Density and Viscosity of Zinc Chloride Solution in N-Methylacetamide

Jul 31, 2018 - The densities of zinc chloride in N-methylacetamide solutions have been ... of solutions have been calculated from the experimental dat...
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Density and Viscosity of Zinc Chloride Solution in N‑Methylacetamide over the Temperature Range from 308.15 to 328.15 K at Atmospheric Pressure Alexey A. Dyshin,* Olga V. Eliseeva, and Michael G. Kiselev

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Laboratory of NMR-Spectroscopy and Computer Simulations, G. A. Krestov Institute of Solution Chemistry of the Russian Academy of Sciences, 1 Akademicheskaya Street, Ivanovo 153045, Russia ABSTRACT: The densities of zinc chloride in N-methylacetamide solutions have been measured at atmospheric pressure (99.6 ± 0.8) kPa using an Anton Paar DMA 5000 M digital vibrating U-tube densimeter at temperatures ranging from 308.15 to 328.15 K, with ΔT = 5 K, and in the concentration range from 0 to 1.3 mol·kg−1. The kinematic viscosity for these compositions has been measured under the same thermodynamic conditions as for the measurements of densities, made with an Ubbelohde viscometer. Partial and apparent molar volumes of all components in solutions and the dynamic viscosity and thermal expansion coefficients of solutions have been calculated from the experimental data. The obtained dependencies were analyzed. Growth in the salt concentration increases the solution viscosity, and an increase in the temperature reduces the solution viscosity, at the same time. The increases in temperature and salt concentration lead to a decrease in the zinc chloride partial molar volume.

1. INTRODUCTION Inorganic ions such as Li+, Na+, K+, Mg2+, Ca2+, Zn2+, and Ba2+ play essential and diverse roles in a variety of cellular processes. The zinc ion is part of the group of trace elements necessary for a living organism. The zinc ion located in the cells easily combines with amino acids, peptides, proteins, purine bases, and nucleic acids. Zinc is a cofactor of more than 300 enzymes. Activating many enzymatic reactions is its physiological role. Therefore, the interaction of zinc ions with peptides and proteins is interesting both scientifically and practically. On the other hand, N-methylacetamide (NMA) is a wellknown mimetic of protein interfaces.1 NMA is also widely used as a model of peptides2−4 because it is suitable for modeling hydrogen bonds between peptide groups.5,6 Despite the importance of NMA as a solvent, there are a very limited number of scientific publications reporting experimental studies of the properties of electrolyte solutions in NMA over wide ranges of concentration and temperature.7−9 Therefore, the aim of this work is to obtain experimental data about the density and viscosity of ZnCl2 solutions in NMA at temperatures ranging from 308.15 to 328.15 K, with ΔT = 5 K. The study of the impact of large and small salt concentrations on N-methylacetamide determined the choice of the ZnCl2 concentration.

crystallization of NMA was carried out at 300 K. This procedure was carried out several times. Then calcium oxide was annealed for 8 h at 1373 K. After cooling in a drybox, calcium oxide was added to N-methylacetamide. The mixture was boiled for 3 h at 358 K and then distilled under reduced pressure with the selection of the middle fraction. The initial zinc chloride was dried at 333 K under vacuum. A Karl Fischer coulometer (MKC-710, Kyoto Electronics, Manufacturing Co., ltd) was used to determine the water content for all compounds after purification, and the water content was found to be 0.001% for NMA and 0.003% for ZnCl2. The standard uncertainty of the water content is 0.001%. A summary of the materials that were used is presented in Table 1. The mixtures were prepared gravimetrically using a Sartorius Genius ME235S analytical balance with an experimental uncertainty of ±1 × 10−5 g. The solutions were prepared from degassed solvents under conditions that minimized the moisture uptake from atmospheric air. 2.2. Experimental Apparatus. 2.2.1. Density Measurement. A vibrating U-tube densimeter from Anton Paar GmbH (model DMA 5000M) was used to measure the density of the binary system and neat solvent. The experimental uncertainty provided by the manufacturer for the density is ±1 × 10−6 g· cm−3. The temperature was determined with an integrated platinum resistor thermometer (Pt 100) together with Peltier

2. EXPERIMENTAL SECTION 2.1. Chemicals and Preparation of Solutions. All of the chemicals that were used were received from Acros Organics. All of the reagents were previously dehydrated. The initial Nmethylacetamide was dried. In the first stage, the fractional © 2018 American Chemical Society

Received: May 14, 2018 Accepted: July 17, 2018 Published: July 31, 2018 3130

DOI: 10.1021/acs.jced.8b00399 J. Chem. Eng. Data 2018, 63, 3130−3135

Journal of Chemical & Engineering Data

Article

Table 1. Purity of Chemicals Used in This Study abbreviated name

IUPAC name

NMA

N-methylacetamide

79-16-3

Acros Organics

99+

0.431

ZnCl2

zinc chloride

7646-85-7

Acros Organics

99.99

0.210

CASRN

initial purity, %

source

initial water content, %

purification method fractional crystallizations and distillation vacuum drying

final water content, %

analysis method

0.001

KFCa

0.003

KFCa

a

Coulometric titration by the Karl Fischer method.

where V1 is the partial molar volume of NMA (m3·mol−1), M1 is the molar mass of N-methylacetamide (kg·mol−1), ρ is the mixture density (kg·m−3), m is the molality of ZnCl2 (mol· kg−1), and M2 is the molar mass of zinc chloride (kg·mol−1). The partial molar volumes of zinc chloride were calculated using the following equation20

elements provided by a high-precision thermostat. The temperature setting accuracy reached in the cell was ±0.001 K. At the end of each measurement, the densimeter was calibrated in accordance with the manufacturer’s instructions using water (liquid density standard, ultrapure water, Reinstwasser, Dichte-Kalibrierflussigkeit) and dry air. 2.2.2. Kinematic Viscosity Measurement. The kinematic viscosity was measured using an automatic Ubbelohde capillary viscometer with a suspended level and optical detection of the liquid flow time. The experimental uncertainty was ±2 × 10−9 m2·s−1. The precision of temperature maintenance while measuring the viscosity was ±0.02 K. Before the series of measurements, the viscometer was calibrated using bidistilled and degassed water.

V2 =

Vφ =

Table 2. Comparison of Measured N-Methylacetamide Densities (ρ) and Dynamic Viscosities (η) with Literature Values at Temperatures Ranging from 308.15 to 328.15 Ka solvent NMA

T/K

this work

308.15

0.94601

313.15

0.94181

318.15

0.93759

323.15 328.15

0.93336 0.92917

lit 10,11

0.9459 0.9459112 0.9462413 0.941515 0.941711 0.9422413 0.943610 0.937611 0.9387213 0.939910 0.933516

lit

3.5701

3.312410 3.38013 3.6714 2.904110 3.01215

3.1518

2.7996

2.607210 2.67313

2.4961 2.2447

2.41117

+

M2 ρ

(3)

(4)

where αp is the thermal expansion coefficient (K−1), ρ is the mixture density (kg·m−3), and T is the temperature (K). The experimental data for the densities and kinematic viscosities were used to calculate the dynamic viscosity by the following equation13 η = ρν

The experimental values of density and kinematic viscosity for the Nmethylacetamide−zinc chloride system at temperature ranging from 308.15 to 328.15 K, with ΔT = 5 K, are reported in Table 3.

(5)

where η is the solution dynamic viscosity (Pa·s), ρ is the solution density (kg·m−3), and ν is the solution kinematic viscosity (m2·s−1). The calculated values for the N-methylacetamide−zinc chloride system are reported in Table 3. The dependence of the solution density on electrolyte concentration is linear. As expected, the solution density grows as the zinc chloride concentration increases and decreases as the temperature increases. Figure 1 shows the partial molar volumes of ZnCl2 as a function of concentration. All of the functions decrease with an increase in the zinc chloride concentration. Apparently, this is related to the electrostriction effect. Because NMA has a large dipole moment (4.12 D), the hydrogen-bonded network destruction, as a result of the salt concentration increase, may reduce the partial molar volume of zinc chloride, in accordance with the electrostriction effect.

of these values with literature data. The differences among solvent densities are due to different degrees and methods of solvent purification. The initial experimental data on the density were processed by a linear relationship. Then these data were used to calculate the partial molar volumes of NMA, the partial and apparent molar volumes of zinc chloride, and the thermal expansion coefficients of the solutions according to eqs 1−4.18 The partial molar volumes of N-methylacetamide were calculated using the following equation19 M1 mM1(1000 + mM 2) ∂ρ + ∂m ρ 1000·ρ2

mρρ0

1 i ∂ρ y αp = − jjj zzz ρ k ∂T { p

a

V1 =

ρ0 − ρ

where Vφ is the apparent molar volume of ZnCl2 (m3·mol−1), ρ is the mixture density (kg·m−3), ρ0 is the density of NMA (kg· m−3), M2 is the molar mass of ZnCl2 (kg·mol−1), and m is the molality of zinc chloride, (mol·kg−1). The thermal expansion coefficients of the solutions were calculated from the experimental data by the following equation22

η × 103/Pa·s this work

(2)

where V2 is the partial molar volume of zinc chloride (cm3· mol−1), m is the molality of ZnCl2 (mol·kg−1), ρ is the mixture density (g·m−3), and M2 is the molar mass of zinc chloride (g· mol−1). The apparent molar volumes of zinc chloride were computed by applying the following equation21

3. RESULTS AND DISCUSSION Table 2 presents the density values of the neat solvent over the temperature range from 308.15 to 328.15 K and a comparison

ρ × 10−3/kg·m−3

M2 (1000 + mM 2) ∂ρ − ∂m ρ ρ2

(1) 3131

DOI: 10.1021/acs.jced.8b00399 J. Chem. Eng. Data 2018, 63, 3130−3135

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Table 3. Densities (ρ), Kinematic (ν) and Dynamic (η) Viscosities, Partial Molar Volumes of NMA (V1), Partial Molar Volumes of ZnCl2 (V2), Apparent Molar Volumes of ZnCl2 (Vφ), and Thermal Expansion Coefficients (αp) for the NMethylacetamide−Zinc Chloride System at Temperatures Ranging from 308.15 to 328.15 K, with ΔT = 5 K and P = (99.6 ± 0.8) kPaa ρ × 10−3

m −1

−3

ν × 106 2 −1

η × 103

mol·kg

kg·m

m ·s

Pa·s

0 0.01212 0.02085 0.04092 0.04735 0.05898 0.06108 0.07786 0.09351 0.10252 0.10829 0.17024 0.22357 0.37203 0.69187 1.29873

0.94601 0.94701 0.94803 0.94955 0.95023 0.95113 0.95143 0.95285 0.95427 0.95514 0.95559 0.96131 0.96613 0.97932 1.00777 1.06068

3.774 3.796 3.813 3.847 3.862 3.888 3.892 3.928 3.959 3.976 3.987 4.123 4.256 4.640 5.642 8.307

3.570 3.595 3.615 3.653 3.669 3.698 3.703 3.743 3.778 3.797 3.810 3.964 4.112 4.544 5.686 8.811

0 0.01212 0.02085 0.04092 0.04735 0.05898 0.06108 0.07786 0.09351 0.10252 0.10829 0.17024 0.22357 0.37203 0.69187 1.29873

0.94181 0.94299 0.94383 0.94527 0.94604 0.94691 0.94718 0.94865 0.94999 0.95092 0.95141 0.95710 0.96188 0.97511 1.00350 1.05636

3.347 3.361 3.375 3.410 3.416 3.438 3.444 3.472 3.499 3.520 3.525 3.652 3.754 4.072 4.912 7.087

3.152 3.169 3.186 3.223 3.232 3.255 3.262 3.293 3.324 3.347 3.354 3.495 3.611 3.970 4.929 7.487

0 0.01212 0.02085 0.04092 0.04735 0.05898 0.06108 0.07786 0.09351 0.10252 0.10829 0.17024 0.22357 0.37203 0.69187 1.29873

0.93759 0.93878 0.93963 0.94106 0.94177 0.94272 0.94296 0.94445 0.94573 0.94663 0.94714 0.95284 0.95761 0.97087 0.99923 1.05200

2.986 3.003 3.016 3.047 3.054 3.071 3.076 3.100 3.125 3.140 3.148 3.253 3.343 3.621 4.323 6.099

2.800 2.819 2.834 2.868 2.876 2.895 2.900 2.928 2.955 2.972 2.982 3.099 3.202 3.516 4.320 6.416

0 0.01212 0.02085 0.04092

0.93336 0.93440 0.93524 0.93682

2.674 2.689 2.703 2.731

2.496 2.512 2.528 2.558

V1 × 106 −1

m ·mol

V2 × 106 −1

Vφ × 106 −1

αp × 104 K−1

m ·mol

m ·mol

77.26 77.26 77.26 77.26 77.26 77.26 77.26 77.26 77.26 77.26 77.26 77.27 77.27 77.30 77.39 77.67

45.16 45.06 44.99 44.82 44.76 44.67 44.65 44.51 44.38 44.31 44.26 43.76 43.33 42.17 39.84 35.91

45.110 45.073 44.989 44.962 44.913 44.905 44.835 44.770 44.732 44.708 44.453 44.236 43.642 42.416 40.268

8.930 8.922 8.916 8.902 8.898 8.890 8.889 8.877 8.867 8.861 8.857 8.815 8.780 8.684 8.485 8.137

77.60 77.60 77.60 77.60 77.60 77.61 77.61 77.61 77.61 77.61 77.61 77.61 77.62 77.64 77.73 78.02

45.03 44.93 44.86 44.69 44.63 44.54 44.52 44.38 44.25 44.18 44.13 43.63 43.20 42.04 39.71 35.78

44.980 44.943 44.859 44.832 44.783 44.774 44.704 44.639 44.602 44.578 44.323 44.106 43.512 42.285 40.138

8.970 8.962 8.956 8.942 8.938 8.930 8.928 8.917 8.906 8.900 8.896 8.854 8.819 8.722 8.521 8.170

77.95 77.95 77.95 77.95 77.95 77.95 77.95 77.96 77.96 77.96 77.96 77.96 77.97 77.99 78.08 78.37

44.89 44.79 44.72 44.55 44.50 44.40 44.38 44.24 44.11 44.04 43.99 43.49 43.06 41.91 39.57 35.64

44.843 44.806 44.722 44.695 44.646 44.637 44.567 44.502 44.465 44.441 44.185 43.968 43.374 42.147 40.001

9.011 9.002 8.996 8.982 8.978 8.970 8.968 8.957 8.946 8.940 8.936 8.894 8.858 8.760 8.558 8.204

78.31 78.31 78.31 78.31

44.71 44.61 44.54 44.37

44.660 44.623 44.539

9.051 9.043 9.037 9.023

3

3

3

T = 308.15 K

T = 313.15 K

T = 318.15 K

T = 323.15 K

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DOI: 10.1021/acs.jced.8b00399 J. Chem. Eng. Data 2018, 63, 3130−3135

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Table 3. continued m

ρ × 10−3

ν × 106

η × 103

V1 × 106

V2 × 106

Vφ × 106

αp × 104

mol·kg−1

kg·m−3

m2·s−1

Pa·s

m3·mol−1

m3·mol−1

m3·mol−1

K−1

0.04735 0.05898 0.06108 0.07786 0.09351 0.10252 0.10829 0.17024 0.22357 0.37203 0.69187 1.29873

0.93756 0.93863 0.93878 0.94025 0.94152 0.94241 0.94293 0.94864 0.95337 0.96657 0.99492 1.04770

2.737 2.753 2.755 2.778 2.799 2.814 2.820 2.915 2.994 3.240 3.839 5.348

2.566 2.584 2.586 2.612 2.635 2.652 2.659 2.765 2.854 3.132 3.820 5.603

78.31 78.31 78.31 78.31 78.31 78.31 78.31 78.32 78.32 78.35 78.44 78.72

44.31 44.22 44.20 44.06 43.93 43.86 43.81 43.31 42.88 41.72 39.39 35.47

44.512 44.463 44.455 44.385 44.320 44.282 44.258 44.003 43.786 43.192 41.966 39.821

9.018 9.010 9.009 8.997 8.986 8.980 8.976 8.934 8.897 8.799 8.594 8.237

0 0.01212 0.02085 0.04092 0.04735 0.05898 0.06108 0.07786 0.09351 0.10252 0.10829 0.17024 0.22357 0.37203 0.69187 1.29873

0.92917 0.93023 0.93105 0.93275 0.93320 0.93426 0.93452 0.93597 0.93733 0.93812 0.93860 0.94440 0.94914 0.96236 0.99069 1.04343

2.416 2.430 2.439 2.462 2.468 2.482 2.485 2.504 2.523 2.535 2.540 2.621 2.690 2.904 3.413 4.696

2.245 2.260 2.271 2.296 2.304 2.319 2.322 2.344 2.364 2.378 2.384 2.475 2.553 2.795 3.381 4.900

78.66 78.66 78.66 78.66 78.67 78.67 78.67 78.67 78.67 78.67 78.67 78.67 78.68 78.70 78.79 79.08

44.47 44.37 44.30 44.13 44.07 43.98 43.96 43.82 43.69 43.62 43.57 43.07 42.64 41.49 39.16 35.24

44.420 44.383 44.299 44.272 44.223 44.214 44.144 44.079 44.042 44.018 43.763 43.546 42.953 41.729 39.588

9.093 9.084 9.078 9.064 9.059 9.051 9.050 9.038 9.027 9.021 9.017 8.974 8.937 8.837 8.632 8.272

T = 323.15 K

T = 328.15 K

a

m is the molality of ZnCl2 in the (ZnCl2 + NMA) solutions. Standard uncertainties u are u(T) = 0.01 and 0.02 K for the density and viscosity measurements, respectively, and the expanded uncertainties U are U(m) = 2 × 10−5 mol·kg−1, U(V1) = 3 × 10−8 m3·mol−1, U(V2) = 3 × 10−8 m3· mol−1, U(Vφ) = 2 × 10−9 m3·mol−1, U(αp) = 2 × 10−7 K−1, Ur(ρ) = 0.002, and Ur(ν) = 0.01 for the 0.95 level of confidence.

Data on the density of solutions of lithium chloride1 and calcium chloride7,8 in N-methylacetamide at temperatures of 308.15−328.15 K were previously published. From these data on the equations presented in this article, the volumetric properties of electrolytes were calculated. These dependences are fairly similar to each other, so the values of the partial molar volumes of lithium are the smallest of all of the partial molar volumes of the electrolytes studied. It is possible to construct a sequence of values of the partial molar volumes of electrolytes: Li+ < Ca2+ < Zn2+. On the other hand, the temperature increase destroys the hydrogen-bonded network and, as a result, increases the thermal expansion coefficient (Figure 2) and reduces the solution density and kinematic viscosity. Figure 3 shows the concentration dependence of the dynamic viscosity of zinc chloride solutions in NMA, corresponding to the general concepts of electrolyte behavior in organic solvents. Growth in the salt concentration increases the solution viscosity, while an increase in the temperature reduces the solution viscosity. An increase in the salt concentration in the solution leads to the binding of free solvent molecules; the fluidity of the mixture decreases, so the viscosity of the solution increases.18 Zinc chloride is a strong electrolyte and completely dissociates in solution. Therefore, increasing the salt concentration in the solution leads to an

Figure 1. Partial molar volumes (V2) of zinc chloride as a function of molality (m). This work: black ■, 308.15 K; red •, 313.15 K; green ▲, 318.15 K; blue ▼, 323.15 K; and aqua ⧫, 328.15 K.

It is now generally accepted that the ion in a condensed phase creates the electric field, which has an effect on the volume of solvent molecules.23 The effect of electrostriction, which is observed in solution, has a significant effect on their structure. This leads to changes in the volumetric properties of the solutions. 3133

DOI: 10.1021/acs.jced.8b00399 J. Chem. Eng. Data 2018, 63, 3130−3135

Journal of Chemical & Engineering Data

Article

ORCID

Alexey A. Dyshin: 0000-0002-0263-642X Funding

Work was performed within the state task (registration number 01201260481). This research was partially supported by the Russian Foundation for Basic Research (RFBR grant no. 1703-00309 A). Notes

The authors declare no competing financial interest.

■

ACKNOWLEDGMENTS All the densimetric studies were performed on an Anton Paar DMA 5000M vibrating tube densimeter at the Center for Joint Use of Scientific Equipment, The Upper Volga Region Center for Physico-Chemical Research.

Figure 2. Thermal expansion coefficient (α) for the N-methylacetamide−zinc chloride system as a function of molality (m). This work: black ■, 308.15 K; red •, 313.15 K; green ▲, 318.15 K; blue ▲, 323.15 K; and aqua ⧫, 328.15 K.

■

Figure 3. Dynamic viscosity (η) for the N-methylacetamide−zinc chloride system at different temperatures as a function of molality (m). This work: black ■, 308.15 K; red •, 313.15 K; green ▲, 318.15 K; blue ▲, 323.15 K; and aqua ⧫, 328.15 K.

increase in the number of ions that bind the solvent molecules. The mobility of solvent molecules in solvate spheres decreases, and the solution viscosity increases.

4. CONCLUSIONS In this article, we have measured the viscosity and volumetric characteristics of ZnCl2 solution in N-methylacetamide and analyzed their dependence on temperature and salt concentration. The increase in both parameters leads to a decrease in the zinc chloride partial molar volume. We explain such behavior as follows: the temperature increase and the growth of the salt concentration destroy the hydrogen-bonded network between the solvent molecules. On the other hand, NMA−cation interactions do not change as much as the hydrogen bonds within the range variation of the studied parameters. As a consequence, the large dipole moment of the NMA causes the charge-dipole interactions to increase at high temperatures and salt concentrations, and the partial molar volume of the zinc chloride becomes smaller.

■

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DOI: 10.1021/acs.jced.8b00399 J. Chem. Eng. Data 2018, 63, 3130−3135

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DOI: 10.1021/acs.jced.8b00399 J. Chem. Eng. Data 2018, 63, 3130−3135