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ABSTRACT:
The solubility of Oxalic acid was studied in different solvents like water, chloroform, acetone, alcohol and many
percentile solutions of different solvents at different temperature. The heat of the solution of Oxalic acid in different
solvent solvents was determined from the temperature–solubility data. The solubility of Oxalic acid in aqueous media
increase with increase temperature while decrease with decrease temperature at constant pressure and electrolytes
concentration. The decrease in the solubility of Oxalic acid was explained on the bases of ionic radii of anions and
cations studies.
INTRODUCTION:
Solubility is the ability of a material to dissolve in water or Temperature -- Generally, an increase in the temperature
any other solvent. The solubility is increase with increase of the solution increases the solubility of a solid solute. A
with temperature of organic compounds. For the few solid solutes, however, are less soluble in warmer
purification of solid the technique are used recrystallization solutions. For all gases, solubility decreases as the
which depends on solute’s different solubilities in solvent. temperature of the solution rises.
When a substance is dissolved in any solvent heat is evolve
or absorbed, the amount of heat depends upon the nature Pressure -- For solids and liquid solutes, changes in
and the quantity or amount of solvent used. When one mole pressure have practically no effect on solubility. For
of solute is dissolved in a solvent the heat is evolved or gaseous solutes, an increase in pressure increases solubility
absorbed is called heat of solution. The quantitative aspect and a decrease in pressure decreases solubility. (When the
of interpreting the solubility data and temperature with heat cap on a bottle of soda pop is removed, pressure is released,
of solution is shown by Van’t Hoff equation. [4] and the gaseous solute bubbles out of solution. This escape
of a gas from solution is called effervescence.)
dlnS/dt = ∆H/RT2 …………………………..(1)
In this equation S is the solubility of the salt in mole per kg The rate of solution is a measure of how fast a substance
of the solvent and ∆H is the of solution per mole. When we dissolves. Some of the factors determining the rate of
integrate the equation (1) then we get the following solution are:
equation.
logS = -∆H/2.303RT + constant ……………..(2) Size of the particles -- When a solute dissolves, the action
takes place only at the surface of each particle. When the
If ∆H is independent of temperture then the curve be a
total surface area of the solute particles is increased, the
straight line of smooth curve, the slop of straight line as -
solute dissolves more rapidly. Breaking a solute into
∆H/2.303RT, the ∆H can be calculated as
smaller pieces increases its surface area and hence its rate of
logS2 – logS1 = ∆H/ 2.303R [1/T2 -1/T1]……..(3) [1] solution. (Sample problem: a cube with sides 1.0 cm long is
The main factors that have an effect on solubility are: cut in half, producing two pieces with dimensions of 1.0 cm
x 1.0 cm x 0.50 cm. How much greater than the surface area
The nature of the solute and solvent -- While only 1 of the original cube is the combined surface areas of the two
gram of lead (II) chloride can be dissolved in 100 grams of pieces? 2.0 cm2
water at room temperature, 200 grams of zinc chloride can
be dissolved. The great difference in the solubilities of the Stirring -- With liquid and solid solutes, stirring brings
of these two substances is the the result of differences in fresh portions of the solvent in contact with the solute,
their natures. thereby increasing the rate of solution.
Received on 13.09.2012 Modified on 18.09.2012
Accepted on 27.09.2012 © AJRC All right reserved
Amount of solute already dissolved -- When there is little
Asian J. Research Chem. 5(11): Nov., 2012; Page 1323-1330 solute already in solution, dissolving takes place relatively
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Asian J. Research Chem. 5(11): Nov., 2012
rapidly. As the solution approaches the point where no nitric acid on sugar, molasses, rice, starch, gum, wool, silk,
solute can be dissolved, dissolving takes place more slowly. hair, and many other organic compounds, which are free
from nitrogen. Berthelot has obtained it synthetically from
Temperature -- For liquids and solid solutes, increasing acetylene, ethylene, propylene, and allylene, by oxidation
the temperature not only increases the amount of solute that with permanganate of potassium.
will dissolve but also increases the rate at which the solute
will dissolve. For gases, the reverse is true. An increase in Description:
temperature decreases both solubility and rate of solution. Oxalic acid crystallizes in colorless, transparent, oblique,
quadrilateral prisms with two-sided summits. The crystals
In order for a solvent to dissolve a solute, the particles of are inodorous, have a strongly acid taste, faintly effloresce
the solvent must be able to separate the particles of the in a dry atmosphere, redden litmus paper, and when pure
solute and occupy the intervening spaces. Polar solvent are completely volatilized by heat, and without becoming
molecules can effectively separate the molecules of other blackened. They dissolve in from 8 to 11 parts of water at
polar substances. This happens when the positive end of a 15.5° C. (60° F.), in their own weight of water at 100° C.
solvent molecule approaches the negative end of a solute (212° F.), and in 4 parts of alcohol; the addition of a small
molecule. A force of attraction then exists between the two quantity of nitric acid to the water causes them to dissolve
molecules. The solute molecule is pulled into solution when more readily. Nearly all the oxalates are insoluble in water,
the force overcomes the attractive force between the solute excepting the alkaline. Oxalate of calcium is insoluble, and
molecule and its neighboring solute molecule. Ethyl alcohol hence oxalic acid is useful as a test for calcium, and is
and water are examples of polar substances that readily usually employed in the form of oxalate of ammonium; if
dissolve in each other. the liquor to be examined contains any free acid, this must
first be neutralized, as the oxalate can only detect calcium
Ammonia, water, and other polar substances do not dissolve in neutral or alkaline fluids. Oxalic acid reduced by
in solvent whose molecules are nonpolar. The nonpolar hydrogen is converted into glycolic and acetic acids, and if
molecules have no attraction for polar molecules and exert the action be kept up sufficiently long the glycolic becomes
no force that can separate them. However, nonpolar wholly formed into acetic acid.
substance such as fat will dissolve in nonpolar solvents.
Oxalic acid may be detected in any solution, by being
Polar solvents can generally dissolve solutes that are ionic. entirely volatilized by heat; by yielding a white precipitate
The negative ion of the substance being dissolved is with nitrate of silver, soluble in nitric acid; and by giving a
attracted to the positive end of a neighboring solvent white precipitate with lime water, which is insoluble in
molecules. The positive ion of the solute is attracted to the water, readily soluble in nitric acid, insoluble in acetic acid,
negative end of the solvent molecule. Dissolving takes and which, when dried and heated to low redness, is
place when the solvent is able to pull ions out of their converted, without blackening, into carbonate of calcium.
crystal lattice or structure. The separation of ions by the Solution of sulphate of calcium produces a bluish-white
action of a solvent is called dissociation. When you precipitate with oxalic acid. Oxalic acid is sometimes
sprinkle table salt (NaCl) in water and stir, the grains of salt contaminated with nitric acid, which gives a faint odor to it,
disappear. From what you have just read (on solubility), and stains the cork of the bottle in which it is kept, yellow.
you have a model to explain what actually happens to the If a very dilute solution of sulphate of indigo, containing the
salt. Sodium chloride, an ionic compound, is made of impure crystals, be boiled, the nitric acid present will
sodium ions and chloride ions. The slightly charged ends of decolorize the solution. On account of the resemblance
water molecules attract these ions. As a result the ions are between crystals of this acid and of magnesium sulphate,
dissociated, or separated by the water molecules and spread the latter has been used as an adulterant. This resemblance
evenly throughout the solution. has also led to cases of poisoning, the person believing the
acid to be Epsom salts. The acid may likewise be used for
Oxalic acid removing iron-rust and ink-stains from linen, and is
Oxalic acid was discovered by Scheele, in 1776, and it is employed in calico printing as a bleaching and discharge
found in the organic as well as in the inorganic kingdoms. agent.
In plants it is generally met in combination with calcium or
potassium; rhubarb, Rumex acetosa, Oxalis acetosella, Action and Toxicology:
phytolacca, belladonna, etc., contain the acid or bin-oxalate Oxalic acid and the oxalates poison the nervous system and
of potassium; rhubarb also contains oxalate of calcium, as the blood, producing, as well, gastro-intestinal lesions. A
likewise do many lichens, and in the human body it forms dose of 60 grains killed a boy (Taylor). Again, by prompt
the mulberry calculus, a frequent form of gravel. In treatment, two cases recovered after a half ounce had been
combination with calcium it is found in ginger, orris-root, swallowed. Death takes place in varying lengths of time, a
squill, valerian, curcuma, quassia, and other drugs. As an circumstance that can not readily be accounted for. Some
ammonium oxalate it is present in the fertilizer guano. In cases die in from 10 minutes to an hour. The above-
the Cicer arietinum or chick pea it occurs in a free mentioned boy died in 8 hours. The symptoms are an
condition. It may also be formed artificially by the action of intensely pure, acid taste, burning of the parts over which
1324
Asian J. Research Chem. 5(11): Nov., 2012
0.008
Heat of solutions: 0.006
Log S was plotted against 1/T , and slop measured . 0.004
Heat of solution was determined by the following formula:
0.002
Slop = H / 2.303 R
0
1 2 3 4 5 6 7 8 9 10 11 12
Temperature
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Asian J. Research Chem. 5(11): Nov., 2012
3: Solubility of oxalic acid in solvent No 3 (Acetone) 5 : Solubility of oxalic acid in solvent No 5 ( methanol)
S# Temperature Oxalic acid Volume of solution S# Temperature Oxalic acid Volume of solution
(Co) Dissolved (gm) (ml) (Co) Dissolved (gm) (ml)
1. 17 0.7 10 1. 10 0.19 10
2. 23 1.69 Do 2. 17 0.27 Do
3. 27 1.87 Do 3. 21 0.36 Do
4. 34 2.01 Do 4. 25 0.4 Do
38 2.16 Do 5. 28 0.51 Do
5.
6. 30 0.62 Do
6. 43 2.66 Do
Chart NO 5
Chart No 3
Oxalic acid Dissolved(gm)
2 per. Mov. Avg. Poly. ( Oxalic acid Dissolved(gm))
3 0.7
0.6
2.5
0.5
2
Solubility
Solubility
0.4
1.5
0.3
1
0.2
0.5 0.1
0 0
1 2 3 4 5 6 7 8 9 10 11 12
Temperature
Te mpe rature
4 : Solubility of oxalic acid in solvent No 4 (Ethanol) 6 : Solubility of oxalic acid in solvent No 6 ( 50% water + 50%
S# Temperature Oxalic acid Volume of solution methanol)
(Co) Dissolved(gm) (ml) S# Temperature Oxalic acid Volume of solution (ml)
1. 17 0.2 10 (Co) Dissolved (gm)
2. 24 0.22 Do 1. 12 0.29 10
3. 28 0.25 Do 2. 16 0.43 Do
4. 32 0.29 Do
3. 22 0.6 Do
5. 36 0.33 Do
4. 27 0.8 Do
6. 40 0.35 Do 33 0.92 Do
5.
6. 40 1.01 Do
CHart NO 4
Chart No 6
Oxalic acid Dissolved(gm)
Poly. ( Oxalic acid Dissolved(gm)) Oxalic acid Dissolved(gm)
0.4 Poly. ( Oxalic acid Dissolved(gm))
0.35
0.3 1.2
1
Solubility
0.25
Solubility
0.2 0.8
0.15 0.6
0.1 0.4
0.05 0.2
0 0
1 2 3 4 5 6 7 8 9 10 11 12 1 2 3 4 5 6 7 8 9 10 11 12
Temperature Temperature
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Asian J. Research Chem. 5(11): Nov., 2012
7 : Solubility of oxalic acid in solvent No 7 (50% water + 50% 9 : Solubility of oxalic acid in solvent No 9 (90% water + 10%
Ethanol) Methanol)
S# Temperature Oxalic acid Volume of S# Temperature Oxalic acid Volume of
(Co) Dissolved (gm) solution (ml) (Co) Dissolved (gm) solution (ml)
1. 10 1.02 10 1. 17 0.49 10
2. 18 1.28 Do 2. 25 0.71 Do
3. 25 1.5 Do 3. 34 0.98 Do
4. 31 1.6 Do 4. 46 1.48 Do
5. 35 1.69 Do 5. 53 1.75 Do
6. 40 1.87 Do 6. 64 2.05 Do
Chart No 7 Chart No 9
Solubility
1.5
Solubility
1.5
1 1
0.5 0.5
0
0
1 2 3 4 5 6 7 8 9 10 11 12
1 2 3 4 5 6 7 8 9 10 11 12
Temperature
Temperature
Solubility
0.8 1
0.6 0.8
0.4 0.6
0.2 0.4
0 0.2
1 2 3 4 5 6 7 8 9 10 11 12 0
Temperature 1 2 3 4 5 6 7 8 9 10 11 12
Temperature
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Asian J. Research Chem. 5(11): Nov., 2012
11 : Solubility of oxalic acid in solvent No 11 ( 50% Water + 50% 13 : Solubility of oxalic acid in solvent No 13 ( 90% Water + 10%
chloroform) Chloroform)
S# Temperature Oxalic acid Volume of S# Temperature Oxalic acid Volume of solution
(Co) Dissolved (gm) solution (ml) (Co) Dissolved (gm) (ml)
1. 16 0.45 10 1. 17 0.26 10
2. 24 0.7 Do 2. 23 0.38 Do
3. 31 0.91 Do 3. 28 0.69 Do
4. 38 1.17 Do 4. 36 1.1 Do
5. 44 1.35 Do 5. 42 1.28 Do
6. 50 1.76 Do 6. 49 1.67 Do
C h art N o 1 3
Chart No 11
O xa lic a c id D is s o lv e d( g m )
Oxalic acid Dissolved(gm) P o ly. ( O xa lic a c id D is s o lv e d ( gm ))
1 .6
2
1 .4
1.5
Solubility
1 .2
1
Solubility
1
0.5
0 .8
0
0 .6
1 2 3 4 5 6 7 8 9 10 11 12
0 .4
Temperature
0 .2
0
12 : Solubility iof oxalic acid in solvent No 12 ( 80% Water + 20% 1 2 3 4 5 6 7 8 9 10 11 12
Chloroform) T e mp e ra ture
S# Temperature Oxalic acid Volume of
(Co) Dissolved(gm) solution(ml)
1. 16 0.39 10 14 : Solubility of oxalic acid in solvent No 14 ( 50% Water + 50%
2. 22 0.65 Do Acetone)
3. 27 0.87 Do S# Temperature Oxalic acid Volume of solution
4. 33 1.09 Do (Co) Dissolved (gm) (ml)
5. 38 1.32 Do 1. 17 0.26 10
6. 43 1.51 Do 2. 23 0.38 Do
3. 28 0.38 Do
4. 36 0.69 Do
Chart N o 12
5. 42 1.1 Do
6. 49 1.67 Do
Oxalic acid Dissolved(gm)
Poly. ( Oxalic acid Dissolved(gm)) C h a rt N o 14
1 2
Solubility
0.8 1.5
solubility
0.6 1
0.4
0.5
0.2
0
0 1 2 3 4 5 6 7 8 9 10 11 12
1 2 3 4 5 6 7 8 9 10 11 12 -0.5
Te mp e ratu re T e mp e rature
1328
Asian J. Research Chem. 5(11): Nov., 2012
15 : Solubility of oxalic acid in solvent No 15 ( 90% Water + 10% Solubility of oxalic acid was less found in acetone as
acetone) compared to other solvents.
S# Temperature Oxalic acid Volume of solution
(Co) Dissolved (gm) (ml)
1. 17 0.09 10 The solubility data obtained from oxalic acid in term of
2. 25 0.38 Do molality (M) in pure water and all alcohol + water mixture
3. 34 0.78 Do was converted to mole fraction (x) by an equation as
4. 43 1.23 Do bellow: [3]
5. 52 1.61 Do
6. 59 1.87 Do X = 0.018M / 1 + 0.018M.
Chart No 15 The solubility of oxalic acid in water in term of mole
fraction (x) was correlated with temperature using a straight
Oxalic acid Dissolved(gm) line equation [4] [5].
Poly. ( Oxalic acid Dissolved(gm)) lnx = A + B (T / K)
1.8
The oxalate coprecipitation is an appropriate method for the
synthesis of precursors for superconducting materials.
1.6
There are some difficulties to control the quantitative
1.4 coprecipitation in the Bi-Sr-Ca-Cu oxalate system. The
1.2 oxalate solubility study shows that Cu-oxalate displays the
solubility
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Asian J. Research Chem. 5(11): Nov., 2012
1330