Article

pubs.acs.org/jced

Solubility Prediction and Measurement of the System

KNO3−LiNO3−NaNO3−H2O
Xia Yin,*,† Xiuli Yu,† Xiaoya Wu,† Xiaoyi Fu,† Han Wu,† and Dewen Zeng‡
†
College of Chemistry and Chemical Engineering, Hunan University, Changsha, 410082, China,
‡
Qinghai Institute of Salt Lakes, Chinese Academy of Science, Xining, 810008, China
*
S Supporting Information

ABSTRACT: A Pitzer−Simonson−Clegg model has been

applied to calculate the isotherms of the system KNO3−
LiNO3−NaNO3−H2O and its subsystems. The model param-
eters are fitted against experimental solubility and water
activity in the sub-binary and sub-ternary systems of the titled
quaternary system. The solubility of the system KNO3−
LiNO3−NaNO3−H2O at 298.1 and 308.5 K and its subsystems
KNO3−LiNO3−H2O at 283.1 K and LiNO3−NaNO3−H2O at
323.1 K are elaborately measured for verifying the reliability of
the model prediction. Comparisons indicated that the calculated
values are in agreement with our experimental data and
literature data.

■ INTRODUCTION
Lithium salts have great practical values in the fields of energy
and new materials science because of their large heat storage
density, especially used for phase change materials (PCMs)
which can store or release latent heat during phase change
processes. According to our previous work,1,2 it is possible that
the eutectic PCM with a melting point at room temperature
will exist in the quaternary system KNO3−LiNO3−NaNO3−
H2O in which the content of these salts are abundant in the
salt lake of China. Solubility data of the quaternary system
KNO3−LiNO3−NaNO3−H2O and its subsystems are of
essential importance for developing new phase change materials
(PCMs). Because of the lack of complete phase equilibrium
information of this system, it is difficult to obtain the correct Figure 1. Schematic diagram of self-made thermostat: (1) thermostat,
ratio of eutectic components just using experimental methods (2) multiposition magnetic stirrer, (3) reference solution, (4) soft iron
which consume time and money.3 Our previous work1,2 has magnetic stirrer, (5) sample, (6) temperature sensor, (7) lamp.
manifested that the theoretical prediction of the phase diagram
of prospective systems may be an effective way for searching Shanghai China-Lithium Industry Co. Ltd.) with nitric acid
the desirable eutectic materials, but whether the calculated (AR from China National Pharmaceutical Industry Co. Ltd.)
results can be reliable needs to be verified with experimental and was purified by double crystallization for three times with
data. 50 % salt recovery in each time. Sodium tetraphenylborate
In this work, we calculate phase diagrams of the system (> 0.99, mass fraction), potassium nitrate (> 0.99, mass fraction),
KNO3−LiNO3−NaNO3−H2O and its subsystems using a and sodium nitrate (> 0.99, mass fraction) were purchased
Pitzer−Simonson−Clegg model (PSC model).4−7 To verify from China National Pharmaceutical Industry, and the last
the reliability of the model values, we elaborately measure part two were purified by double crystallization for three times
of the solubility data of these systems and compare these experi- with 50 % salt recovery in each time. Doubly distilled water
mental data with model results. (S < 1.5·10−4 S·m−1) was used in the experiment.

■ EXPERIMENTAL SECTION
Chemicals and Apparatus. Lithium nitrate was prepared
Received: March 13, 2013
Accepted: May 7, 2013
by neutralizing lithium carbonate (mass fraction purity > 0.9999, Published: May 20, 2013

© 2013 American Chemical Society 1839 dx.doi.org/10.1021/je400233v | J. Chem. Eng. Data 2013, 58, 1839−1844
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Table 1. The Binary PSC Parameters

Bca = B1 + B2T WW,ca = W1 + W2T UW,ca = U1 + U2T VW,ca = V1 + V2T
electrolyte B1 B2 W1 W2 U1 U2 V1 V2 T/K ref
KNO3 −65.03 0.1905 1.28 −0.0024 −6.79 0.0158 0 0 298.15 to 425.5 13, 17
LiNO3 100.6 −0.287 −7.125 0.00998 2.70 −0.0035 −8.848 0.02233 298.15 to 373.4 13, 16
NaNO3 −517.39 1.7565 −3.066 0.00812 −7.859 0.02376 8.114 −0.02721 298.15 to 424.9 14, 15

Table 2. The Parameters ln k of Solid Phase in the System KNO3−LiNO3−NaNO3−H2O

ln k = A + B/T + CT + D ln T
solid phase A B C D solubility source
KNO3 1366.210 −40957.9 0.36917 −236.448 18
LiNO3 74.431 −3004.1 0 −11.015 19
LiNO3·3H2O 7.898 −3242.5 0 0 19
NaNO3 −84.734 1317.8 0 13.137 18

Table 3. The Ternary PSC Model Parameters

Wijk = a + b(T/K) QW,ijk = c + d(T/K) Uijk = e + f(T/K)
system a b c d e f T /K ref
KNO3−LiNO3−H2O −18.563 0.03972 4.852 −0.0144 −19.265 0.06401 298 to 373 16, 20, 23
KNO3−NaNO3−H2O 6.605 −0.02604 −8.35 0.028 0 0 298 to 323 18
LiNO3−NaNO3−H2O −13.432 0.0316 23.229 −0.06752 −1.0713 0.0036 298 to 323 21, 22

Figure 2. Comparison of calculated and experimental solubility of the

system KNO3−LiNO3−H2O. The lines represent the calculated values
according to Tables 1 to 3, the symbols represent the experimental
data: ☆, 273.1 K;20 ○, 298.1 K;20 △, 298.1 K.23
In this work, solubility measurements were carried out in a
thermostat (TECHNE 18/TE-10D, England) with temperature
stability of ± 0.03 K or were carried out in a self-made
isothermal box (Figure 1). A Sartorius BS224S balance was
used for weighing with an error of ± 0.1 mg.
Measurement of the Solubility of the System KNO3−
LiNO3−H2O at 283.1 K. The solid−liquid phase equilibrium
experiments were carried out in a 250 cm3 Erlenmeyer flask
with ground glass stopper,8 and the flask was immersed in the
thermostat. The sample of the saturated solution KNO3−
LiNO3−H2O containing different ratios of KNO3 and LiNO3
salt was stirred with a magnetic stirrer for 74 h and then kept
static for about 6 h; the sample of saturated solution was taken
with a syringe into a weighed 30 cm3 quartz bottle with cover
1840
Figure 3. Comparison of calculated and experimental solubility of the
system KNO3−NaNO3−H2O. The lines represent the calculated
values according to Table 1 to 3, the symbols represent the experi-
mental data:18 □, 273.1 K; ○, 298.1 K; △, 313.1 K; ▽, 323.1 K;
■, 333.1 K; ☆, 348.1 K.
and was weighed accurately. The content of H2O in the sample
was determined by evaporation to dryness at 503 K, cooling
and weighing. The KNO3 content in the sample was analyzed
with sodium tetraphenylborate9 where the error of method can
be controlled less than 0.5 % in mass percentage. The wet solid
was taken out with a glass scoop and analyzed the same way as
for the solution.
Duplicate analyses of every sample including solution and
wet solid gave a maximum deviation of 0.05 %, and the total
errors of experimental solubility results can be reasonably
evaluated to be less than 0.7 % in mass percentage for the ternary
system KNO3−LiNO3−H2O.
dx.doi.org/10.1021/je400233v | J. Chem. Eng. Data 2013, 58, 1839−1844
Journal of Chemical & Engineering Data Article

Figure 5. Isothermal solubility of the system KNO3−LiNO3−H2O at

283.1 K. symbols represent experimental data in this work: ●, liquid
Figure 4. Comparison of calculated and experimental solubility of the phase composition; ○, corresponding wet solid phase; , predicted
system LiNO3−NaNO3−H2O. The lines represent the calculated isotherm with model parameters of Tables 1 to 3.
values according to Table 1 to 3, the symbols represent the experi-
mental data: □, 298.1 K;21 ○, 323.1 K.22 Table 5. Solubility of the Ternary System LiNO3−NaNO3−
H2O at 323.1 K
Measurement of the Solubility of the Systems LiNO3− composition of saturation solution (100 w)
NaNO3−H2O and KNO3−LiNO3−NaNO3−H2O. For the
solution including Li+ and Na+, it is difficult to analyze LiNO3 H2O NaNO3 predicted solid phase
accurately the concentration of both ions in the meantime. So 0 46.80 53.20 NaNO3
a solid disappearance method10−12 was used for measuring the 15.17 48.54 36.29 NaNO3
solubility of the systems LiNO3−NaNO3−H2O at 323.1 K and 19.83 48.61 31.56 NaNO3
KNO3−LiNO3−NaNO3−H2O at 298.1 K and 308.5 K. The 42.07 42.35 15.58 NaNO3
procedures in detail are repeated briefly as follows: (1) MNO3 53.10 35.32 11.58 NaNO3
(M = K, Li, Na) stock solution was prepared using the salts 57.84 32.51 9.65 LiNO3
purified in this work, and the concentration of solution was 61.00 34.87 4.13 LiNO3
determined by evaporation to dryness at 503 K. (2) A sample 63.23 36.77 0 LiNO3
mixture of known mass of every stock solution was put into
a weighed 150 cm3 flask with a ground glass stopper and a soft last trace of salts was observed to disappear and a clear solution
iron magnetic stirrer. The flask was placed in a self-made was obtained, the total amount of mixture solution and flask
thermostat with an accuracy of ± 0.1 K (see Figure 1) and was was weighed, so the mass percents of dry salts and water in the
kept at a certain constant temperature. (3) The mixture was saturated solution at a constant temperature were calculated.
isothermally evaporated slowly until a small amount of crystal (7) We repeated steps 3, 4, 5, and 6 until the relative error
between the weighed total mass at step 6 was less than 0.3 %.

appeared. (4) The mixed solutions were placed in a refrigerator
and frozen in a long enough time to ensure that all possible
crystal types had formed, and then the frozen sample was
moved to the self-made thermostat and kept at the same
temperature for 24 h. (5) A drop of water (about 0.005 g) was
added to the sample mixture using a syringe every 2 h. When
the turbidity of the solution was decreased, the duration
between additions of water was increased to 5 h. (6) When the
■
THERMODYNAMIC CALCULATION
The expressions of the PSC model for the activity coefficients
of the solvent, cation M and anion X are given in the
Supporting Information.
The binary parameters Bca, WW,ca, UW,ca and VW,ca at various
temperature were fitted against experimental water activity

Table 4. Solubility of the Ternary System KNO3−LiNO3−H2O at 283.1 K

composition of solution (100 w) composition of wet-solid-phase (100 w)
LiNO3 KNO3 H2O LiNO3 KNO3 H2O solid phase
37.22 0.00 62.78 LiNO3·3H2O
4.63 13.66 81.71 1.85 54.53 43.62 LiNO3·3H2O
9.85 10.96 79.19 5.34 56.64 38.02 LiNO3·3H2O
20.91 9.14 69.95 11.27 50.17 38.56 LiNO3·3H2O
35.26 10.32 54.42 42.99 8.92 48.09 LiNO3·3H2O + KNO3
36.91 2.45 60.64 46.05 1.24 52.71 KNO3
36.45 6.14 57.41 46.53 3.00 50.47 KNO3
0.00 17.20 82.80 KNO3

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The parameters of ln k are obtained from the solubility data18,19

of the binary systems and presented in Table 2.
The ternary parameters Wijk, Uijk, and QW,ijk of the systems
KNO3−LiNO3−H2O, KNO3−NaNO3−H2O and LiNO3−
NaNO3−H2O were determined by regressing ternary exper-
imental solubility and water activity16,18,20−23 and listed in
Table 3.
Solubility isotherms in the ternary systems were predicted
and compared with experimental data by applying the param-
eters of Table 1 to 3, and were shown in Figures 2 to 4.
The results showed that the calculated values agree with the
experimental values very well.

■ EXPERIMENTAL RESULTS AND DISCUSSION

Figure 6. Isothermal solubility of the system LiNO3−NaNO3−H2O at
323.1 K: ▲, experimental data in this work; □, reference data;22 ,
calculated isotherm with model parameters of Tables 1 to 3.
data13−17 of the systems KNO3−H2O, LiNO3−H2O and
NaNO3−H2O, and listed in Table 1.
For a hydrated salt Mν+Xν−·nH2O, its solubility product ln k
at a definite temperature for the dissolution reaction
M ν +X ν −·nH 2O = ν+ M+ + ν− X− + nH 2O
can be expressed by
ln k = ν+ ln a M+ + ν− ln a X− + n ln a H2O
The System KNO3−LiNO3−H2O. The solubility of the
system KNO3−LiNO3−H2O at 283.1 K was determined, and
the data are shown in Table 4. We predicted isotherm of this
system at 283.1 K with the PSC model parameters listed in
Tables 1 to 3 and compared with our experimental data (see
Table 4 and Figure 5), and the results are in quite good agreement.
The System LiNO3−NaNO3−H2O. The experimental
solubility data of the ternary system LiNO3−NaNO3−H2O at
323.1 K, which were determined with the solid disappearance
method in this work, are listed in Table 5. These data are most
consistent with Andronova’s data22 and the calculated value of
PSC model (see Figure 6), and the predicted solid phases were
shown in Table 5. The results indicate that the experimental
data from the solid disappearance are reliable.
The System KNO3−LiNO3−NaNO3−H2O. Using the
method of solid disappearance, we determined the solubility
data of the system KNO3−LiNO3−NaNO3−H2O at 298.1 and

Table 6. Comparison of Experimental Data of the System KNO3−LiNO3−NaNO3−H2O and Model Predicted Values at 298.1 K
dry basis quality ratio (100 w)

KNO3 LiNO3 NaNO3 wH2O (exp)a wH2O (pred)b Re (%)c predicted solid phase
1 4.31 83.49 12.20 46.284 46.427 0.309 LiNO3·3H2O+NaNO3
2 11.78 77.21 11.01 42.095 42.336 0.572 LiNO3·3H2O+NaNO3
3 27.57 61.12 11.31 35.838 35.661 0.494 NaNO3
4 30.13 39.46 30.41 44.087 44.019 0.154 NaNO3
5 30.32 0 69.68 41.935 41.549 0.920 NaNO3
6 31.33 20.86 47.81 43.782 43.674 0.249 NaNO3
average Red 0.450
a
: wH2O(exp) are experimental mass percent of H2O in the saturated solution. b: wH2O (pred) are PSC calculated mass percent of H2O in the
saturated solution. c: Re (%) = (|wH2O (exp) − wH2O (pred)|)/(wH2O (exp))·100. d: Average Re = ∑ni Re/n.

Table 7. Comparison of Experimental Data of the System KNO3−LiNO3−NaNO3−H2O and Model Predicted Values at 308.5 K
dry basis quality ratio (100 w)

KNO3 LiNO3 NaNO3 wH2O (exp)a wH2O (pred)b Re (%)c predicted solid phase
1 5.78 59.81 34.41 48.277 50.227 4.0392 NaNO3
2 10.85 79.23 9.92 32.06 31.379 2.124 LiNO3
3 17.37 72.81 9.82 28.645 28.821 0.615 LiNO3
4 22.63 67.78 9.59 26.434 26.690 0.968 LiNO3
5 32.78 47.21 20.01 35.321 35.415 0.267 NaNO3
6 33.98 32.81 33.21 39.016 38.886 0.333 NaNO3
7 35.03 18.38 46.59 38.893 38.978 0.218 KNO3+NaNO3
8 35.02 64.98 0 24.146 24.423 2.294 KNO3+LiNO3
Average Red 1.357
a
: wH2O(exp) are experimental mass percent of H2O in the saturated solution. b: wH2O (pred) are PSC calculated mass percent of H2O in the
saturated solution c: Re (%) = (|wH2O (exp) − wH2O (pred)|)/(wH2O (exp))·100. d: Average Re = ∑ni Re/n.

1842 dx.doi.org/10.1021/je400233v | J. Chem. Eng. Data 2013, 58, 1839−1844

Journal of Chemical & Engineering Data
Figure 7. Phase diagram of the system KNO3−LiNO3−NaNO3−H2O
at 298.1 K: ○, experimental data in this work; lines are predicted
values with PSC model: bold line, eutectic line; ---, predicted waterline
with the same value, value = mass of H2O/mass of the saturated
solution ×100 %.
Figure 8. Phase diagram of the system KNO3−LiNO3−NaNO3−H2O
at 308.5 K: ○, experimental data in this work; lines are predicted
values with PSC model: bold line, eutectic line predicted with PSC
model; ---, predicted waterline with the same value, value = mass of
H2O/mass of the saturated solution ×100 %.
308.5 K and obtained the mass percents of every dry salt
(KNO3, LiNO3, and NaNO3) and mass percent of H2O in the
saturated solutions (see Tables 6 and 7). Combining the binary
and ternary parameters of Tablex 1 to 3 with the mass percents
of dry salts (columns 2 to 4 in Tables 6 and 7), we predicted
the mass percent of H2O in the saturated solution of the system
KNO3−LiNO3−NaNO3−H2O at 298.1 and 308.5 K and
predicted the corresponding solid phases, as shown in columns
6 and 8 of Table 6 and Table 7, and gave the relative errors
between the experimental mass percents of H2O and predicted
values (see column 7 of Table 6 and Table 7). The average
relative error between the experimental data and predicted
1843
Article
values at 298.1 K and 308.5 K are less than 0.5 % and 1.36 %,
respectively. The reason that the predicted values at 298 K are
more accurate than the ones at 308 K may be the parametriza-
tion of model was obtained by regressing the binary and ternary
experimental data at different temperatures including 298 K but
without 308 K, so the prediction difficulty increases at 308.5 K.
Furthermore we predicted the isothermal eutectic lines and
waterlines with the same mass percent of H2O in the saturated
solution at 298.1 and 308.5 K (see Figure 7 and Figure 8). The
results of the predicted values and experimental data are seen to
be in good agreement, so it can be reasonably believed that the
phase diagram of the system KNO3−LiNO3−NaNO3−H2O
predicted using the PSC model parameters of Table 1 to 3 are
reliable.
■ CONCLUSIONS
We calculated the solubility of the ternary systems KNO3−
LiNO−H2O, LiNO3−NaNO3−H2O, and KNO3−NaNO3−
H2O with a PSC model, based on available experimental data,
and we predicted the solubility of the quaternary system
KNO3−LiNO3−NaNO3−H2O at 298.1 and 308.5 K. To check
the reliability of the model calculation, the solubility of the
system KNO3−LiNO3−H2O at 283.1 K was determined using
the phase equilibrium method, and the solubilities of the system
LiNO3−NaNO3−H2O at 323.1 K and KNO3−LiNO3−
NaNO3−H2O at 298.1 and 308.5 K were measured with the
solid disappearance method.
Comparisons showed that the PSC model can calculate
accurately the phase diagrams of the ternary salt-water systems
by using available binary and ternary experimental data. That
the predicted solubility data are in good agreement with the
experimental results for the quaternary system indicates that the
PSC model parameters determined in this work are reliable and
thus can serve for the theoretical design in PCMs development.
■
*
ASSOCIATED CONTENT
S Supporting Information
The expressions of the PSC model for the activity coefficients
of the solvent, cation M, and anion X. This material is available
free of charge via the Internet at http://pubs.acs.org.
■ AUTHOR INFORMATION
Corresponding Author
*E-mail: yinxia@hnu.edu.cn.
Funding
This work was financially supported by the National Natural
Science Foundation of China (Grant J1210040, J1103312), the
Hunan Provincial Natural Science Foundation of China (Grant
11JJ2011), China’s Ministry of Science and Technology (Grant
2012AA052503)
Notes
The authors declare no competing financial interest.
■
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