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ATIKAH
POSTGRADUATE CHEMISTRY PROGRAMME
MATHEMATICAL AND NATURAL SCIENCES FACULTY
BRAWIJAYA UNIVERSITY
2012
6-chemical parameter measurement-3
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Phenolic
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K3Fe(CN)6
+
pH 10
OH
Phenol
N
H3C-N
N
C=O
H3C - C
C- NH2
H3C-N
H3C - C
C=O
C- N=
4-Aminoantipyrin
Yellowis red
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1.
2.
3.
4.
5.
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Biological
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1.
2.
3.
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1.
2.
3.
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Prepare
Conc. F g/L
0.0
0.5
50.0
1.0
100.0
2.0
200.0
5.0
500.0
8.0
800.0
10.0
1000.0
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To
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Using
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mL of working solution B
Conc. F g/L
0.0
0.0
3.0
6.0
5.0
10.0
10.0
20.0
20.0
40.0
25.0
50.0
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10.1
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1.
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The
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In
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Scope
and Application
1.1 This method is applicable to the
measurement of total and dissolved sulfides
in drinking, surface and saline waters,
domestic and industrial wastes.
1.2 Acid insoluble sulfides are not measured by
this method. Copper sulfide is the only
common sulfide in this class.
1.3 The method is suitable for the
measurement of sulfide in concentrations up
to 20 mg/L.
6-chemical parameter measurement-3
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Color
development
Transfer 7.5 mL of sample to each of two
matched test tubes using a special wide
tipped pipet or filling to a mark on the test
tubes.
To tube A add 0.5 mL amine-sulfuric acid
reagent (5.2) and 0.15 mL (3 drops) FeCl
solution (5.3).
Mix immediately by inverting the tube only
once.
To tube B add 0.5 mL 1 + 1 H2SO4 (5.4) and
0.15 mL (3 drops) FeCl 2 solution (5.3) and
mix.
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Color
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Visual
Add methylene blue solution 1 (5.6) and/or II
(5.7) (depending on sulfide concentration
and accuracy desired) dropwise to tube B
(6.1.4) until the color matches that
developed in the first tube.
If the concentration exceeds 20 mg/L, repeat
6.2.1.1 using a portion of the sample diluted
to one tenth.
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1938
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Fluorides
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Summary of Method
Following distillation to remove
interferences, the sample is treated with the
SPADNS reagent.
The loss of color resulting from the reaction
of fluoride with the zirconyl- SPADNS dye is a
function of the fluoride concentration.
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This
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SPADNS
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The
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The
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Uses
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Interferences
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Alizarin
Formation
of pre-formed color:
Zr2+ + Alizarin
Zr- Alizarin complex
Yellow
reddish color
Zr- Alizarin complex + 6F
ZrF62- + Alizarin
reddish color
Yellow
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Monitoring
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1.
2.
A.
Volumetric
Argentiometric or Mohrs Method
Chloride (Titrimetric, Mercuric Nitrate)
Inorganic, Non-Metallics: Chlorine, Total
Residual, Titrimetric, Amperometric
Instrumental Methods
Spectrophotometric
Chloride (Colorimetric, Automated
Ferricyanide AAI)
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Chloride
(Colorimetric, Automated
Ferricyanide AAII)
Inorganic, Non-Metallics: Chloride,
Colorimetric, Automated Ferricyanide, AA I
: Inorganic, Non-Metallics: Chloride,
Colorimetric, Automated Ferricyanide, AA II
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Chlorine,
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Summary
of Method
Water adjusted to pH 8.3 is titrated with
silver nitrate solution in the presence of
potassium chromate indicator.
The end point is indicated by persistence of
the orange-silver chromate color.
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This
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Cl
+ AgNO3
0.0141N
2Ag+
+ CrO42-
Ag2CrO4
reddish-brown ppt
Calibration: use high purity NaCl
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use same quantity if indicator to avoid "toosoon" or "not-soon-enough" color changes leading
to inadequate blank correction;typical value =
0.2-0.4mL
Cl- (mg/L) = (mL AgNO3 - blank) x 0.5x1000
mL sample
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This
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Average value
(g/g)
Repeatability
(g/g)
Reproducibility
(g/g)
500
180
355
1,000
360
710
1,500
540
1,065
2,000
720
1,420
2,500
900
1,775
3,000
1,080
2,130
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Amount
Expected (g/g)
Amount
Found
(g/g)
Bias; (g/g)
Percent
bias
320
645
325
+102
480
665
185
+39
920
855
-65
-7
1,498
1,515
17
+1
1,527
1,369
-158
-10
3,029
2,570
-460
-15
3,045
2,683
-362
-12
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For
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THANK YOU
atikah_chem@ub.ac.id
atikadhikara@yahoo.com
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