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3) Department of Soil Sciences, Faculty of Agriculture, Brawijaya University, Malang, East Java 65145 Indonesia
Keywords : speciation,
added with 1 mL of distilled water. Each test Tabel 2. The solution added to mix of Cr(III)
tube was acidified by adding 0.15 mL of a and Cr(VI)
solution of H2SO4 (1:3). Each one is oxidized No. Addition of Oxidation Cr
with KMnO4 solution drop wise in a test tube Fe(III) and with measured
that is inserted in the beaker glass containing NaF solution KMnO4 as
1. 0 mL Fe(III) Without Cr(VI) only
water that is heated on a hot plate, as Figure 1. and 0 mL NaF oxidation
The addition of KMnO4 solution is stopped 2. 3 mL Fe(III) Without Cr(VI) only
when there is little excess KMnO4 solution and 0 mL NaF oxidation
which marked the formation of a permanent 3. 3 mL Fe(III) Without Cr(VI) only
pink color. and 6 mL NaF oxidation
When it is cold, each plussolution was 4. 0 mL Fe(III) Oxidation Cr(VI) and
added with 3 mL of 1 M H3PO4 and 3.0 mL of and 0 mL NaF by KMnO4 Cr(III)
0.05% DPC. 5. 3 mL Fe(III) Oxidation Cr(VI) and
Each solution was diluted with distilled and 0 mL NaF by KMnO4 Cr(III)
water to 100 mL. Shaken and left for 5 6. 3 mL Fe(III) Oxidation Cr(VI) and
minutes. Absorbance was measured at the and 6 mL NaF by KMnO4 Cr(III)
maximum λ of 540 nm with a UV-vis
spectrophotometer. The absorbance of each No. 1, 2, 3 : each in a 100 mL volumetric flask,
solution were extrapolated to the standard added 3 mL of 1 M H3PO4 and 3.0 mL of
curve of Cr(VI) and concentration can be 0.05% DPC.
known. No. 4, 5, 6: oxidation carried out in a test
tube and added with 1 mL of distilled water.
2) Determination of Cr(VI) to Cr(III) in an Each test tube was acidified by adding 0.15
artificial of water sample. mL of a solution of H2SO4 (1:3). Each one is
By using the optimum conditions (from oxidized with KMnO4 solution drop wise in a
the experiment c.2. and c.3.), concentration of test tube that is inserted in the glass beaker
Cr(VI) to Cr(III) in artificial samples were containing water that is heated in a hot plate, as
determined. Figure 1. The addition of KMnO4 solution is
stopped when there is little excess KMnO4
A) Standard curve Cr (VI) solution which marked the formation of a
Prepared a series of solution of Cr(VI) permanent pink color.
100 ppm in a 100 mL volumetric flask, When it is cold, a solution of each test
namely: 0.0; 0.1; 0.2; 0.3; 0.4; 0.5 mL of tube transferred to a different flask, added with
Cr(VI) of 100 ppm. Each plus 3 mL of 1 M 3 mL of 1 M H3PO4 and 3.0 mL of 0.05%
H3PO4 and 3.0 mL of 0.05% solution DPC. DPC.
Each solution was diluted with distilled Each solution was diluted with distilled
water to 100 mL. Shaken and left for 5 water to 100 mL. Shaken and left for 5
minutes. Absorbance was measured at the minutes. Absorbance was measured at the
maximum λ of 540 nm with a UV-vis maximum λ is 540 nm with a UV-vis spectro-
spectrophotometer. photometer.
The absorbance of each solution were
B) Mixing Cr(VI) and Cr(III) in a sample of extrapolated to the standard curve of Cr(VI)
artificial water. and concentration can be known.
Prepared a series of artificial sample
solution, a mixture of 0.2 ppm Cr(III) and 0.2 3. RESULT AND DISCUSION
ppm Cr(VI), then treated as table 2 : 3.1. Diphenylcarbazide(DPC) optimum
concentration.
Absorbance was measured at the
maximum λ of 540 nm with a UV-vis
spectrophotometer. From Figure 2 taken
0.0015% DFC as the optimum concentration.
Figure 3. The effect of H3PO4 concentration to the Figure 5. The effect of Fe(III) concentration to the
absorbance. absorbance.
3.3. The influence of the absorbance 3.5. Overcome Fe(III) interference using NaF
measurement time after preparation. solution
Absorbance was measured at the From this experiment as presented in
maximum λ of 540 nm with a UV-vis Figure 6, NaF optimum concentration is 0.3%.
spektrofotometr with variation of time: 5, 15,
45, 75, 105, 135 minutes after preparation.
From the Figure 4, the optimum time is 5
minutes after preparation.
Y = 0.632381 X + 0.006429
Equation for calculate limit of detection:
2. Measuring Cr(VI) in the artificial sampel 2. Selection of H2SO4 solution as acid media
0.5 ppm Cr(VI). for the oxidation of Cr(III) to Cr(VI).
The absorbance of each solution From the experimental results as
(column 3, Table 3) were extrapolated to the presented in Figure 12, have been known that
standard curve of Cr(VI), Figure 10 and volume of solution of H2SO4 (1: 3) optimum is
concentration Cr(VI) can be known (column 4, 0.15 mL.
table 3).
Table 3. Measuring the artificial 0.50 ppm Cr(VI)
with Fe(III) interference and adding NaF solution.
Solution Repli Abs. Cr6+ Mean of SD
added to -cates measured Cr6+ (%)
Cr(VI) (ppm) measured
± SD
6 mL NaF
3 mL Fe3+ 1 0.279 0.4964 0.4988
3 mL 2 0.280 0.4982 ± 0.54
H3PO4 0.0027
3 mL DFC 3 0.282 0,5018
4 mL NaF
3 mL Fe3+ 1 0.258 0.4591 0.4549
3 mL 2 0.255 0.4537 ± 0.81 Figure 12. The effect of H2SO4 solution as acid
H3PO4 0.0037
0.254 0. 519
media to the oxidation of Cr(III) to
3 mL DFC 3
Cr(VI)
3. Measurement of the sample (artificial) Table 5. Measuring the artificial mixing solution of
Cr(III) which was oxidized to Cr(VI) by 0.20 ppm Cr(III) and 0.20 ppm Cr(VI) with Fe(III)
KMnO4 in H2SO4 as acid media. interference and adding NaF solution
No. Solution Cr6+ Mean of SD
The absorbance of each solution (column Added to Repli- Abs. measured Cr6+ (%)
3, Table 4) were extrapolated to the standard Cr cates (ppm) measured
solution + SD
curve of Cr(VI), Figure 11 and concentration
1. None 1 0.146 0.1997 0.2020
Cr(III), as Cr(VI), can be known (column 4, 2 0.149 0.2038 ± 0.59
table 4). 3 0.148 0.2025 0.0012
2. 3 mL 1 0.117 0.1601 0.1596
Table 4. Measuring Cr(III) in the artificial solution Fe(III) 2 0.115 0.1573 ± 1.31
3 0.118 0.1614 0.0021
of Cr(III) with Fe(III) interference and adding NaF
3. 3 mL 1 0.143 0.1956 0.1965
solution. ±
Fe(III) + 2 0.146 0.1997 1.45
6 mL 3 0.142 0.1943 0.0028
Mean of
ppm Repli
Cr3+
Cr3+ SD
NaF
Abs. measured 4. KMnO4 1 0.294 0.4022 0.4004
Cr3+ -cates measured (%)
(ppm)
± SD 2 0.289 0.3953 ± 0.63
0.20 1 0.156 0.2069 0.2034 3 0.295 0.4036 0.0025
2 0.154 0.2042 ± 1.99 5. 3 mL 1 0.233 0.3187 0.3128
3 0,150 0.1989 0.0041 Fe(III) + 2 0.229 0.3119 ± 1.02
0.30 1 0.258 0.3024 0.3059 1.09 0.3078 0.0032
KMnO4 3 0.225
2 0.255 0.3064 ±
3 0.254 0.3090 0.0033 6. 3 mL 1 0.291 0.3981 0.3949
0.40 1 0.174 0.4005 0.4036 0.68 Fe(III) + 2 0.288 0.3940 ± 0.72
2 0.172 0.4058 ± KMnO4 3 0.287 0.3926 0.0028
3 0.168 0.4045 0.0028 + 6 mL
NaF
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