Complexo

International Journal of Advanced Scientific and Technical Research
Available online on http://www.rspublication.com/ijst/index.html
Issue 4 volume 4, July-August 2014

ISSN 2249-9954
DETERMINATION OF ALUMINIUM AND MAGNESIUM IONS IN SOME

COMMERCIAL ADSORPTIVE ANTACIDS BY COMPLEXOMETRIC TITRATIONS
*M.D.Sangale; 1A.S.Daptare; 2D.V.Sonawane;

* Head Department of Chemistry, A.A.College, Manchar, Dist-pune(M.S.)
1&2 Department of Chemistry, A.A.College Manchar, Dist- Pune (M.S.)
Abstract:
The study is presented here for titrimetric analysis of consumer products-antacids, which involves active
ingredients Aluminum and Magnesium ions. It is an experiment, involving determination of Aluminum and
Magnesium ions, which enables the student to gain knowledge about complexometric direct and back titrations
containing the concepts and usages of masking, buffer controls and metallic indicators. The commercial antacids
which are analyzed include such as Tablets- Digene, Gelucil MPS, Alcid and Suspensions- Gelucil MPS, Gascidity,
Digusil MPS. As tablets contain silicates therefore silica determination is also possible by gravimetry. The setting of
procedure is done by analyzing standard solution of Aluminum and Magnesium and there synthetic mixtures.
Key words: ingredients of Aland Mg ions, silica, Alcid, Gascidity, Digusil.
Introduction:
The teaching of titrimetric analysis has now introduced purposeful exercise involving analysis of consumer
products such as antacids. S.P.Yang and R.Y.Tsai have recently mentioned complexometric estimation of some
adsorptive antacids. Based on this article an experiment is designed for the determination of aluminum and
magnesium ions in antacids available in Indian market. Antacids- antacids are useful to relive acid indigestion upset
and sour stomach or heartburn. Antacids are the substance, which neutralize or counteracts acidity. Antacids are
widely divided into two classes: Chemical antacids & Adsorptive antacids.
Chemical antacids work by chemical neutralization of gastric acid. e.g. Sodium Bicarbonate. A chemical
antacid shows most rapid action but May cause acid rebound a condition in which the gastric acid returns in
greater concentration after the drug effect has stopped .Adsorptive antacid works by adsorbing the acid. eg. These
are present in following forms:
Al & Mg with identical form in an antacid eg. Al (OH)3 & Mg(OH)2
Al & Mg with different form in an antacid eg. 1) Al(OH)3 & MgO 2) Al2O3 & Mg(OH)2
Al & Mg with identical form and constituent of the same compound eg. Al(OH) 3, Mg(OH)2 & MgAl2(SiO4)2H2O.
Adsorptive antacids are less prone to rebound effect. Antacids with aluminium ion used as the active
ingredient in the form of alumina, aluminium hydroxide and basic aluminium carbonate. Antacids with magnesium
ion usually contain magnesia and magnesium trisilicate, magnesium carbonate, magnesium hydroxide.
Complexometric titration: Complexometric reactions may have uses in analytical chemistry but their classical
application is in complexometric titrations. Here metal ion reacts with suitable ligand to form a complex and
endpoint and it is determined by an indicator or by an appropriate instrumental method. Most simple inorganic
ligands are unidentate which can lead to low complex stability and indistinct end point. As titrants, Multidentade
R S. Publication, [email protected]
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ISSN 2249-9954
ligands, particularly those having 4 or 6 donor groups have two advantages over their unidentate counterparts. First,
they generally react more completely with cations and thus provide sharper end points. Secondly, they ordinarily
react with metal ions in a single step process, whereas complex formation with unidentade ligands usually involving
two or more intermediate species.
EDTA as Titrant: Ethylene diamine tetra acetic acid also called ethylene dinitrito tetra acetic acid, Trillion-B,
Complexone-III and chelation-B.
EDTA has structural formula:
Zwitter ion form of EDTA:
Structure of metal ion EDTA complex:

n
O
O
O
HOOCH2C
CH2COOH
N
H2
C
H2
C
HOOCH2C
H CH COO
2
OOCH2C
H2
C
H2
C
N
O
M
N
O
OOCH2C
CH2COOH
M=Al3+/MG2+/Zn2+
CH2COO
O
O
n=-1/-2/-2
In most of complexometric titrations EDTA is used as a titrants because -Its relatively low prices and it acts as a
hexadentate ligand. EDTA is a species which behaves like an amino acid when dissolved in water. The various
forms of EDTA are often abbreviated as H4Y, H3Y-, H2Y2-, HY3-, Y4-. Relative amounts of this species varies as
function of pH.
pH5
H2Y2-
Na2H2Y
2H+
+
+ 2Na
pH10
Na2H2Y
HY3-
3H+
+
+ 2Na
Fully protonated form, H4Y is only major component in very acidic solutions (pH<3). Through ought the
pH to range of 3-10 the species H2Y2- and HY3- are predominant. The fully unprotonated form Y4- is significant
component only in very basic solutions (pH>10).There are four types of EDTA Titrations as follows: Direct
titration, Back titration, Replacement titration, Alkali metric titration. Here in present experiment involves Direct
titration and Back titration.
Direct titration: Direct titration procedure with a metal ion indicator used when response of indicator to metal ion
is easiest and most convenient to use. The end point may also be determined by Amperometry, Conductometry and
Spectrophotometry.
Back titration: Many metals cannot for various reasons be titrated directly; thus they may precipitated form the
solution in the pH range necessary for the titration or they may form complexes too slowly or a suitable metal
indicator is not available i.e. they may block indicator. In this method excess of standard EDTA solution is added,
the resulting solution is buffered to a desired pH and excess of reagent is back titrated with standard metal ion
solution and end point is detected by suitable indicator.
Metallochromic indicators: The success of an EDTA titration depends upon the precise determination of the end
points. The requisites of metal ion indicators for use in the visual detection of end points include: The colour
reaction should be specific of at least selective. The metal-indicator complex should possess sufficient stability. But
the metal-indicator complex should be less stable than metal EDTA complex. The colour contrast between the free
indicator and metal-indicator complex should be such as to be readily observed. The indicator must be very sensitive
to metal ions so that colour changes occur as near to the equivalence point as possible. The above requirements must
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ISSN 2249-9954
be fulfilled within the pH range at which the titration is performed. The indicators which are used in this experiment
are: Eriochrome black-T, Calmagite, Xylenol orange.
Structure of the indicators:
Eriochrome black-T
Calmagite
Xylenol orange: Tetra sodium salt of xylenol orange

O
NaO
SO3
O2N
SO3
NaO
ONa
HO
OH
N
OH
N
N
OH
H3C
CH3
SO3H
HO
CH3
Yellow --- Slight Red.
Eriochrome black-T is generally represented as: H2InpH10.5-12.5
pH5.3-7.3
H2In-
HIn2-
(Red)
(Blue)
In3(Orange)
Buffers: Generally pH of solution changes on addition of small amount of acids or based to it. But if the solution
contains weak acid and its conjugated base or a weak base and its conjugate acids such solution can resist changes in
pH and is called buffer solution. The ability of buffer solution to resist changes in pH on addition of small amount of
acids or bases is called buffer action. Depending upon pH values buffers solutions are divided into two classes. If the
pH of solution is less than 7 it is called as acidic buffer. eg. Acetate-acetic used as acidic buffer solution. If the pH is
more than 7 it is called basic buffer eg. Bicarbonate-carbonate used as basic buffer solution.
Masking agents: EDTA is very unselective reagent because it complexes with numerous di-, tri- and tetra-valent
cations, so masking is one of the method helps to increase the selectivity. Masking may be defined as the process in
which a substance, without physical separation of it or its reaction products, is so transformed that it does enter into
a particular reaction. Damasking is the process in which masked substance regains its ability to enter into a
particular reaction.
e.g. Tri ethanol amine
Al-TEA complex
N
CH2CH2OH
CH2CH2OH
CH2CH2OH
IIIAl
O
O
O
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ISSN 2249-9954
Information about the antacids used for analysis:

Assay:
Brand
name
(Tablet)
Manufacturer
Average
weight of
Tablet(gm)
Each uncoated chewable tablet

contains
Aluminium
Magnesium
Simethicone = S
Activated
Dimethicone = AD
Dignen
Briocia Pharma (i)

Pvt.ltd. E1,MIDC.Jejuri-412303
Pfizer Ltd. Shirgaon,
Kolhapur-416234.
Alkem Laboratories
Ltd.B.No-AIT-50641
1.208
113.4mg = 4.203
mmoles
147.4mg= 0.606
mmoles
S = 25mg
1.116
96.1mg = 3.561
mmoles
113.4mg = 4.203
mmoles
108.5mg= 4.464
mmoles
147.4mg= 0.606
mmoles
AD = 50mg
GelucilMPS
Alcid
1.201
S = 25mg
*coloured components= Erythrosine & Ponceau4R, *colour=Pink, *Al=Al(OH)3 & MgAl(SiO4)2.H2O, *Mg=Mg(OH)2 & MgAl2(SiO4)2.H2O.
Table-2
Brand name
(Suspension)
Gelucil-MPS
Gascidity
Digucil-MPS
Manufacturer
Pfizer Ltd.
Shirgaon,Kolhapur416234.
ESPI Industries &
Chemical Pvt. Ltd.
Hydrabad-500039.
Cipla Ltd. Mumbai
Central Mumbai400008.
Each teaspoon (5ml) contains
Sorbitol solution
(70%) IP (gm)
Aluminium
Magnesium
86.49mg= 3.205
mmoles
104.2mg= 4.279
mmoles
1.25
86.49mg= 3.205
mmoles
104.2mg= 4.279
mmoles
0.65
86.49mg= 3.205
mmoles
104.2mg= 4.279
mmoles
1.25
* 5ml suspension= 50mg of Activated dimethicone, *coloured component=Erythrosine, *Colour=Pink, *Al = Al(OH) 3, *Mg = Mg(OH)2
Useful information:
In the tablet- Al is in form of Al(OH)3 & MgAl2(SiO4)H2O

Mg is in the form of Mg(OH)2 & MgAl2(SiO4)H2O
In the suspension-Al is in form of Al(OH)3 only.
Mg is in the form of Mg(OH)2 only.
Roll of ingredientsMgAl2(SiO4)H2O:- magnesium aluminium silicate hydrate binds surplus gastric acid & quickly eliminates pain,
heartburn & other discomforts that accompany excessive secretion of gastric acid.
Simethicone:- It is an oral antifoaming agent. Used to reduce bloating, discomfort & pain caused by excess gas in
the stomach or internal tract. It is mixture of polydimethyl siloxane & silica gel (silicon diioide)
Dimeticone:- It is most widely used silicon based organic polymer & it is particularly known its rheological
properties.
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O
Si

ISSN 2249-9954
O
Si
Si
Chemical formula= [(CH3)2OSi]n : It is common additive to antacids.

Sorbitol:- it is also known as glucitol, is a sugar alcohol the body metabolises, it is obtained by reduction of glucose.
It is mostly used as sweetener. IUPAC name of sorbitol is Hexane1, 2, 3, 4, 5, 6 hexanol.
CH2OH
H
HO
H
H
OH
H
OH
OH
CH2OH
Aluminium hydroxide or Al (OH)3:Pharmacologically this compound is also known as Alu-cap or Aludrox, is used as an antacid. The hydroxide reacts
with excess of acid. In the stomach, reducing its acidity of the content of the stomach may in turn help to relive the
symptoms of ulcers heartburn.
Al(OH)3+ 3HCl AlCl3 +3H2O
Magnesium hydroxide or Mg(OH)2:It also known as milk of magnesia & is commonly used as an antacid to remove stomach acid.
Mg(OH)2 + 2HCl MgCl2 + 2H2O
Ponceau 4R:- Its a synthetic coal tar & red azo dye which can be used in variety of food products. Ponceau 4R is
also known as food red 7, C.I., 16255E Number-E214.
Erythrosine:- It is a cherry ponk coal based fluorine dye. E. number-E127.
ONa
O
I
NaO
O
I
max=530nm
Masses of Al3+, Mg2+, SiO2 in Tablets/Suspension:Gelucil MPS:
Mg(OH)2:- by manufacturer:
Mg(OH)2 1Mg
58.305
= 24.305
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250mg

ISSN 2249-9954
= ?
= 104.20mg of Mg.
By stoichiometry: 250mg Mg(OH)2 x

58.305x103mg
1Mole Mg
1Mole Mg(OH)2
24.305x103mg of Mg
Mole of Mg
=104.21 mg of Mg
MgAl2(SiO4)2H2O:by manufacturer:
MgAl2(SiO4)2H2O 1Mg
280.985 = 24.305gm Mg
50mg
=?
=4.325 mg of Mg.
By stoichiometry:
50
280.985x103mg of
1Mole Mg
1Mole MgAl2(SiO4)2H2O
24.305x103mg of Mg
Mole of Mg
MgAl2(SiO4)2H2O
=4.324 mg of Mg
Al(OH)3: by manufacturer:
Al(OH)3 1Al
77.98gm = 26.98gm
250mg
=?
= 86.49 mg of Al.
By stoichiometry: =
250
77.98x103mg of Al(OH)3
1Mole Al
1Mole MgAl(OH)3
26.98x103mg of Mg
Mole of Al
= 86.49 mg of Al.
\MgAl2(SiO4)2H2O: by manufacturer:
MgAl2 (SiO4)2H2O 2Al
280.985
= 53.96gm Al
50mg
=?
= 9.601 mg of Al.
Page 457

By stoichiometry: =
50
280.985x103mg of
2Mole Al

ISSN 2249-9954
26.98x103mg of Al
1Mole MgAl2(SiO4)2H2O
Mole of Al
MgAl2(SiO4)2H2O
=9.601 mg of Al
MgAl2(SiO4)2H2O: by manufacturer:
MgAl2(SiO4)2H2O (SiO4)2
280.985 = 184.172gm Mg
50mg
=?
= 32.77 mg of Mg.
By stoichiometry: =
50
280.985x103mg of 1Mole
2Mole SiO4
MgAl2(SiO4)2H2O
92.086x103mg of SiO4
Mole of SiO4
MgAl2(SiO4)2H2O
= 32.77 mg of SiO4
Brand name
Salt of Al/Mg
Mass of elemental Al/Mg in mg.
Gelucil MPS(Tab)
Al(OH)3
By manufacturer
86.49
By Stoichiometry
86.49
Digene/Alcid (Tab)
Mg(OH)2
MgAl2(SiO4)2 H2O
MgAl2(SiO4)2 H2O
MgAl2(SiO4)2 H2O
Al(OH)3
104.20
4.325
9.601
32.77
103.790
104.21
4.324
9.601
32.77
103.795
Mg(OH)2
MgAl2(SiO4)2 H2O
MgAl2(SiO4)2 H2O
MgAl2(SiO4)2 H2O
Al(OH)3
10.421
4.325
9.601
32.77
86.49
10.421
4.324
9.601
32.77
86.49
Mg(OH)2
104.20
104.21
Gelucil MPS/ Gascidity/ Digucil

MPS (Suspension)
Overview of the method used: First the antacid sample distinguished using acid mixture (HCl+HNO3) then
resulted solution is diluted to known volume. The metal ion from this solution is determined by complexometric
direct and back titration and silica oxide is determined by gravimetry.
Page 458

H
Reactions:
Al3+
Salts ofAl &Mg

ISSN 2249-9954
Mg2+
Volatile Products
Organic Matter
Method A- Determination of both (Al3+ +Mg2+) from mixture:

Aliquote(10ml)
1.pH=10
2.known excess EDTA
3.Heat= Al-EDTA
4.Cool
5.EBT-indicator
Titration with Zn2+
Zn-In complex(purpal)
amount of Al3+& Mg2+
gets determined
Blank titration: used same procedure instead of taking aliquot.

Reactions:
AlY- + MgY2-+ HY3- (unused)
3Al3+ + Mg2+ + HY (excess)
Zn2+
Burette
flask
AlY- +
After titration
2MgY2-+ HY3- (unused) + HIn (blue)
ZnIn(purple)
Method B: Determination of Al3+ from mixture

Aliquote(10ml)
1.pH=5
2.known excess EDTA
3.Heat
4.Cool
5.xylenol orange
Titration with Zn2+
Zn-xylenol complex(orange)
amount of Al3+
gets determined
Page 459

Reactions:
AlY- + MgY2-+ HY3- (unused)
3Al3+ + Mg2+ + HY (excess)
Zn2+
Burette
flask

ISSN 2249-9954
2AlY- + H2Y (unused) + xylenol orange(yellow)
Zn-xylenol orange (slight red)
After titration
Method C: Determination of only Mg2+from mixture

Aliquote(10ml)
1.pH=10
2.TEA-->(Al-TEA)
3.EBT-->MgIn-(wine red)
4.Cool
5.xylenol orange
Direct Titration with EDTA
Free HIn2-(blue)
amount of Mg2+
gets determined
Blank titration: used same procedure instead of taking aliquot.

Reactions:
MgIn-(wine red + H+ + Al-TEA(masked)
2Al3+ + Mg2+ + HIn (blue)
Burette
flask
After titration
EDTA(HY3-)
Al-TEA + MgIn-(wine red

MgY- + HIn2-(blue)
Experimental work:
Reagent preparation: EDTA standard solution (0.01M); Standardize Zn2+ solution (0.01M); Acetate-Acetic buffer
solution; Bicarbonate-Carbonate buffer solution; Xylenol Orange indicator; Eriochrome Black-T indicator
Analysis of Samples:
Individual metal ions: solution of Al3+ is prepared by dissolving known quantity of Al3+ foil in hydrochloric acid
and then diluted to known volume. Solution of Mg2+ is prepared by dissolving known quantity of magnesium
sulphate heptahydrate in minimum amount of water and then diluted to known volume.These solutions are analysed
by using procedure mentioned in article (1.3.2,d)
Synthetic mixture: after individual metal ion analysis synthetic mixture is prepared by taking known quantity of
each solution, mixed them. Then diluted to known volume. This solution is analyzed by using procedure mentioned
in article (1.3.2,d)
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ISSN 2249-9954
Antacid Disintegration: Take an antacid sample and record its brand name, active ingredient and declared quantity
of each component. Weigh the tablet or precisely /measure the volume of suspension precisely. There is no need of
grinding, as tablet simply gets dissolved in acid mixture. Transfer the Tablet/ suspension in 100ml Erlenmeyer flask.
To it add 10 ml of HCl+HNO 3 in the proportion of (3:1). Heat it on open flame till disappearance of brown fumes.
Cool the content adds 20ml of distilled water and again boil it. Remove the flask and allow it to cool and after
cooling filter the mixture. Dilute the filtrate to calibration mark (250ml) with distilled water. Stopper the flask and
mix the solution well by inverting and shaking it repeatedly, label this solution. Dry the residue in an oven and used
for further analysis of silica.
Procedure used:
Method 1: Determination of total (Al3+ &Mg2+) content:
Pipette out a 10ml aliquot of the sample solution into 125ml Erlenmeyer flask followed by adding about
15ml of bicarbonate-carbonate buffer solution (pH10) transfer quantitatively a 35.00ml of aliquot of standard EDTA
solution to the flask using a burette (denoted Vedta). Boil gently the mixture for 5minutes on open flame to speed up
the formation of Al-EDTA complex. Cool it under tap water. Add 5drops of Eriochrome Black-T indicator and mix
it well. The solution should be pure blue in colour if the EDTA is not enough to chelate all of the metallic ions
completely the solution should be wine red in colour, at this wine red solution. Boil again until colour changes to
purpul blue. Back titrate the solution with standardized the Zinc solution until colour changes to purpule at the end
point. Record the volume (as Vzn). Repeat the titration twice and perform the blank titration using same procedure
instead of taking aliquot. Calculate the total mill moles of Aluminium and Magnesium ions in the sample.
Method 2- Determination of only Al3+ content:
Pipette a 10ml aliquot of the sample solution to 125ml Erlenmeyer flask add 15ml of acetate-acetic acid
buffer solution (pH5) to mask the formation of Mg-EDTA complex. Transfer exact 25ml of aliquot of standard
EDTA solution to the flask using burette.(denoted by V EDTA). Boil it gently on open flame for 5minutes to speed up
the formation of Al-EDTA complex. Cool the content under running water and then add 5drops of Xylenol orange
indicator and mix well. The solution should appear lemon yellow in colour at this moment. If the EDTA is not
enough to chelate Aluminium ion, the solution should be deep red in colour. In this case put an additional 5ml or
more aliquot of the EDTA solution to this deep red solution. Boil gently until colour changes to lemon yellow. Back
titrate the solution with a standardized Zinc solution until colour changes to light red at the end point(no deep red
colour should appear). If the light red colour shortly turns back to lemon yellow, continuously titrate the solution
until light red colour persists for more than 3minutes. Record the volume used. Repeat the titration twice and
perform the blank titration using same procedure instead of taking aliquot. Calculate the mill moles of Aluminium
ions in the sample.
Method C: Determination of only Mg2+:Pipette a 10ml aliquot of the sample solution to 125ml of Erlenmeyer flask followed by adding about 15ml
bicarbonate-carbonate buffer solution (pH10) add 3ml of triethanolamine (TEA) and swirl the mixture for 2minutes
to enhance the formation of Al-triethanolamine complex and to mask Al-EDTA complex. Stand it for a while until
turbid solution becomes mostly clear for every observation of end point. Add pinch of Eriochrome black-T indicator
and mix well. The solution should appear wine red colour at this moment. Then direct titrate the solution with
EDTA until colour changes to pure blue at the end point. Record the used volume of EDTA (V EDTA). Repeat the
titration twice. Calculate the mill moles of magnesium in antacid sample.
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ISSN 2249-9954
Method D- Determination of SiO2 content:

Transfer the precipitation along with filter paper in previously weighed porcelain crucible. Heat the crucible on pipe
clay triangle using blue flame keeping the lid slightly open (first use low flame) continue heating with strong flame
till appearance of white ash. Cool the crucible and lid thoroughly and weigh it. Repeat the process of heating,
cooling and weighing till constant weight is obtained.
Results:
Table-1: individual metal ion and synthetic mixture.
A] Individual metal ions:
Method used
Method-B Determination of Al3+ only
Method-C Determination of Mg2+ only
B]Metal ions in synthetic mixture:
Method-A Determination of both Al3+&Mg2+
Method-B Determination of Al3+ only
Method-C Determination of Mg2+ only
Observed mmoles
1.840
2.057
Expected mmoles
2.001
2.060
% error
+8.04
+0.14
0.736
0.335
0.422
0.809
0.384
0.425
+9.02
+13.02
+0.70
Method A-(Determination of total Al3+ &Mg2+ contents)

Brand
name
Volume
of EDTA
used (ml)
Molarit
y MEDTA
DigeneI
30.00
0.01037
Mmoles
of
EDTA
mmEDTA
0.3111
Gelusil
MPS -I
40.00
0.01008
0.4032
Alcid-I
35.00
0.01008
0.3582
Gelusil
MPS-II
40.00
0.01008
0.4032
Gasidity
-II
40.00
0.01008
0.4032
DigusilII
40.00
0.01008
0.4032
Volume of
Zn2+
needed
(ml) VZn
14.10
13.90
13.90
10.90
10.90
10.90
18.10
18.10
18.20
12.40
12.40
12.40
12.6
12.8
12.8
11.4
11.4
11.4
Mmoles
of Zn2+
mmZn
0.141
0.139
0.139
0.109
0.109
0.109
0.181
0.181
0.182
0.124
0.124
0.124
0.126
0.128
0.128
0.114
0.114
0.114
Mmoles of
Al3+ &Mg2+
in 10ml
sample.
0.1701
0.1721
0.1721
0.2942
0.2942
0.2942
0.1718
0.1718
0.1708
0.2792
0.2792
0.2792
0.2772
0.2752
0.2752
0.2892
0.2892
0.2892
Average
mmoles
250ml
of
sample
Expected
mmoles
%
Error
0.1714
4.285
4.809
10.89
0.2942
7.355
8.025
8.34
0.1714
4.286
4.809
+10.8
7
0.2792
6.980
7.484
06.73
0.2758
6.896
7.484
+07.8
4
0.2892
7.230
7.484
3.39
Aliquot of sample used during each analysis= 10ml from 250ml.

Molarity of EDTA used = 0.01M.
mmoles of EDTA =MEDTAx VEDTA
mmoles of Zn2+ = MZn x VZn
mm(Al3++Mg2+)250= mm(Al3+ + Mg2+)10x250
10
I= Tablet and II = Suspension.
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ISSN 2249-9954
Method B-(Determination of Al3+ content)

Brand
name
Volume
of EDTA
used (ml)
Molarity
MEDTA
DigeneI
25.00
0.01037
Mmoles
of
EDTA
mmEDTA
0.2592
Gelusil
MPS -I
30.00
0.01008
0.3024
Alcid-I
25.00
0.01008
0.2520
Gelusil
MPS-II
25.00
0.01008
0.2520
Gasidity
-II
25.00
0.01008
0.2520
DigusilII
25.00
0.01008
0.2520
Volume of
Zn2+
needed
(ml) VZn
12.5
12.5
12.5
18.5
18.5
18.5
12.4
11.8
11.8
14.8
14.8
14.8
14.7
14.7
14.9
15.4
15.4
15.4
Mmoles
of Zn2+
mmZn
0.125
0.125
0.125
0.185
0.185
0.185
0.124
0.118
0.118
0.148
0.148
0.148
0.147
0.147
0.149
0.154
0.154
0.154
Mmoles of
Al3+& Mg2+
in 10ml
sample.
0.1342
0.1342
0.1342
0.1174
0.1174
0.1174
0.1280
0.1340
0.1340
0.1040
0.1040
0.1040
0.1050
0.1050
0.1030
0.0980
0.0980
0.0980
Average
mmoles
250ml
of
sample
Expected
mmoles
%
Error
0.1342
3.355
4.203
+20.19
0.1174
2.935
3.561
+17.57
0.1320
3.300
4.203
+21.45
0.1040
2.600
3.205
+18.87
0.1043
2.607
3.205
+18.64
0.0980
2.450
3.205
+23.55

Molarity of EDTA used = 0.01M.
mm(Al3+)250= mm(Al3+)10x250
10
I= Tablet & II = Suspension.
Method C-Determination of Mg2+ content:

Brand
name
Digene-I
Gelusil
MPS -I
Alcid-I
Gelusil
MPS-II
GasidityII
Digusil-II
Volume of
EDTA
needed(ml)
2.40
2.40
2.30
17.40
17.40
17.50
2.40
2.40
2.40
16.90
16.90
16.90
17.00
17.00
17.00
17.10
17.10
17.10
Molarity
of EDTA
MEDTA
0.01037
0.01008
0.01008
0.01008
0.01008
0.01008
Mmoles of
EDTA=
(mmMg)10
0.248
0.238
0.248
0.1753
0.1764
0.1764
0.0242
0.0242
0.0242
0.1703
0.1703
0.1703
0.1714
0.1714
0.1714
0.1723
0.1723
0.1723
Average
mmoles
Expected
mmoles
% Error
0.02446
250ml
of
sample
0.612
0.606
-0.99
0.1760
4.400
4.464
+1.43
0.0242
0.6048
0.606
+0.33
0.1703
4.258
4.279
+0.49
0.1714
4.284
4.279
-0.11
0.1723
4.309
4.279
-0.70
Page 463


ISSN 2249-9954

mm(Mg2+)250= mm(Mg2+)10x250
10
I= Tablet & II = Suspension.
Method-D Determination of Silica sample

Sr.no.
1
2
3
Brand name of Table

Digene
Gelusil-MPS
Alcid
Observed Mmoles
0.158
0.168
0.166
Expected Mmoles
0.177
0.178
0.178
% Error
+11.23
+05.43
+06.65
Conclusions:
Solvent: Use of distilled water instead of demonized water.

Disintegration reagent: Use of (HCl+HNO3) Acid mixture instead of HCl only because after disintegration by
HCl pink colour remains as it is which interfere in titration.
SiO2: Determination of Silica is possible, as tablet contains silicates.

Indicator: Use of Eriochrome Black-T instead of Calmagite.
Slow titration: In method B slow titration gives good result because the turning back slowly to lemon yellow
colour results from the complex formation of EDTA with Zinc ion at low pH solution which is thermodynamically
more stable and kinetically slower than Zn-indicator complexation.
Fast titration: In method C fast titration gives good results because if the titration is slowly the Aluminium ion
will be released from Al-triethanolamine complex and generate Aluminium Eriochrome black-T complex with wine
red colour so it will give highly positive error due to aluminium blocking Eriochrome black-T indicator.
% Error: Error minimization is not possible in method A and B though we changed all possible conditions like
heating period, pH quantity of buffer, type of buffers (NH4Cl+NH4OH) etc.
Acknowledgements:
We express our gratitude to UGC (WRO) Pune and BCUD University of pune, who have financially
supported through research projects for their kind help.
References:
1.
2.
3.
4.
S.Yang., R.Tsai; J.Chem. educ. 2008,83,908.

D.A.Skoog; D.M.West; F.J.Holler; S.R.Crouch; Analytical Chemistry an introduction,8 th ed. Harcourt
college publishers Forth worth, 2005,458-479.
A.I.Vogel, Quantitative Inorganic Analysis, 4th ed. ELBS & Longman, London (1978) 415-428.
Stratton, W. J.; Steehler, G. A.; Pienta, N. J.; Middlecamp, C. H. Chemistry in Context Laboratory Manual:
Applying Chemistry to Society, 4th ed.; McGraw Hill: Boston, 2003.
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5.
6.
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13.
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17.
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19.
20.
21.
22.

ISSN 2249-9954
Greco, T. G.; Rickard, L. H.; Weiss, G. S. Experiments in General Chemistry: Principles and Modern
Applications, 8th ed.; Prentice Hall: Upper Saddle River, NJ, 2002; (vinegar) pp 6570; (aspirin tablet) pp
107118; (antacid) pp 187192; (water hardness) pp 227234.
Hunt, H. R.; Block, T. F.; McKelvy, G. M. Laboratory Experiments for General Chemistry, 4th ed.;
Brooks/Cole: Montery, CA, 2002; (vinegar) pp 97104; (cola drink) pp 257264.
Wentworth, R. A. D. Experiments in General Chemistry, 7th ed.; Houghton Miffin Company: Boston, 2003;
(vinegar) pp 97104; (water hardness) pp 225236.
Bettelheim, F. A.; Landesberg, J. M. Laboratory Experiments for General, Organic, and Biochemistry, 4th
ed. Harcourt College Publishers: Fort Worth, TX, 2001; (antacid) pp 239246; (vitamin) pp 507514.
Zvi, S.; Pike, R. M.; Foster, J. C. Microscale General Chemistry Laboratory with Selected Macroscale
Experiments, 2nd ed.; John Wiley: New York, 2003; (vitamin) pp 195204; (antacid) pp 249258.
Mowery, K. A.; Blanchard, D. E.; Smith, S.; Betts, T. A. J.Chem. Educ. 2004, 81, 87.
Davis, C. M.; Mauck, M. C. J. Chem. Educ. 2003, 80, 552.
Mabrouk, P. A.; Castriotta, K. J. Chem. Educ. 2001, 78, 1385.
Herman, H. B.; Jezorek, John R.; Tang, Z. J. Chem. Educ. 2000, 77, 743.
Hall, J. F. Experimental Chemistry, 6th ed.; Houghton Mifflin Company: Boston, 2003; (antacid) pp 361
374.
Wink, D. J.; Gislason, S. F.; Kuehn, J. E. Working with Chemistry: A Laboratory Inquiry Program; W. H.
Freeman and Company: New York, 2000; (antacid) pp 103108.
Bishop, C. B.; Bishop, M. B.; Whitten, K. W. Standard and Microscale Experiments in General Chemistry,
4th ed.; Saunders College Publishing: Fort Worth, TX, 2000; (antacid) pp 309 320.
Postma, J. M.; Roberts, J. L., Jr.; Hollenberg, J. L.; Postma, J. M. Chemistry in the Laboratory, 5th ed.; W.
H. Freeman: New York, 2000; (water hardness) pp 367376.
Murov, S.; Stedjee, B. Experiments and Exercises in Basic Chemistry, 6th ed.; John Wiley: New York,
2004; (water hardness) pp 175186.
Weigand, W. A. J. Chem. Educ. 2000, 77, 1334.
Hudson, R. J. M.; Rue, E. L.; Bruland, K. W. Environ. Sci. Technol. 2003, 37, 15531562.
Jo, K. D.; Dasgupta, P. K. Talanta 2003, 60, 131137.
Shui-Ping Yang; Ruei-Ying Tsai Journal of Chemical Education June 2006, 83(6) 906-909
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International Journal of Advanced Scientific and Technical Research

Available online on http://www.rspublication.com/ijst/index.html

Issue 4 volume 4, July-August 2014

DETERMINATION OF ALUMINIUM AND MAGNESIUM IONS IN SOME

*M.D.Sangale; 1A.S.Daptare; 2D.V.Sonawane;

Key words: ingredients of Aland Mg ions, silica, Alcid, Gascidity, Digusil.

International Journal of Advanced Scientific and Technical Research

Issue 4 volume 4, July-August 2014

Zwitter ion form of EDTA:

Structure of metal ion EDTA complex:

International Journal of Advanced Scientific and Technical Research

Issue 4 volume 4, July-August 2014

Xylenol orange: Tetra sodium salt of xylenol orange

Yellow --- Slight Red.

Eriochrome black-T is generally represented as: H2InpH10.5-12.5

International Journal of Advanced Scientific and Technical Research

Issue 4 volume 4, July-August 2014

Information about the antacids used for analysis:

Each uncoated chewable tablet

Briocia Pharma (i)

Each teaspoon (5ml) contains

In the tablet- Al is in form of Al(OH)3 & MgAl2(SiO4)H2O

International Journal of Advanced Scientific and Technical Research

Issue 4 volume 4, July-August 2014

Chemical formula= [(CH3)2OSi]n : It is common additive to antacids.

International Journal of Advanced Scientific and Technical Research

Issue 4 volume 4, July-August 2014

By stoichiometry: 250mg Mg(OH)2 x

International Journal of Advanced Scientific and Technical Research

Issue 4 volume 4, July-August 2014

Mass of elemental Al/Mg in mg.

Gelucil MPS/ Gascidity/ Digucil

International Journal of Advanced Scientific and Technical Research

Salts ofAl &Mg

Issue 4 volume 4, July-August 2014

Method A- Determination of both (Al3+ +Mg2+) from mixture:

Blank titration: used same procedure instead of taking aliquot.

AlY- + MgY2-+ HY3- (unused)

3Al3+ + Mg2+ + HY (excess)

2MgY2-+ HY3- (unused) + HIn (blue)

Method B: Determination of Al3+ from mixture

International Journal of Advanced Scientific and Technical Research

AlY- + MgY2-+ HY3- (unused)

3Al3+ + Mg2+ + HY (excess)

Issue 4 volume 4, July-August 2014

2AlY- + H2Y (unused) + xylenol orange(yellow)

Zn-xylenol orange (slight red)

Method C: Determination of only Mg2+from mixture

Blank titration: used same procedure instead of taking aliquot.

MgIn-(wine red + H+ + Al-TEA(masked)

2Al3+ + Mg2+ + HIn (blue)

Al-TEA + MgIn-(wine red

International Journal of Advanced Scientific and Technical Research

Issue 4 volume 4, July-August 2014

International Journal of Advanced Scientific and Technical Research

Issue 4 volume 4, July-August 2014

Method D- Determination of SiO2 content:

Method A-(Determination of total Al3+ &Mg2+ contents)

Aliquot of sample used during each analysis= 10ml from 250ml.