Isentropic Compressibility and Viscosity of Aqueou
Isentropic Compressibility and Viscosity of Aqueou
Isentropic Compressibility and Viscosity of Aqueou
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Abstract: Densities, speeds of sound, and viscosities of aqueous and methanolic lithium chloride solutions were mea-
sured as functions of concentration, m (mol kg–1) (0.3911 ≤ m ≤ 19.47) and temperature (273.15 ≤ T ≤ 323.15 K).
Measured values of the density, speeds of sound, and viscosity agree well with previously reported data. The isentropic
compressibility isotherms for the aqueous solutions converge at a particular concentration, in the temperature range of
the study, providing crucial information regarding the solvation behaviour of the ions. However, for the methanol solu-
tions, the isentropic compressibility isotherms decrease smoothly with concentration and converge on extrapolation. An-
ion solvation controls the viscosity processes at low temperatures whereas cation solvation controls the same at high
temperatures. Total primary solvation numbers of lithium chloride in water and methanol were estimated to be 6.0 and
1.9, respectively.
Key words: lithium chloride, speeds of sound, viscosity, isentropic compressibility, solvation number.
Résumé : On a mesuré les densités, vitesses du son et viscosités de solutions aqueuses et méthanoliques de chlorure
de lithium en fonction de la concentration, m (mol kg–1) (0,3911 ≤ m ≤ 19,47) et de la température (273,15 ≤ T ≤
323,15 K). Les valeurs mesurées pour les densités, les vitesses du son et les viscosités sont en bon accord avec les
données rapportées antérieurement. Dans le domaine des températures étudiées, les isothermes de compressibilité isen-
trope pour les solutions aqueuses convergent à une concentration particulière, fournissant de l’information cruciale
concernant le comportement des ions vis-à-vis de la solvatation. Toutefois, pour les solutions dans le méthanol, les iso-
thermes de compressibilité isentrope diminue de façon régulière avec la concentration et elles convergent par extrapola-
tion. La solvatation de l’anion contrôle les processus de viscosité à basses températures alors que la solvatation de
l’anion la contrôle à températures élevées. Les nombres totaux de solvatation primaire du chlorure de lithium dans
l’eau et dans le méthanol sont évalués respectivement à 6,0 et 1,9.
Mots clés : chlorure de lithium, vitesses du son, viscosité, compressibilité isentrope, nombre de solvatation.
Can. J. Chem. 80: 175–182 (2002) DOI: 10.1139/V02-007 © 2002 NRC Canada
176 Can. J. Chem. Vol. 80, 2002
X-ray diffraction studies and showed that the primary 0.6812 ≤ m ≤ 9.684 for aqueous and methanolic lithium
hydration shell of Li+ becomes ordered at high temperatures chloride solutions, respectively) and temperature (273.15 ≤
whereas Cl– tends to form a rigid hydration shell at low tem- T ≤ 323.15 K). Thermostat types Schott–Geräte CT 1450,
peratures. Very recently, femtosecond mid-IR non-linear Lauda RLS 6D, or Julabo F32 HP was used to control the
spectroscopic studies (22) have led to a firm conclusion that temperature of all the solutions within ±0.02 K.
the hydration shell of Cl– is rigid relative to that of the cat-
ion. From the above discussion it seems that the temperature Results and discussion
and concentration are the decisive parameters for the flexi-
ble nature of the primary hydration shells of Li+ and Cl–. The experimental densities of aqueous and methanolic
From NMR measurements, Vogrin and Malinowski (23) lithium chloride solutions were found to be linear functions
reported a consistent solvation phenomena of LiCl in metha- of the temperature at a particular concentration. The values
nol and water media and found total solvation numbers of of the parameters of the density equation are given in Ta-
4.5 ± 0.2 and 2.8 ± 0.4, in the respective solvents. Recent ble 1. Figure 1 shows the isotherms of ρ vs. m at 298.15 K
theoretical (24, 25) as well as experimental (26) studies sug- along with the literature data. The measured densities of
gest strikingly different solvation dynamics in methanol rela- aqueous lithium chloride solutions are in good agreement
tive to water. with the literature data (30–32) within ±0.4% at 298.15 K.
In earlier papers (27, 28), it was reported that the The density values of methanolic solutions are comparable
isentropic compressibility isotherms converge at a particular within ±0.5% with the reported data (33) at 287.65 K.
concentration because of the saturation of the primary solva- The measured values of speeds of sound in aqueous and
tion shell of an electrolyte resulting in a rigid structure. On methanolic lithium chloride solutions are collected in Ta-
the other hand, the ion–solvent and ion–ion interactions and ble 1S (Supplementary materials).2 The present values of the
equilibria in different concentration regions have an influ- speeds of sound in aqueous lithium chloride solutions are
ence on transport properties. Therefore, in this paper, we re- comparable within ±0.5% with the reported values (34) at
port speeds of sound and viscosities of aqueous and 298.15 K. We could not compare the speeds of sound values
methanolic lithium chloride solutions as functions of con- for the methanolic lithium chloride solutions because of a
centration and temperature. lack of literature data. However, the present isentropic
compressibilities of methanolic lithium chloride solutions
are ~2.6% higher than the reported values (35) at 298.15 K.
Experimental The isentropic compressibility (κ s) values for aqueous and
Lithium chloride (>99%, E. Merck, Darmstad, Germany) methanolic solutions were calculated by using the relationship
was recrystallized twice from double-distilled water and was [1] κ s = 1/u2ρ
kept in a vacuum desiccator over P2O5. Finally, lithium chlo-
ride was dried by heating at 120°C under vacuum before The isentropic compressibilities against concentration of
preparing solutions. Anhydrous methanol was prepared from aqueous and methanolic lithium chloride solutions are plotted
A.R. grade methanol (>99.5%, Qualigens Fine Chemicals, in Figs. 2 and 3, respectively, at three temperatures. As ear-
Mumbai, India) as described elsewhere (29). All solutions lier, an isothermal equation of the following form (27, 28)
were prepared by mass with ±0.2% accuracy. The lithium [2] κ s = a1 + b1m + c1md
chloride concentrations were checked by gravimetric analy-
sis using AgNO3. was used to fit the isentropic compressibilities over the en-
Densities (ρ) of all solutions were measured with an accu- tire concentration range. In eq. [2], a1, b1, and c1 are the
racy of ±0.01% by using a single-stem graduated pycno- temperature-dependent parameters, d is a constant parame-
meter of ~9 cm3 capacity. The pycnometer was calibrated by ter, and m is the concentration in mol kg–1. The least-squares
using double-distilled water. Speeds of sound (u) in aqueous fitted values of the parameters of eq. [2] are listed in Ta-
and methanolic lithium chloride solutions were measured ble 2. From Table 2 and Figs. 2 and 3, it is apparent that
with an accuracy of ±0.1 m s–1 by using a variable path in- eq. [2] can reproduce the isentropic compressibilities within
terferometer (multifrequency ultrasonic interferometer, M- ±1.1% for aqueous lithium chloride; for methanolic lithium
83, Mittal Enterprises, New Delhi, India) at 2 MHz as de- chloride solutions, it was within ±2.2%. It has been observed
scribed previously (27). that the isentropic compressibility isotherms of aqueous lith-
Viscosities (η) were measured with a Schott–Geräte AVS ium chloride solutions converge in the concentration range
310 unit equipped with micro Ubbelohde viscometers. Vis- of 9.25–13.5 mol kg–1 in the temperature range of the study
cometers of different constants of 0.009595, 0.03004, (Fig. 2).
0.1126, and 0.3099 mm2 s–2 were used to measure the efflux Previous studies (15–17, 21) reveal contradictory views
time in different concentration and temperature ranges. An about the nature of the hydration sphere of Li+ and Cl–.
average of five efflux times was used for viscosity calcula- Tanaka et al. (21) suggested a rigid geometrical arrangement
tions at each temperature. The experimental uncertainties in of water molecules around the Li+ against randomly ar-
the viscosities were within ±0.5%. ranged water molecules around the Cl–. On the other hand,
All the measurements were performed as functions of Yamanaka et al. (17) observed a flexible primary hydration
concentration, m (mol kg–1) (0.3911 ≤ m ≤ 19.47 and sphere for Li+ at low temperatures and an ordered arrange-
2
Supplementary material may be purchased from the Depository of Unpublished Data, Document Delivery, CISTI, National Research Coun-
cil Canada, Ottawa, ON K1A 0S2, Canada (http://www.nrc.ca/cisti/irm/unpub_e.shtml for information on ordering electronically).
Table 1. Least-squares fitted values of the constant parameters of the density equation ρ = a – b(T – 273.15)
(T is in K) for aqueous and methanolic lithium chloride solutions.
m (mol kg–1) a (kg m–3) b (kg m–3 K–1) Standard deviation in ρ
Aqueous lithium chloride
0.3911 1016.5 ± 0.4 0.3627 ± 0.0092 0.22
1.156 1036.6 ± 0.5 0.3930 ± 0.0109 0.16
1.357 1039.0 ± 0.3 0.3609 ± 0.0090 0.18
2.129 1054.9 ± 0.3 0.3622 ± 0.0085 0.22
2.472 1063.3 ± 0.3 0.3361 ± 0.0086 0.22
3.771 1086.1 ± 0.3 0.3440 ± 0.0069 0.16
5.055 1106.4 ± 0.2 0.3323 ± 0.0047 0.11
6.229 1128.5 ± 0.4 0.3559 ± 0.0096 0.23
6.473 1129.4 ± 0.2 0.3319 ± 0.0039 0.09
7.544 1146.0 ± 0.1 0.3277 ± 0.0038 0.09
8.613 1160.6 ± 0.1 0.3290 ± 0.0033 0.06
9.211 1173.7 ± 0.2 0.3262 ± 0.0057 0.14
9.325 1176.1 ± 0.2 0.3418 ± 0.0040 0.08
10.33 1190.7 ± 0.1 0.3340 ± 0.0028 0.07
10.58 1194.6 ± 0.1 0.3414 ± 0.0036 0.09
11.42 1206.8 ± 0.2 0.3445 ± 0.0042 0.09
12.44 1216.8 ± 0.1 0.3446 ± 0.0025 0.05
13.44 1234.4 ± 0.2 0.3597 ± 0.0038 0.07
13.61 1235.3 ± 0.1 0.3541 ± 0.0022 0.05
15.07 1253.1 ± 0.1 0.3648 ± 0.0025 0.06
15.59 1258.7 ± 0.1 0.3643 ± 0.0015 0.04
16.20 1266.8 ± 0.1 0.3712 ± 0.0037 0.07
17.13 1277.4 ± 0.1 0.3805 ± 0.0031 0.07
18.09 1287.8 ± 0.1 0.3848 ± 0.0029 0.06
19.47 1301.6 ± 0.1 0.3886 ± 0.0019 0.05
Methanolic lithium chloride
0.6812 831.73 ± 0.14 0.9114 ± 0.0036 0.05
1.257 848.31 ± 0.22 0.8539 ± 0.0055 0.09
1.881 866.47 ± 0.15 0.8291 ± 0.0037 0.06
2.450 878.86 ± 0.18 0.7810 ± 0.0046 0.08
2.900 890.57 ± 0.14 0.7605 ± 0.0038 0.07
3.801 913.39 ± 0.17 0.7275 ± 0.0044 0.09
4.450 931.14 ± 0.23 0.6927 ± 0.0058 0.12
5.242 949.00 ± 0.06 0.7050 ± 0.0016 0.03
5.985 964.49 ± 0.19 0.6727 ± 0.0047 0.11
6.810 980.83 ± 0.19 0.6704 ± 0.0048 0.11
8.167 1008.8 ± 0.2 0.6682 ± 0.0050 0.11
8.883 1020.2 ± 0.3 0.6710 ± 0.0064 0.13
9.684 1031.7 ± 0.1 0.6496 ± 0.0030 0.07
ment for Cl– at supercooled and glassy states; they also neutron diffraction study. Tao and Lindsay (16) reported a
showed that the hydration number of Li+ decreases with the possible structural transition in aqueous LiCl solution at
decrease in temperature (5.7 at 373 K and 3.5 at 138 K), around 9.4 mol kg–1 (Fig. 11 of ref. 16) and suggested that
whereas the hydration number for Cl– increases with the the charged ions cause polarization of water molecules in
lowering of temperature. The hydration numbers of Li+ and the primary hydration shell. Furthermore, a transition was
Cl– reported in the literature by several researchers using also observed by Millero et al. (36) at 10.7 ± 0.7 mol kg–1 in
different techniques, for easy comparison, are summarized the plot of (u – u0)/m vs. m1/2, where u0 is the speeds of
in Table 3. sound of pure water and correlated the transition with the
It is evident from Fig. 2 that the lowest concentration of hydration structure of the cation. However, we found a tran-
convergence of the isentropic compressibility isotherms is sition at 8.8 ± 0.2 mol kg–1 in the (u – u0)/m vs. m1/2 plot for
9.25 mol kg–1, at which the primary hydration shell of the the present system.
solute is just saturated with κ s,h = 2.548 × 10–10 Pa–1 (where At 9.25 mol kg–1, over the specified temperature range, all
κ s,h is the isentropic compressibility of the hydrated sphere). the water molecules were incorporated in the primary
For the LiCl·nH2O system, a full hydration of Li+ and Cl– hydration shell of lithium chloride resulting in a rigid struc-
has been reported (15) at n = 6 (9.25 mol kg–1) from the ture due to the strong and predominant ion–solvent interac-
Fig. 1. Plots of density (ρ) against molality (m) at 298.15 K for Fig. 3. Variation of isentropic compressibility (κs) with molality
aqueous and methanolic lithium chloride solutions. (m) at 273.15 K (䊊), 298.15 K (䊐), and 323.15 K (∆) for
methanolic lithium chloride solutions (symbols and solid curves
represent experimental and calculated (from eq. [2]) values, re-
spectively, and broken curves represent the extrapolated values).
Table 2. Least-squares fitted values of the parameters of eq. [2] for aqueous and methanolic lithium chloride solutions.
a1 (1 × 1010) b1 (1 × 1010) c1 (1 × 1010) Standard deviation
T (K) (Pa–1) (Pa–1 kg mol–1) (Pa–1 kgd mol–d) d in κs (1 × 1012)
Aqueous lithium chloride
273.15 5.341 ± 0.074 0.1834 ± 0.0419 –1.136 ± 0.035 0.6137 ± 0.0440 1.75
298.15 4.626 ± 0.039 0.2018 ± 0.0480 –0.8167 ± 0.0157 0.7079 ± 0.0404 1.25
323.15 4.350 ± 0.024 0.2541 ± 0.0623 –0.7361 ± 0.0404 0.7777 ± 0.0357 0.890
Methanolic lithium chloride
273.15 8.918 ± 0.065 –1.507 ± 0.175 0.4132 ± 0.1256 1.387 ± 0.059 3.10
298.15 10.70 ± 0.09 – 4.295 ± 1.441 2.723 ± 1.369 1.128 ± 0.048 3.80
323.15 13.32 ± 0.28 3.331 ± 1.963 –5.889 ± 1.719 0.8513 ± 0.0748 6.77
Table 3. Hydration numbers of ions or salt estimated from molecular dynamics (MD), Monte Carlo (MC), ab initio simulation, Raman
spectra (R), NMR spectra (NMR), X-ray (X) and neutron (N) diffraction, and adiabatic compressibility (AC) methods.
Solute Concentrationa Hydration number Method Reference
+ 2
Li (aq) 13.9–0.258 m 3–7 MD, MC
14.0, 3.6, 1.0 m 3.2, 6.0, 6.5 N 4
4 Ab initio 3
4 Ab initio 5
4.1 MD 6
2.64 M, 7.48 M 4 R 7
5.38 m 4 R 8
2M 4 N 9
4 X 10
6 MD 11
5.9 Ab initio 12
6 X 13
6.6 Freezing point depression 14
11.1 m 5.7 (373 K) X 17
3.5 (138 K)
4 Ab initio 39
4 Ab initio 40
Cl–(aq) 11.1 m 6.07 X 17
4.6 m, 10.6 m 6.1 X 18
3.57 m, 9.95 m 5.9, 5.3 N 19
6 N 20
18.5–0.258 m 4.9, 8.5 MD, MC 2
7.2 MD 6
7 Ab initio 12
LiCl(aq) 2.8 NMR 23
6.0 AC 35
LiCl (methanol) 4.5 NMR 23
4.2 AC 35
a
m = mol kg–1, M = mol dm–3.
where κ s,φ is the conventional apparent molal isentropic To bifurcate the total hydration number of lithium chlor-
compressibility (38) of the solution, Vφ is the apparent molal ide into its individual ionic values, we need the reliable
volume of the solute, and κ s,1 and V1 are the isentropic com- primary hydration number of either Li+ or Cl–. Recently, ab
pressibility and the molar volume of the solvent, respec- initio (39) and quasichemical (3) approaches have established
tively. The estimated hydration and (or) solvation numbers that tetra-coordinated Li+(aq) is energetically most favored
of lithium chloride in water and methanol are illustrated in (40). Most attempts (41, 42) to incorporate more than four
Fig. 4. The primary hydration number for lithium chloride in water molecules in the primary hydration sphere lead invari-
water was found to be 6.0 at 9.25 mol kg–1 and is in excel- ably to the migration of extra water molecules into the sec-
lent agreement with the number of available water molecules ondary hydration sphere. Hence, by selecting the primary
per mol of the solute (6.0) at that concentration. The total hydration number of Li+ as 4.0, the primary hydration
primary solvation number of lithium chloride in methanol at number of Cl– is estimated to be 2.0, which is lower than the
16.30 mol kg–1 was estimated to be 1.9, which is much frequently reported values (2, 17–20) but more or less in agree-
smaller than that in water. ment with the findings of Yamanaka et al. (17). We could not
Fig. 4. Hydration/solvation number (nh) vs. molality (m) for (䊊) Fig. 6. Variation of viscosities (η) with molality (m) at
aqueous lithium chloride and (䊐, ∆) methanolic lithium chloride 273.15 K (Ο), 298.15 K (䊐), and 323.15 K (∆) for methanolic
solutions (circles and squares are experimental values and trian- lithium chloride solutions.
gles are extrapolated values) at 298.15 K.
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