UV VIS Analysis

VISIBLE AND
ULTRAVIOLET
SPECTROPHOTOMETRY
11/22/2012
dcapodaca_CHM115_MAPUA
SPECTROPHOTOMETER
Instrumental measurement of the absorption of

radiant energy by a solution at a given
wavelength
extremely valuable instrument for colorimetric
analyses.
has a wide range of adaptability.
recommended where a wide variety of
determination is made.
its versatility allows the best wavelength of
light
to be used at
all time.
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PRINCIPLES OF UV
SPECTROPHOTOMETER
Light source usually a

hydrogen or deuterium lamp
Monochromatic
light
is
obtained by allowing a beam
of light to pass through a
color filter
Photoelectric cell is translated
into % transmission or
absorbance
Instrument is adjusted to
yield a light transmission
corresponding to 100% with
the cell containing blank
sample
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CALIBRATION
Prepare a series of standards

Prepare sample solutions
Set the instrument
Adjust the specified wavelength
Start measurement
Data are plotted
Evaluate the samples from the calibration graph.
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POINTS TO REMEMBER
Instrument should be in good working

condition
Cells are always kept clean
Turbidity of samples is eliminated
Analyst must make sure that unknown
errors in reagents and the like do not lead
to faulty results.
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CALIBRATION GRAPH
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COLORIMETRIC
DETERMINATION OF
PHOSPHATES IN WATER
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OCCURRENCE
natural water and wastewater

minor element in natural water
low solubility
dissolved concentration
0.01-0.1 mg/L and seldom exceed 0.2 mg/L
essential to metabolism
occurs as orthophosphates (H3PO4,H2PO4-HPO4-2,PO4-3)

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USES
Corrosion control in water supply and

industrial cooling water system
Insecticides
Fertilizers
Production of synthetic detergents
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10
PRINCIPLE
Orthophosphoric acid reacts with molybdate forming

a yellow coloured phosphomolybdic acid which by
reduction with tin gives a blue complex. Tungsten
anion which reacts in the same way is added to
improve coloration at concentration below 1 mg PO43per L.
CHEMICAL REACTIONS:
PO43- + 12 (NH4)2MoO4 + 24 H + (NH4)3PO4 .12 MoO3 +
21 NH4+ + 12
H2O
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RANGE OF APPLICATION
negligible As+5 and Cr+6 content
less than50 mg/L silicic acid
1 mg/L Fe+3
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12
APPLICATIONS
natural
industrial
sewage-type
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13
EQUIPMENT/APPARATUS
Spectrophotometer
Magnetic stirrer
timer
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14
REAGENTS
Standard solution containing (0.1 mg

HPO4-2/ml)
Molybdate reagent
Metallic tin
Sulphuric acid (1+4)
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15
PROCEDURE
Sample
50 ml aliq.
in 150 ml beaker
Measure
at 700 nm
Add 1 ml
Molybdate
reagent
20 min. after
ending
reduction
Add few tin

beads reduce
5 min. while
mixing
Separate sample
from tin leave
standing
Evaluate from
calibration graph
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PREPARATION OF STANDARDS
mg HPO4-2
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0.01
Vol. of Std.
(ml)
0.1
0.02
0.2
0.04
0.4
0.06
0.6
0.08
0.8
0.10
1.0
0.20
2.0
17
COMPUTATION
Conc. of HPO4-2 = amount of HPO4-2 (mg)

vol. of sample (L)
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INTERFERENCES
Silicic acid
Arsenic
Iron
Chromate or dichromate
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SPECTROPHOTOMETRIC
DETERMINATION
OF NITRATES IN WATER WITH
SODIUM SALICYLATE
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OCCURRENCE
Most prevalent form of nitrogen in water

End product of the aerobic decomposition of
organic nitrogen
Unpolluted water seldom exceed 10 mg/L
Major components of human and animal waste
Cyanosis due to methemoglobinemia occurs in
infants.
More than 10-20 mg/L of nitrate nitrogen cannot
be used in infant feeding
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PRINCIPLE
In concentrated sulphuric acid medium
nitrates react with salicylic.Making the
solution alkaline the yellow anion of
nitrosalicylic acid is formed and measured
by spectrophotometry.
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COOH
COOH
OH
OH
+ 2HNO3
2-hydroxybenzoic acid
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H2SO4
+ 2H2O + Na2SO4
O2N
2-hydroxy-5-nitrobenzoic acid
23
APPLICATION
Surface and ground water

0-20 mg NO3-/ L
Cl- over 200 mg/L
Fe+2 over 5 mg/L
nitrates over 1 mg/L
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EQUIPMENT AND APPARATUS
Spectrophotometer
water bath
evaporating dish
volumetric flask
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REAGENTS
Standard solution (0.1 mg NO3- )
0.5% m/v sodium salicylate
10M NaOH
sulphuric acid
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PROCEDURE
Measure 10 ml
sample in
evaporating dish
Transfer to
50 ml vol. flask
Add 7 ml
NaOH, mix
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Evaporate
To
dryness
Add 1 ml
Sodium salicylate
Leave standing
For 10 min
Fill up to the
mark with
dist.water
Add 1 ml
Conc.H2SO4
Measurement
Cool
Evaluate
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PREPARATION OF STANDARDS
NO3mg/L
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Vol. Of std
(ml).
0.05
0.5
0.10
1.0
0.20
2.0
0.50
5.0
1.00
10.0
2.00
20.0
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MEASUREMENT
Evaluate the sample from the calibration

graph
INTERFERENCES
Chloride ions
Organic colloids
Nitrates
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Table IX: Result of Analysis for NO3- and HPO42Starting with different sample aliquots
(San Roque Dam Project)
Samples
2 ml aliquot
5 ml
aliquot
10 ml
aliquot
SW-1
0.40
0.38
0.39 mg/L
NO3-_
SW-2
0.41
0.39
0.43 mg/L
NO3-
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Samples
25 ml
aliquot
50 ml
aliquot
75 ml
aliquot
SW-3
1.42
1.41
____
SW-7
SW-10
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0.70
___
0.68
0.04
100 ml
Aliquot
__
mg/L
HPO42-
0.64
____
mg/L
HPO42-
___
0.04
mg/L
HPO42-
31
CONCLUSION:
For sample with low and medium

mineralization,the procedure provide
correct data
For samples with high and medium high
mineralization,the procedure should be
checked if such samples come for analysis
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32

UV VIS Analysis

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UV VIS Analysis

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VISIBLE AND

Instrumental measurement of the absorption of

Light source usually a

Prepare a series of standards

Instrument should be in good working

natural water and wastewater

occurs as orthophosphates (H3PO4,H2PO4-HPO4-2,PO4-3)

Corrosion control in water supply and

Orthophosphoric acid reacts with molybdate forming

negligible As+5 and Cr+6 content

less than50 mg/L silicic acid

Standard solution containing (0.1 mg

Add few tin

Conc. of HPO4-2 = amount of HPO4-2 (mg)

Most prevalent form of nitrogen in water

Surface and ground water

EQUIPMENT AND APPARATUS

Standard solution (0.1 mg NO3- )

0.5% m/v sodium salicylate

Evaluate the sample from the calibration

For sample with low and medium

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