IJPSR11-02-09-003 (J.AI - Percb 1)

R. S. Lokhande et al.
/ International Journal of Pharma Sciences and Research (IJPSR)

Vol.2(9), 2011,184-188
Extraction and Spectrophotometric
Determination of Cu (II) Metal ions using
Hydrazinecarboxymide2-[(2-
hydroxyphenyl) methylene (HC22HPM)
as an Analytical Reagent

R. S. Lokhande
1
, Santosh Kulkarni
2
, Shirish Pitale
3
, S.K.Patil

, S. P. Janwadkar
3

1
Department of Chemistry,University of Mumbai, Santa Cruz(E),Mumbai-400098
2
K.M. Agrawal College of Arts,Commerce and Science Kalyan(W) 421301.
3
S.D.Arts,V.S.A. Commerce,M.H.M,Science College, Palghar, DistThane,Maharashtra.401404.
Email: [email protected].
[email protected]

Abstract: A spectrophotometric method has been developed for the determination of Cu (II) using
Hydrazinecarboxymide2-[(2-hydroxyphenyl) methylene (HC22HPM)
1
as an extractive reagent .The reagent
forms a colored complex which has been quantitatively extracted into n-butanol at pH 6.80. The method obeys
Beers law over a range of 1 to 10 ppm. The molar absorptivity is 0.33290 X 10
5
L mol
-1
cm
-1
and Sandells
sensitivity is 0.01220 g cm
-2
respectively. The propose method is very sensitive and selective. This method has
been successfully applied to synthetic and commercial samples.

Keywords: Copper, Spectrophotometric determination, n-butanol, Hydrazinecarboxymide2-[(2-hydroxyphenyl)
methylene (HC22HPM).

INTRODUCTION
The cursory look at the literature survey revels the fact that Copper reacts with many organic reagents. It also
indicates that some of the reagents recommended suffering through limitations such as interference of Ni(II)
2
,
W(VI)
3
, etc. complex formation takes place after several minutes
4,5
some of the regents are not selective
6,7
and
sensitive also some are less stable
8
In this paper a new method has been developed using
Hydrazinecarboxymide2-[(2-hydroxyphenyl) methylene (HC22HPM) for extraction and Spectrophotometric
determination of copper Cu (II), which is simple, selective and sensitive.

EXPERIMENTAL
The reagent Hydrazinecarboxymide2-[(2-hydroxyphenyl) methylene (HC22HPM) was synthesized by the given
procedure
1
. The stock solution of Cu (II) was prepared by dissolving a weighed amount of copper sulphate
pentahydrate in double distilled water and then diluted to the desired volume with double distilled water and
standardized with EDTA
1
. The absorbance and pH measurements were carried out on a Shimadzu UV-Visible
2100 spectrophotometer with 1 cm quartz cells and digital pH meter with combined glass electrode respectively.

PROCEDURE FOR THE EXTRACTION:
0.1 ml of aqueous solution containing 1g of copper metal and 2 ml of reagent was mixed in a 50 ml beaker.
The pH of the solution adjusted to 6.8, it must be noted that the total volume should not exceed 10 ml. The
solution was transferred to 100 ml separatory funnel. The beaker was washed twice with n-butanol and
transferred to the same funnel. The two phases were shaken for two minutes and allowed to separate. The
organic phase was passed through anhydrous sodium sulphate in order to absorb trace amount of water from
ISSN : 0975-9492 184
R. S. Lokhande et al. / International Journal of Pharma Sciences and Research (IJPSR)
Vol.2(9), 2011,184-188
organic phase and then collected in 10 ml measuring flask and made up to the mark with organic solvent if
required. The amount of copper present in the organic phase determined quantitatively by spectrophotometric
method by taking absorbance at 359 nm and that in the aqueous phase was determined by EDTA method.

RESULTS AND DISCUSSION:
The results of various studies are discussed below.

Extraction as a function of pH:
The extraction of copper with Hydrazinecarboxymide2-[(2-hydroxyphenyl) methylene (HC22HPM) has been
studied over the pH range 1-10 and was observed that percentage extraction of Cu (II) is maximum at pH 6.8.

Absorption spectrum:
The absorption spectrum of Cu (II): Hydrazinecarboxymide2-[(2-hydroxyphenyl) methylene (HC22HPM) in n-
butanol shows the maximum absorption at 359 nm. The absorption due to reagent at this wavelength is nearly
negligible. Hence the absorption measurements were carried out at 359nm.

Influence of diluents:
The suitability of solvent was investigated using various organic solvents and the extraction of Cu
(II):HC22HPM was quantitative in n-butanol. Hence, n-butanol was used for further extraction studies as it
gave better and quicker phase separation.

Effect of reagent concentration:

It was found that 2 ml of 0.1% reagent is sufficient for the colour development of the metal
Cu (II) in 10 ml of aqueous solution at pH 6.8.

Effect of equilibration time and stability of the complex:
The equilibration time of 1-2 minute is sufficient for the quantitative extraction of Copper. The stability of
colour of the Cu (II):HC22HPM complex with respect to time shows that the absorbance due to extracted
species is stable up to 24-30 hours, after which slight decrease in absorbance is observed.

Calibration plot:
The Beers law is obeyed from 1 to 10 ppm. The molar absorptivity and sandells sensitivity were calculated to
be is 0.33290 X 10
5
L mol
-1
cm
-1
and 0.01220 g cm
-2
respectively. (Fig 1).

Effect of divalent ions and foreign ions:
The effect of other ions present in various amount indicated no interference in the spectrophotometric
determination of 10 ppm of Copper. The ions which show interference in the spectrophotometric determination
of Copper were overcome by using appropriate masking agents.(Table no 1)

Precision and accuracy:
The precision and accuracy of the developed spectrophotometric method have been studied by analyzing ten
solutions each containing 5 g of Copper in the aqueous phase. The average of ten determinations was 5.023
and variation from mean at 95% confidence limit was 0.0449.

Nature of extracted species:
The composition of extracted Cu (II) : HC22HPM complex has been determined by Jobs continuous variation
method, Slope ratio method and Mole ratio method. It shows that the composition of Cu (II): HC22HPM
complex is 1:2 (Fig 2).

ISSN : 0975-9492 185
Vol.2(9), 2011,184-188
Applications:
The proposed method was successfully applied for the determination of Copper from various alloys, ores and
pharmaceutical samples. The results found to be in good agreement with those obtained by the standard known
method. (Table 2).

References:

[1] Vogel, A. I., Textbook of Quantitative Inorganic Analysis, 3rd ed., London, (1975).
[2] M. Salillas, P. Tarin and M. Blanco. Microchem. J. 31, 61 (1985).
[3] A.K. Malik and A.L. Rao. Ind. J. Chem. 329A, 829 (1983).
[4] T. Sekine and D.J. Dryssen. Inorg. Nuclear. Chem. 26, 2013 (1964).
[5] D.M. Rao, K.H. Reddy, D.V. Reddy and Shrikrishnadevaraya. Ind. J. Chem. 28A, Sec A (1989).
[6] J.R. Jhonston and W.J. Holland. Mikrochim Acta. 1, 126, (1972).
[7] L. Devis and J. Skoda. Chem Listy. 48, 539 (1934).
[8] J. Mineze waski, B. Kerezwak and Z. Marczen. Che. Analy. (Warsaw). 6501 (1961).

Table No 1
Effect of divalent ions and foreign ions:

Sr. No. Interfering ions

Masking agents added
1 pb(II), Sodium thiosulfate
2 Th(IV) Sodium fluoride
3 Citrate, Tartarate, Sodium molybdate
4 Ni(II) Sodium cynide
5 Zr(IV) Sodium fluoride
6 Be(II) Sodium fluoride
7 Se(IV) Oxidation with KMnO4
8 CN-
Boiling with Conc. HNO3 and
Formaldehyde
9 Cr(II) Ammonium acetate
10 Cd(II) Potassium iodide
11 Ag (I) Potassium iodide

Table No 2
Application in different samples
Synthetic mixtures

Synthet i c mi xture

Cu(II) standard
ppm

Cu(II) present ppm
Cu(II) + Cd(II ) + Zr(IV)
(10 + 10 + 10)
10 9. 82
Cu(II) + Pt(IV) + Mn(II)
(10 + 10 + 10)
10 9. 75
Cu(II) + Mg(II) + Ni(II)
(10 + 10 + 10)
10 9. 90
ISSN : 0975-9492 186
Vol.2(9), 2011,184-188
Alloy Samples

Sampl e

% Cu( II)
Standard
method

% Cu(II) present
method
Br ass 80 79. 32
Monel 90 90. 09
Devardas 48 47. 6
Cupra nickel 35 34. 78
German silver 50 49. 8

Pharmaceutical samples

Pharmaceutical samples

Cu(II) standard
ppm

Cu(II) present ppm
Multivitamin tablet 5 4.75
Coversyl tablet 4 3.80
Light honey 0.290 0.278
Dark honey 0.560 0.545

Fig 1

CAL I BRAT I ON CURVE F OR Cu ( I I ) : HC2 2 HP M

0
0.1
0.2
0.3
0.4
0.5
0.6
0 2 4 6 8
A
b
s
o
r
b
a
n
c
e
Concentration of Cu(II)
ISSN : 0975-9492 187
Vol.2(9), 2011,184-188
Fig 2

JOBS CONTINUOUS VARIATION METHOD
0
0.05
0.1
0.15
0.2
0.25
0.3
0.35
0.4
0 0.2 0.4 0.6 0.8 1
A
b
s
o
r
b
a
n
c
e
Mole fraction
ISSN : 0975-9492 188

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R. S. Lokhande et al.

/ International Journal of Pharma Sciences and Research (IJPSR)

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