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LAB NO
: 2
TITLE
GROUP
: AS2294A
GRADER
DATE OF
EXPERIMENT
: 17 MARCH 2016
NAME / STUDENT ID :
INTRODUCTION
10.
The flasks was placed on a magnetic stirrer and was rapidly
titrated with 0.1 N ferrous ammonium sulphate to the first red-brown
endpoint.
2) REACTOR DIGESTION (CLOSE REFLUX)
1. The COD reactor was turned on and was preheat to 150 . The
safety shield was placed in front of the reactor.
2. The caps of a COD digestion reagent vials was removed for the
appropriate range.
3. The vials was hold at a 45 angle. 2.0 ml of the sample was
pipetted into the vial.
4. The vials was capped tightly. The outside of the COD vial was rinsed
with deionised water and the vial was wipe cleaned with paper
towel.
5. The vial cap was hold and over a sink. It was gently inverted several
times to mix the contents. The vial was placed in the preheat COD
reactor.
6. A blank was prepared by repeating steps 2 to 5, substituting 2.0 ml
deionised water for the sample.
7. The vials was heated for 2 hours.
8. The reactor was turned off and waited about 20 minutes for the vials
to cool to 120 or less.
9. Each vial was inverted several times while still warm. The vials was
placed into a rack and cooled to room temperature.
10.
The was proceed to the colorimetric determination to measure
the COD.
( mL K 2 Cr 2 O7 ) (0.25)
mL FAS requir ed
=
10 (0.25)
47.8
= 0.052 mL
BLANK A =
BLANK B =
= 81.54 mg/L
DISCUSSIONS
From the experiment of open reflux, most types of organic matter
are oxidized by a boiling mixture of chromic and sulfuric acids. A sample is
refluxed in strongly acid solution with a known excess of potassium
dichromate (K2Cr2O7). After digestion, the remaining unreduced K2Cr2O7 is
titrated with ferrous ammonium sulfate to determine the amount of
K2Cr2O7 consumed and the oxidizable matter is calculated in terms of
oxygen equivalent. Keep ratios of reagent weights, volumes, and strengths
constant when sample volumes other than 50 mL are used. The standard
2-h reflux time may be reduced if it has been shown that a shorter period
yields the same results. Some samples with very low COD or with highly
heterogeneous solids content may need to be analyzed in replicate to
yield the most reliable data. Results are further enhanced by reacting a
maximum quantity of dichromate, provided that some residual dichromate
remains.
In the reactor digestion method test, the COD procedure is greatly
simplified over the Dichromate Reflux Method. Small volume of the water
sample is pipette into vials containing the pre-measured reagents,
including catalysts and chloride compensator. The vials are incubated until
digestion is complete and then cooled. The COD determination is made
with the spectrophotometer.
CONCLUSIONS
The Chemical Oxygen Demand (COD) has been determined. The
normality of FAS have obtained to be 0.052 and from FAS, the calculation
of COD can make to get the result for the sample. From the calculation of
open reflux method, were obtain 104.83 mg/L for blank A while 81.54 mg/L
for blank B of COD value. The sample was use the amount of oxygen
(COD) consumed to completely chemically oxidize the organic water
constituents to inorganic end products. For the reactor digestion method,
the COD result for blank, standard and sample has to be 0, 97, and 193
mg/L.
REFERENCES
1. www.pavloschemicals.com/lab
2. https://www.norweco.com/html/lab/test_methods/5220bfp.htm
3. www.labseeker.com/labsupplies/lablist
QUESTIONS
1.
2.
The main reason for using the blank sample is to control the
volume of organic material in the sample. COD was carried
out to measure the oxygen demand of organic compounds in a
sample of water, and we have to ensure there were no
accidentally outside organic materials added to the sample to
be measured. A blank sample is created by adding the
reagents to a volume of distilled water. Both water and blank
sample will be compared. The oxygen demand for the blank
sample is subtracted from the COD for the original sample to
ensure the true measurement of organic matter.
3.