3.3. Effect of the extraction solvent
The choice of extraction solvent is very important for a DLLME
process in order to maximize the extraction efficiency and increase
selectivity for the target compounds. In this case, the extraction
solvent should have low solubility in water, high capability with
the target analytes and be miscible with the dispersive solvent.
Three commonly used solvents including dichloromethane,
chloroform and carbon tetrachloride were examined as an extraction
solvent. The result shows that only carbon tetrachloride can
efficiently extract the desired analytes. So carbon tetrachloride
was selected as an extraction solvent.
The effect of volume of extraction solvent on the absorbance
was also studied in the range of 50–200 lL. According to Fig. 2b,
the absorbance of the complex was increased with increasing the
volume of CCl4 from 50 to 100 lL. Then the absorbance of the complex
decreases gradually when the volume of CCl4 was higher than
120 lL. Hence, 100 lL CCl4 was selected as optimum volume.
3.4. Effect of the disperser solvent
Dispersive solvents have effect on the dispersion, stability and
equilibrium of the ternary-phase system, which should have miscibility
with the extraction solvent and the aqueous sample. Different
solvents (methanol, ethanol, acetonitrile and acetone) were
taken into consideration. Ethanol was selected as dispersive solvent
synthesizing each kind of situation for its best performance
and the lowest toxicity. The effect of the volume of ethanol on
the absorbance was shown in Fig. 2c. The maximum absorbance
was obtained in the range of 200–300 lL. The optimum volume
of ethanol was chosen at 200 lL in all experiments.
3.5. Effect of ascorbic acid concentration
Ascorbic acid is responsible for reducing all the Fe(III) to Fe(II)
form in aqueous phase. The amount of ascorbic acid must be
enough and do not bring about interference. The influence of ascorbic
acid concentration was investigated by varying volumes of
5 103 mol L1 in the range of 0.3–2 mL. The maximum
absorbance was obtained in the range of 0.3–1.0 mL. Hence,
1.0 mL of 5 103 mol L1 ascorbic acid was used for the further
experiments.
3.6. Effect of 5-Br-PADAP concentration
The effect of concentration of 5-Br-PADAP on the absorbance
was evaluated in the range of 0.1 105
–2.5 105
mol L1
. The
results are given in Fig. 2d. The absorbance of the complex
increases with increasing 5-Br-PADAP concentration up to
0.5 105 mol L1
. Then it remains constant at much higher
concentrations. The excessive chromogenic agent could be
co-extracted into the organic phase. Therefore, 2.5 105 mol L1
5-Br-PADAP was selected as the optimal concentration in present
study.
3.7. Interferences
The influence of coexisting ions on the determination of
100 lg L1 of Fe(III) was investigated under the optimized conditions
according to the recommended procedure. The tolerance
limit of various ions is defined as the largest amount making a
variation of less than ±5% in the determination of iron. As shown
in Table 1, most of divalent ions whose complexes with 5-BrPADAP
generally have maximum absorption around 538–586 nm,
do not produce remarkable interfere at the wavelength of
740 nm. In addition, the tolerance limits can be further improved
by the addition of suitable masking agent.
Table 1
Toleran
3.3. Effect of the extraction solventThe choice of extraction solvent is very important for a DLLMEprocess in order to maximize the extraction efficiency and increaseselectivity for the target compounds. In this case, the extractionsolvent should have low solubility in water, high capability withthe target analytes and be miscible with the dispersive solvent.Three commonly used solvents including dichloromethane,chloroform and carbon tetrachloride were examined as an extractionsolvent. The result shows that only carbon tetrachloride canefficiently extract the desired analytes. So carbon tetrachloridewas selected as an extraction solvent.The effect of volume of extraction solvent on the absorbancewas also studied in the range of 50–200 lL. According to Fig. 2b,the absorbance of the complex was increased with increasing thevolume of CCl4 from 50 to 100 lL. Then the absorbance of the complexdecreases gradually when the volume of CCl4 was higher than120 lL. Hence, 100 lL CCl4 was selected as optimum volume.3.4. Effect of the disperser solventDispersive solvents have effect on the dispersion, stability andequilibrium of the ternary-phase system, which should have miscibilitywith the extraction solvent and the aqueous sample. Differentsolvents (methanol, ethanol, acetonitrile and acetone) weretaken into consideration. Ethanol was selected as dispersive solventsynthesizing each kind of situation for its best performanceand the lowest toxicity. The effect of the volume of ethanol onthe absorbance was shown in Fig. 2c. The maximum absorbancewas obtained in the range of 200–300 lL. The optimum volumeof ethanol was chosen at 200 lL in all experiments.3.5. Effect of ascorbic acid concentrationAscorbic acid is responsible for reducing all the Fe(III) to Fe(II)form in aqueous phase. The amount of ascorbic acid must beenough and do not bring about interference. The influence of ascorbicacid concentration was investigated by varying volumes of5 103 mol L1 in the range of 0.3–2 mL. The maximumabsorbance was obtained in the range of 0.3–1.0 mL. Hence,1.0 mL of 5 103 mol L1 ascorbic acid was used for the furtherexperiments.3.6. Effect of 5-Br-PADAP concentrationThe effect of concentration of 5-Br-PADAP on the absorbancewas evaluated in the range of 0.1 105–2.5 105mol L1. Theresults are given in Fig. 2d. The absorbance of the complexincreases with increasing 5-Br-PADAP concentration up to0.5 105 mol L1. Then it remains constant at much higherconcentrations. The excessive chromogenic agent could beco-extracted into the organic phase. Therefore, 2.5 105 mol L15-Br-PADAP was selected as the optimal concentration in presentstudy.3.7. InterferencesThe influence of coexisting ions on the determination of100 lg L1 of Fe(III) was investigated under the optimized conditionsaccording to the recommended procedure. The tolerancelimit of various ions is defined as the largest amount making avariation of less than ±5% in the determination of iron. As shownin Table 1, most of divalent ions whose complexes with 5-BrPADAPgenerally have maximum absorption around 538–586 nm,do not produce remarkable interfere at the wavelength of740 nm. In addition, the tolerance limits can be further improvedby the addition of suitable masking agent.Table 1Toleran
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