128E. A. Cantillo, D. R. Delgado, and F. Martinez, J. Mol. Liq. 181, 62 (2013).
(2) Ethanol; C2H6O;[64-17-5]
(3) 1,2-Propanediol; C3H8O2; [57-55-6]
Variables: Prepared by:
Temperature; Solvent composition W. E. Acree, Jr.
Experimental Values
awðsÞ2 : initial mass fraction of component 2 in the binary solvent mixture.
bx1: mole fraction solubility of the solute.
Auxiliary Information Method/Apparatus/Procedure:
Thermostatic mechanical shaker bath, recirculating thermostatic bath, and an UV/visible spectrophotometer.
Excess solute and solvent were placed in a stoppered dark glass flask and allowed to equilibrate with stirring in a thermostatic mechanical shaker bath (for measurements at 303.15, 308.15, and 313.15 K), or in a recirculating thermostatic bath (for measurements at 293.15 and 298.15 K) for at least three days. An aliquot of the saturated solution was removed, isothermally filtered, and diluted quantitatively with an aqueous 0.10 molar sodium hydroxide solution. The molar solubility of the drug was determined by
spectrophotometric analysis at 281 nm. The reported values represent the average of at least three determinations. The densities of the saturated solutions were measured in order to convert the measured molar solubilities (in units of mol dm3) to mole fraction solubilities.
Source and Purity of Chemicals:
(1) Purity not given, Sigma-Aldrich Chemical Company, USA, no purification details were given in the paper.
(2) Absolute, Analytical Reagent grade, Merck Chemical Company, Germany, no purification details were given in the paper.
(3) Purity not given, Dow Chemical Company, USA, no purification details were given in the paper.
Estimated Error:
Technol. 34, 1667 (2011).
(2) Methanol; CH4O;[67-56-1]
(3) Dichloromethane; CH2Cl2; [75-09-2]
Variables: Prepared by:
T/K ¼ 298.2; Solvent composition W. E. Acree, Jr.
Experimental Values
x2
(s)a m1
b Equilibrated solid phasec
0.000 0.135 α-form + solvate
0.227 0.783 α-form + solvate
0.397 0.969 α-form + solvate
0.399 0.930 α-form + solvate
0.532 0.885 α-form + solvate
0.534 0.862 Solvate
0.638 0.731 Solvate
0.640 0.696 Solvate
0.799 0.336 Solvate
1.000 0.0712 α-form + solvate
ax2(s)
: initial mole fraction of component 2 in the binary solvent mixture.
bm1: molal solubility of the solute given as moles of dissolved solute per kilogram of solvent.
cPossible phases:α-form of indomethacin, γ-form of indomethacin, and solid solvate.
Auxiliary Information Method/Apparatus/Procedure:
Constant-temperature bath, analytical balance, confocal Raman microscope equipped with a laser.
Solubility was determined gravimetrically using the shake flask method.
Excess solute and solvent were placed in sealed flasks and allowed to equilibrate in a constant-temperature bath with stirring for 24 h. An aliquot of the saturated solution was withdrawn using a syringe equipped with a 0.20μm pore size cellulose membrane filter. The sample was transferred to a tared container, weighed, and the solvent evaporated at reduced pressure at 309 K until constant mass was obtained. The solubility was calculated from the mass of the solid residue and the mass of the sample analyzed. The equilibrated solid phase was analyzed using a confocal Raman microscope equipped with a laser operating at 785 nm as the excitation source.
Source and Purity of Chemicals:
(1) Purity not given, USP grade, Hawkins, Inc., used as received.
(2) Purity not given, LiChrosolv, Merck Chemical Company, used as received.
(3) Purity not given, stabilized with 0.5% of methanol, Orion, used as received.
Estimated Error:
Technol. 34, 1667 (2011).
(2) Ethanol; C2H6O;[64-17-5]
(3) Dichloromethane; CH2Cl2; [75-09-2]
Variables: Prepared by:
T/K ¼ 298.2; Solvent composition W. E. Acree, Jr.
Experimental Values
x2(s)a m1b Equilibrated solid phasec
0.000 0.135 α-form + solvate
0.170 0.653 Solvate
0.245 0.672 Solvate
0.315 0.710 Solvate
0.316 0.498 Solvate
0.381 0.468 α-form + γ-form
0.442 0.766 Solvate
0.443 0.787 Solvate
0.549 0.610 γ-form + solvate
0.552 0.469 α-form
0.646 0.476 α-form + γ-form
0.729 0.335 γ-form
1.000 0.078 α-form + γ-form
ax2
(s): initial mole fraction of component 2 in the binary solvent mixture.
bm1: molal solubility of the solute given as moles of dissolved solute per kilogram of solvent.
cPossible phases:α-form of indomethacin, γ-form of indomethacin, and solid solvate.
Auxiliary Information Method/Apparatus/Procedure:
Constant-temperature bath, analytical balance, confocal Raman microscope equipped with a laser.
Solubility was determined gravimetrically using the shake flask method.
Excess solute and solvent were placed in sealed flasks and allowed to equilibrate in a constant-temperature bath with stirring for 24 h. An aliquot of the saturated solution was withdrawn using a syringe equipped with a 0.20μm pore size cellulose membrane filter. The sample was transferred to a tared container, weighed, and the solvent evaporated at reduced pressure at 309 K until constant mass was obtained. The solubility was calculated from the mass of the solid residue and the mass of the sample analyzed. The equilibrated solid phase was analyzed using a confocal Raman microscope equipped with a laser operating at 785 nm as the excitation source.
Source and Purity of Chemicals:
(1) Purity not given, USP grade, Hawkins, Inc., used as received.
(2) 99.5%, Altia Chemical Company, used as received.
(3) Purity not given, stabilized with 0.5% of methanol, Orion, used as received.
Estimated Error:
Technol. 34, 1667 (2011).
(2) Methanol; CH4O;[67-56-1]
(3) Propanone; C3H6O;[67-64-1]
Variables: Prepared by:
T/K ¼ 298.2; Solvent composition W. E. Acree, Jr.
Experimental Values
x2(s)a m1b Equilibrated solid phasec
0.000 0.358 α-form + solvate
0.233 0.339 Solvate
0.234 0.585 Solvate
0.407 0.634 γ-form + solvate
0.408 0.621 α-form
0.477 0.635 γ-form
0.478 0.673 Solvate
0.540 0.612 γ-form
0.541 0.640 γ-form + solvate
0.646 0.579 α-form + solvate
0.647 0.576 α-form + γ-form
0.804 0.385 α-form + γ-form
0.805 0.395 γ-form + solvate
1.000 0.071 α-form + solvate
ax2
(s): initial mole fraction of component 2 in the binary solvent mixture.
bm1: molal solubility of the solute given as moles of dissolved solute per kilogram of solvent.
cPossible phases:α-form of indomethacin, γ-form of indomethacin, and solid solvate.
Auxiliary Information Method/Apparatus/Procedure:
Constant-temperature bath, analytical balance, confocal Raman microscope equipped with a laser.
Solubility was determined gravimetrically using the shake flask method.
Excess solute and solvent were placed in sealed flasks and allowed to equilibrate in a constant-temperature bath with stirring for 24 h. An aliquot of the saturated solution was withdrawn using a syringe equipped with a 0.20μm pore size cellulose membrane filter. The sample was transferred to a tared container, weighed, and the solvent evaporated at reduced pressure at 309 K until constant mass was obtained. The solubility was calculated from the mass of the solid residue and the mass of the sample analyzed. The equilibrated solid phase was analyzed using a confocal Raman microscope equipped with a laser operating at 785 nm as the excitation source.
Source and Purity of Chemicals:
(1) Purity not given, USP grade, Hawkins, Inc., used as received.
(2) Purity not given, LiChrosolv, Merck Chemical Company, used as received.
(3) Purity not give, Analytical Reagent grade, Merck Chemical Company, used as received.
Technol. 34, 1667 (2011).
(2) Ethanol; C2H6O;[64-17-5]
(3) Propanone; C3H6O;[67-64-1]
Variables: Prepared by:
T/K ¼ 298.2; Solvent composition W. E. Acree, Jr.
Experimental Values
x2(s)a m1b Equilibrated solid phasec
0.000 0.358 α-form + solvate
0.175 0.501 Solvate
0.255 0.558 γ-form + solvate
0.323 0.589 γ-form + solvate
0.324 0.609 α-form + solvate
0.450 0.593 α-form + γ-form + solvate
0.451 0.601 α-form + γ-form
0.560 0.568 α-form + γ-form + solvate
0.562 0.573 α-form + γ-form
0.657 0.505 α-form + γ-form
0.741 0.423 α-form + γ-form
0.741 0.421 α-form
1.000 0.078 α-form + solvate
ax2
(s): initial mole fraction of component 2 in the binary solvent mixture.
bm1: molal solubility of the solute given as moles of dissolved solute per kilogram of solvent.
cPossible phases:α-form of indomethacin, γ-form of indomethacin, and solid solvate.
Auxiliary Information Method/Apparatus/Procedure:
Constant-temperature bath, analytical balance, confocal Raman microscope equipped with a laser.
Solubility was determined gravimetrically using the shake flask method.
Excess solute and solvent were placed in sealed flasks and allowed to equilibrate in a constant-temperature bath with stirring for 24 h. An aliquot of the saturated solution was withdrawn using a syringe equipped with a 0.20μm pore size cellulose membrane filter. The sample was transferred to a tared container, weighed, and the solvent evaporated at reduced pressure at 309 K until constant mass was obtained. The solubility was calculated from the mass of the solid residue and the mass of the sample analyzed. The equilibrated solid phase was analyzed using a confocal Raman microscope equipped with a laser operating at 785 nm as the excitation source.
Source and Purity of Chemicals:
(1) Purity not given, USP grade, Hawkins, Inc., used as received.
(2) 99.5%, Altia Chemical Company, was used as received.
(3) Purity not given, Analytical Reagent grade, Merck Chemical Company, used as received.
Technol. 34, 1667 (2011).
(2) Methanol; CH4O;[67-56-1]
(3) Ethyl ethanoate; C4H8O2; [141-78-6]
Variables: Prepared by:
T/K ¼ 298.2; Solvent composition W. E. Acree, Jr.
Experimental Values
x2(s)a m1b Equilibrated solid phasec
0.000 0.127 α-form + γ-form + solvate
0.234 0.297 α-form + γ-form
0.407 0.406 α-form + γ-form
0.409 0.393 γ-form
0.437 0.425 α-form
0.478 0.418 α-form
0.539 0.430 α-form
0.541 0.416 α-form + γ-form
0.597 0.418 α-form + γ-form
0.647 0.402 α-form + γ-form
0.650 0.406 γ-form
0.733 0.359 α-form + γ-form + solvate
0.805 0.268 α-form + solvate
1.000 0.071 α-form + solvate
ax2
(s): initial mole fraction of component 2 in the binary solvent mixture.
bm1: molal solubility of the solute given as moles of dissolved solute per kilogram of solvent.
cPossible phases:α-form of indomethacin, γ-form of indomethacin, and solid solvate.
Auxiliary Information Method/Apparatus/Procedure:
Constant-temperature bath, analytical balance, confocal Raman microscope equipped with a laser.
Solubility was determined gravimetrically using the shake flask method.
Excess solute and solvent were placed in sealed flasks and allowed to equilibrate in a constant-temperature bath with stirring for 24 h. An aliquot of the saturated solution was withdrawn using a syringe equipped with a 0.20μm pore size cellulose membrane filter. The sample was transferred to a tared container, weighed, and the solvent evaporated at reduced pressure at 309 K until constant mass was obtained. The solubility was calculated from the mass of the solid residue and the mass of the sample analyzed. The equilibrated solid phase was analyzed using a confocal Raman microscope equipped with a laser operating at 785 nm as the excitation source.
Source and Purity of Chemicals:
(1) Purity not given, USP grade, Hawkins, Inc., used as received.
(2) Purity not given, LiChrosolv, Merck Chemical Company, used as received.
(3) 99.5%, Merck Chemical Company, Germany, used as received.
Estimated Error:
Technol. 34, 1667 (2011).
(2) Ethanol; C2H6O;[64-17-5]
(3) Ethyl ethanoate; C4H8O2; [141-78-6]
Variables: Prepared by:
T/K ¼ 298.2; Solvent composition W. E. Acree, Jr.
Experimental Values
x2(s)a m1b Equilibrated solid phasec
0.000 0.127 α-form + γ-form + solvate
0.328 0.349 α-form
0.451 0.377 α-form + γ-form
0.481 0.374 α-form
0.512 0.387 α-form
0.559 0.366 α-form
0.561 0.367 α-form
0.610 0.358 α-form + solvate
0.656 0.329 α-form + γ-form
0.656 0.331 α-form + γ-form
0.700 0.303 α-form + γ-form
0.742 0.275 γ-form
0.816 0.222 γ-form
0.818 0.219 α-form
1.000 0.078 α-form + γ-form
ax2
(s): initial mole fraction of component 2 in the binary solvent mixture.
bm1: molal solubility of the solute given as moles of dissolved solute per kilogram of solvent.
cPossible phases:α-form of indomethacin, γ-form of indomethacin, and solid solvate.
Auxiliary Information Method/Apparatus/Procedure:
Constant-temperature bath, analytical balance, confocal Raman microscope equipped with a laser.
Solubility was determined gravimetrically using the shake flask method.
Excess solute and solvent were placed in sealed flasks and allowed to equilibrate in a constant-temperature bath with stirring for 24 h. An aliquot of the saturated solution was withdrawn using a syringe equipped with a 0.20μm pore size cellulose membrane filter. The sample was transferred to a tared container, weighed, and the solvent evaporated at reduced pressure at 309 K until constant mass was obtained. The solubility was calculated from the mass of the solid residue and the mass of the sample analyzed. The equilibrated solid phase was analyzed using a confocal Raman microscope equipped with a laser operating at 785 nm as the excitation source.
Source and Purity of Chemicals:
(1) Purity not given, USP grade, Hawkins, Inc., used as received.
(2) 99.5%, Altia Chemical Company, was used as received.
(3) 99.5%, Merck Chemical Company, Germany, used as received.
Estimated Error:
Temperature:0.2 K.
x2(s)
:0.001.
m1:3% (relative error).