture content in the crucible is
evaporated. Now weigh the crucible which contains residue (w2), the difference
between w1 and w2 gives us the weight of residue. The weight of the sample divided
by the volume of the sample gives the result of total solids in mg/L.
J. Total Suspended Solids Take the empty weight of the Wattman filter paper (w1),
fold the filter paper in a cone shape add 25ml of the sample to the filter paper by
holding it in a conical flask, and keep the filter paper in the hot air oven until the
moisture content in the filter paper is evaporated. Now weigh the filter paper which
contains residue (w2), the difference between w1 and w2 gives us the weight of
residue. The weight of the sample divided by the volume of the sample gives the
result of total solids in mg/L.
K. Total Dissolved Solids Are calculated as the difference between total solids and
total suspended solids.

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CHARACTERIZATION OF SPENT WASH

A. Ph Determination of pH was done by using the pH meter after all necessary

B. Electrical Conductivity Determination of electrical conductivity was done using an

C. Dissolved Oxygen The estimation of dissolved oxygen is done by Winkler’s Azide

D. Chlorides Estimation of chlorides is done by Mohr’s titrimetric method Spent wash

E. Biochemical Oxygen Demand (B.O.D) Biological Oxygen Demand estimation was

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