3. Materials
The materials used silica gel as adsorbent obtained from Merck
(Darmstadt Company) with a size of 60 mesh and partical 0.063 to 0.200 nm. It
was treated with nitric acid (HNO3: H2O = 1: 1) at 100 ° C for 3 hours, 37%
hydrochloric acid at 100 ° C for 6 h to activate the particles of silica gel
[11.19]. The silica gel activation was washed with distilled water and
dried under vacuum for 24 hours [20]. Agents silylant 3 aminopropyltrimethoxy
silane (APTS) was used without further purification and
toluene is distilled under reduced pressure prior to use. 5
bromosalicylaldehyde and furfuraldehyde was purchased from Merck
and 3.4-dihydroxybenzaldehyde, copper acetate monohydrate
nickel acetate tetrahydrate was purchased from Fluka.
Use organic solvents include absolute ethanol (Riedel-de Haen) and diethyl ether
(Merck) for washing.
3.1. Silica gel Organofunctionalization actived
The phase silica gel bound amine derivative thereto have been prepared
from the reaction with (3-aminopropyl) trimethoxysilane as silylation
agents [21-23]. A 10.0 g sample of silica gel activated suspended in
50.0 cm3 of dry tolune reflux and stir for 72 h
at 110 ° C in dry nitrogen. The silica gel amendment was filtered out,
washed twice with toluene, and dried under vacuum at room
temperature for several hours. Functional surfaces was named
SiNH2 (Fig. 1).
3.2. Novel Surface preparation with other aldehydes
0.
69 g (5 mmol) of 3,4-toluene dihydroxybenzaldehyde in 50.0 cm3 reacted with a 5 g sample SiNH2, containing a few
drops of triethylamine to facilitate the equilibrium reaction.
Triethylamine was added as agents disprotonant to increase
the efficiency of the reaction. The mixture was reflux and machinery
stirred for 72 hours at 100 ° C. The final product, 3,4-dihydroxybenzaldehyde
be fixed on silica, filtered, washed with toluene,
ethanol and diethyl ether, and dried under vacuum at room temperature
for 24 hours [11]. It was named the I / SiNH2 (Fig. 2).
Other aldehydes, furfuraldehyde and 5-bromosalicylaldehyde,
silica gel was fixed up on modified according to
the respective procedures and named II / SiNH2, III / SiNH2 (Fig. 2).
3.3. Research absorptive capacity of the I / SiNH2, II / SiNH2, III / SiNH2 for nickel and
copper ions
The stock solution of Cu (CH3COO) 2 · H2O and Ni (CH3COO) 2 · 4H2O
salt was prepared in appropriate concentration (200 mg / dm3
), respectively.
Then, the stock solution was diluted at concentrations of 10,
15, 20, 25, 30 mg / dm3
, respectively. The effect of concentration on the
adsorptions of Ni (II) and Cu (II) was studied by adding 20.0 mg of
adsorbent silica gel to an aqueous solution of 10 cm3 in different
concentration values, in 50 cm3 Erlenmeyer flask.
The base mixture was shaken for 4 hours at 25 ° C (optimal conditions, at
room temperature and pH 6.0) [18.24] to achieve equilibrium,
respectively. Then, a certain volume of the solution was separated
from the adsorbent and the remaining concentrations of Ni (II) and Cu
(II) was determined by means of an atomic absorption spectrophotometer .
The number of metal ions absorbed by the adsorbent is calculated as
shown in the following equation:
Q = Þ ð Co-CV
W d1Th
where Q is the amount of metal ions adsorbed on the number of units of
plants adsorbent (mmol / g), C0 and C is the concentration of metal ions in
the initial concentration and equilibrium of metal ions in aqueous solution at room temperature and pH 6.0) [ 18.24] to achieve equilibrium, respectively. Then, a certain volume of the solution was separated from the adsorbent and the remaining concentrations of Ni (II) and Cu (II) was determined by means of an atomic absorption spectrophotometer . The number of metal ions absorbed by the adsorbent is calculated as shown in the following equation: Q = Þ ð Co-CV W d1Th where Q is the amount of metal ions adsorbed on the number of units of plants adsorbent (mmol / g), C0 and C is the concentration of metal ions in the initial concentration and equilibrium of metal ions in aqueous solution at room temperature and pH 6.0) [ 18.24] to achieve equilibrium, respectively. Then, a certain volume of the solution was separated from the adsorbent and the remaining concentrations of Ni (II) and Cu (II) was determined by means of an atomic absorption spectrophotometer . The number of metal ions absorbed by the adsorbent is calculated as shown in the following equation: Q = Þ ð Co-CV W d1Th where Q is the amount of metal ions adsorbed on the number of units of plants adsorbent (mmol / g), C0 and C is the concentration of metal ions in the initial concentration and equilibrium of metal ions in aqueous solution, then, a certain volume of solution Justice has been separated from the adsorbent and the remaining concentrations of Ni (II) and Cu (II) was determined by means of an atomic absorption spectroscopy. The number of metal ions absorbed by the adsorbent is calculated as shown in the following equation: Q = Þ ð Co-CV W d1Th where Q is the amount of metal ions adsorbed on the number of units of plants adsorbent (mmol / g), C0 and C is the concentration of metal ions in the initial concentration and equilibrium of metal ions in aqueous solution, then, a certain volume of solution Justice has been separated from the adsorbent and the remaining concentrations of Ni (II) and Cu (II) was determined by means of an atomic absorption spectroscopy. The number of metal ions absorbed by the adsorbent is calculated as shown in the following equation: Q = Þ ð Co-CV W d1Th where Q is the amount of metal ions adsorbed on the number of units of plants adsorbent (mmol / g), C0 and C is the concentration of metal ions in the initial concentration and equilibrium of metal ions in aqueous solution
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