Beruflich Dokumente
Kultur Dokumente
161171
Abstract
A modified spectrophotometric method has been developed for the determination of phenol in water. The method
is based on the reaction between phenol, sodium nitroprusside and hydroxylamine hydrochloride in a buffer medium
of pH 10.611.8. The linear dynamic range is 0.055.0 mg ly1. The optimum determination wavelength is at 700 nm.
The molar absorptivity is 1.23= 10 4 mol ly1 cmy1. The relative standard deviation of the standard solution of phenol
is 1.3% n s 10, C s 0.5 mg ly1 .. The average recovery of water samples spiked with phenol of 2.0 mg ly1 is 98.8%
n s 10.. The relative error of standard sample C s 0.394" 0.003 mg ly1 . is 2.0%. F values of the statistical analysis
show that there is no significant difference between the proposed method and the 4-aminoantipyrine method. The
crystal of the product of the colored reaction was synthesized. According to its IR spectrum, Raman spectrum,
Mossbauer
spectrum and elemental analysis, the composition and structure of the product have been deduced and
the mechanism of the colored reaction has also been investigated. 2000 Elsevier Science B.V. All rights reserved.
Keywords: Phenol; Spectrophotometry; Water
1. Introduction
Phenolic compounds have been extensively used
as pesticides, herbicides and fungicides and are
present in the wastewater from the production of
Corresponding author.
E-mail address: duyg@mail.jli.edu.cn C. Kang.
0026-265Xr00r$ - see front matter 2000 Elsevier Science B.V. All rights reserved.
PII: S 0 0 2 6 - 2 6 5 X 9 9 . 0 0 0 2 2 - 3
162
2. Experimental
2.1. Instrumentation
The following equipment was used: a Model
721 spectrophotometer with 2-cm glass cells
163
164
Fig. 2. Effects of the amounts of the reagents: B. hydroxylamine hydrochloride; . sodium nitroprusside; and '. buffer.
Fig. 3. Effect of the reaction time. The concentrations of phenol are: 3.00 mg ly1 '.; 1.50 mg ly1 B.; and 0.50 mg ly1 .,
respectively.
165
Table 1
The reaction features of various phenolic compounds
Compounds
Color
ma x nm.
Phenol
o-Cresol
m-Cresol
p-Cresol
2,4-Dimethylphenol
1-Naphthol
4-Chlorophenol
4-Chloro-3-methyl phenol
2,4-Dichlorophenol
4-Aminophenol
Greenblue
Greenblue
Greenblue
Greenyellow
Light-green
Greenblue
Greenyellow
Greenblue
Greenblue
Greenblue
700
700
700
700
700
680
700
720
700
700
1.23= 104
1.62= 104
1.35= 104
41.9
1.67= 102
5.46= 103
93.1
2.93= 102
1.01= 102
1.38= 103
Under the above optimum conditions, the linear regression equation is A s 0.2669C y 0.01516
n s 7, r s 0.9996, C s 0.055.0 mg ly1 ..
For a 0.5-mg ly1 standard solution of phenol,
R.S.D.%s 1.3, which was obtained by the parallel
determinations of two samples each day within 5
consecutive days.
4-AAP method
mg ly1 .
Relative error
%.
1
2
3
4
5
0.240
0.201
0.282
0.320
0.242
0.244
0.208
0.275
0.323
0.245
1.7
3.5
y2.5
0.94
1.2
166
Fig. 4. Absorption spectra of the solid product in water: . blue solid product; and B. green solid product.
dried in a desiccator.
167
168
Fig. 6. The Raman spectrum of the solid product power 500 mW, scanning 100 times..
169
Its molecular formula should be Na 10 wFe 2CN.10 x. Compared with Na 2 wFeCN.5 NOx 2H 2 O,
the ferro valence degraded to 0 and the absorption frequency of the cyano group CN. in the IR
spectrum also shifted significantly, from 2150 to
2057 cmy1 .
The results of elemental analysis also indicate
that the solid product contains some crystallization water, which can also be proved by the IR
spectrum 1628 cmy1 ..
In the color reaction process in aqueous solu-
170
171