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1 Introduction
Struvite or ammonium magnesium phosphate
hexahydrate (AMP) containing urinary stones are
usually found in women. These struvite stones are
infection stones associated with urea generating
organisms1. A study of struvite precipitation and
urease activity in bacteria isolated from patients with
urinary infections and their possible involvement in
the formation of renal calculi has been reported by
Rivadeneyra et al2. The in-vitro inhibition of struvite
crystal growth by acetohydroxyamic acid has been
reported by Downey et al3. They have grown struvite
crystals by Proteus mirabilis in artificial urine in the
presence of urease inhibitors acetohydroxyamic acid
(AHA). In the absence of AHA, struvite crystals
assumed dendritic growth along (100) axis but in the
presence of AHA the growth was reduced and the
crystals achieved octahedral morphology.
Struvite or AMP, (NH4)MgPO4. 6H2O, possesses
orthorhombic unit cell with cell dimensions, a =6.945
, b = 11.208 and c = 6.135 with space group4
Pmn21. These crystals have been grown by single
diffusion gel growth technique and characterized by
powder XRD, FT-IR, thermogravimetry analysis and
dielectric study. The kinetic and thermodynamic
parameters for dehydration as well as decomposition
are obtained from the thermogram.
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#
2 Experimental Details
Sodium metasilicate (SMS) solutions of specific
gravity range from 1.05 to 1.08 were used to prepare
the gel. Aqueous solutions of ammonium dihydrogen
phosphate (ADP) of 0.25, 0.5, 1.0 and 1.5 M
concentrations were mixed with the SMS solution in
appropriate amount so that the pH values 5.0, 5.5, 6.0,
6.5, 7.0, 7.5, 8.0, 8.5, 9.0, 9.5 and 10.0 could be set
for the mixture. The gel solutions were transferred
into the test tubes of 140 mm length and 25 mm
diameter. Magnesium acetate solution of 1.0 M and
1.5 M concentration was gently poured on the set gels
in test tubes. AMP crystals were found to be growing
after one day of pouring solutions for 6.0 to 10.0 pH
values. The growth was completed within a period of
25 days. Crystals with different morphologies were
obtained for different conditions. Rectangular platelets
were obtained for specific gravity 1.07, 0.5 M ADP
and 1 M magnesium acetate concentration at 7.0 pH.
For specific gravity 1.08, 1.5 M ADP and 1.5 M
magnesium acetate concentration at 7.0 pH dendritic
type crystals were obtained. In case of specific gravity
1.07, 0.5 M ADP and 1.0 M magnesium acetate
concentration at 6.5 pH, transparent, prismatic shape
crystals were obtained. Whereas for specific gravity
1.05, 0.5 M ADP and 1.0 M magnesium acetate
concentration at 6.5pH, star shape crystals were
obtained. Elongated dendritic type crystals were
obtained for specific gravity 1.08, 0.5 M ADP and
1.0 M magnesium acetate concentration at 7.5 pH and
needle type crystals were obtained for specific gravity
508
Fig. 1 (ad) Different morphologies of grown struvite crystals, which are (a) rectangular platelets, (b) prismatic, (c) star, (d) elongated
dendritic.
509
510
Standard
Enthalpy
#H
Fig. 5 Coats and Redfern plot for n = 2, where Y = -log10 [{1(1-) 1-n}/{T2(1-n)}] and X = 1/T K-1
log
1
10
T 2 (1 n )
10
aE
55.04 kJ M-1
2 . 3 RT
(1)
where E is the activation energy of the reaction, A the
frequency factor, the fraction of decomposed
material at time t, n the order of reaction and T is the
absolute temperature. The plots of Y = -log10 [{1-(1-)
1-n
}/{T2(1-n)}] versus X = 1/T were straight lines for
different values of n, however, the best linear fit plot
gives the correct value of n. The value of activation
energy is obtained from the slope of the best linear fit
plot. Fig. 5 shows the Coats and Redfern plot. The
ac = 2 f cD t
511
(3)
(4)
512
References
1 Menon M, Parulker B G & Drach G W Urinary lithiasis :
Etiology, Diagnosis and Medical Management, Campbells
Urology, 7th Edn,(W.B. Saunders, New York) 1998, p-26612733.
2 Rivadeneyra M A, Gutierrez Calderon A., Rivadeneyra A
M & Ramos Cormenzana A., Urologia Int, 63 (1999) 188
3 Downey J A, Nickel J C, Clapham L & Mc Lean R J, Br J
Urol., 70 (1992) 355.
4 Encyclopedia of Minerals, 2nd Edn, 1990.
5 Srinivasan N & Natarajan S, Indian J Phys, 70A (1996)563.
6 Joseph K C, Ph D Thesis, Saurashtra University, (2005).
7 Joshi V S & Joshi M J, Cryst Res & Technol, 38 (2003) 817.
8 Joshi V S, Ph D Thesis, Saurashtra University, (2001).
9 Girija E K, Christic Latha S, Kalkura S N, Subramanian C &
Ramasamy P, Mater Chem & Phys, B (1998) 253.