Journal of Thermal Analysis and Calorimetry

https://doi.org/10.1007/s10973-018-7058-5(0123456789().,-volV)(0123456789().,-volV)

Investigation on standard molar enthalpy of combustion, specific heat

capacity and thermal behavior of methionine
Qian Niu1• Cairong Zhou1 • Zili Zhan1

Received: 26 October 2017 / Accepted: 7 February 2018

 Akadémiai Kiadó, Budapest, Hungary 2018

Abstract
The standard molar enthalpy of combustion of methionine was determined to be - 6661.03 kJ mol-1 by XRY-1C
microcomputer oxygen bomb calorimeter. The standard molar enthalpy of formation was calculated to be
3121.35 kJ mol-1 based on the standard molar combustion enthalpy. The thermal stability behavior of methionine was
studied by the thermal gravimetric analysis. The results show that melting process of methionine was accompanied by the
decomposition reaction in the temperature range of 500.15–520.15 K, displayed one-stage decomposition process. The
absorb heat of methionine was obtained to be 974.34 kJ mol-1 (6530.00 J g-1) at 550.51 K by DSC-60 differential
scanning calorimetry. Moreover, the specific heat capacity of methionine from 373.15 to 453.15 K in the solid state was
measured, and then the relationship between the constant pressure specific heat capacity Cp and the temperature has been
established. These data provide a thermodynamic basis for process development, engineering design and industrial pro-
duction of methionine.

Keywords Methionine  Enthalpy of combustion  Specific heat capacity  Thermal behavior

List of symbols Introduction

c Specific heat capacity (J g-1 K-1 or kJ kg-1 K-1)
Q Heat of combustion (kJ mol-1) Methionine (CAS: 59-51-8, C5H11O2NS with the molecu-
H Enthalpy (kJ mol-1) lar mass of 149.21) is a kind of protein of containing amino
U Thermodynamic energy (kJ mol-1) acids, it helps to metabolize and decompose fats, and it is a
m Mass of the sample (mg or g) major source of sulfur in the body. In addition, it plays an
n Molar number of the gaseous substance (mol) important role in removing heavy metals (such as mercury)
R Gas constant, 8.314 J (mol K)-1 or the in the body. Its structure is shown in Fig. 1.
determination coefficient The chemistry synthesis research of methionine are by
DSC DSC signal (lV) making use of acrolein, aminolacfone, malonate and solid–
liquid phase transfer catalytic alkylation, and is focused
Subscript mainly on hydrolysis of 5-(2-methylethyl) hydantoin [1].
p Constant pressure Although methionine is widely used in food, medicine and
v Constant volume feed additive, industry is mainly through chemical syn-
w Water thesis of DL-methionine, some problems such as environ-
f Additional heat or formation heat mental pollution, difficult separation and purification,
s Sample several of its important thermodynamic data are scarce, and
std Standard substance the research on the thermal behavior and decomposition
b Baseline process has not been reported. Therefore, in this manu-
script, we examined these thermodynamics data of
methionine such as the relationship between the specific
& Cairong Zhou
heat capacity and temperature, and the constant volume
zhoucairong@zzu.edu.cn combustion energy of the pure substance. Then, the stan-
dard molar enthalpy of formation was calculated by ther-
1
School of Chemical Engineering and Energy, Zhengzhou modynamics principle. The study can not only provide
University, Zhengzhou, Henan, China

123

O bomb, g; DT is the change of water temperature in inner
S
H3C OH
NH2
Fig. 1 Molecular structure of methionine
basic data for methionine, but also are available for the
exploiting new synthesis method, engineering design and
industry production of methionine and its derivatives.
Experimental
Materials
The compound (CAS: 59-51-8) was purchased from
Sinopharm Chemical Reagent Co., Ltd, China. According
to the certificate, the substance was more than 0.990 in
purity, it did not been further purified; Benzoic acid (pu-
rity, [ 99.5%, commercially analytical pure); naphthalene
(purity, [ 99.8%, Shanghai chemical reagent, procure-
ment, supply station distribution); a-Al2O3(a-Al2O3 Power
for TG Standard Material, Japan Shimadzu Corporation).
Methods
Theoretical analysis of enthalpy of combustion
According to the laws of thermodynamics, when a sub-
stance burns completely, the constant volume combustion
enthalpy Qv is equal to variation of thermodynamic energy
DU (that is Qv = DU), the enthalpy of combustion at
constant pressure is Qp ¼ DH(enthalpy change). And the
relationship between them is expressed by Eq. (1) [2–5]:
DH ¼ Qp ¼ Qv þ DnRT ð1Þ
where n is the molar variation of gaseous substances before
and after the reaction; R is the universal gas constant; T is
the absolute temperature of the reaction. When the sample
is completely burned, the heat released increases the tem-
perature of both the calorimeter (oxygen bomb) and the
surrounding medium (water in this experiment), and mea-
sures the temperature change of water before and after
combustion, the constant volume combustion enthalpy of
the sample was obtained by Eq. (2) derived from the law of
conservation of energy.
mQv ¼ ð3200cw þ cÞDT þ Qf ð2Þ
where m is mass of the tested sample (g); 3200 is mass of
deionized water (at 25 C) in inner cylinder for an oxygen
123
Q. Niu et al.
cylinder before and after the combustion reaction, g; cw is
count as the specific heat capacity of water,
4.18 J g-1 K-1; c is the calorimeter’s thermal capacity,
J K-1; Qf is the additional heat produced by the air in the
oxygen bomb, which is 0 J under ideal conditions, and Qv
is a heat release of the tested sample at the constant volume
combustion, that is variation of thermodynamic energy.
Procedure for enthalpy of combustion
The determination of combustion heat has an important use
in industrial production [6, 7]. From Eq. (1), once given
heat of combustion Qv, the enthalpy of combustion DH can
be calculated out. The principle is simple, and a certain
amount of material sample is ignited in the oxygen bomb
through the ignition wire and completely burned, the heat
released by the combustion increases the ambient temper-
ature of the oxygen bomb, the combustion heat of the
sample to be measured was determined by measuring the
environmental temperature before and after combustion
[8]. The combustion heat of methionine was measured by
XRY-1C bomb calorimeter (Shanghai Changji Geological
Instrument Co., Ltd. China) from the difference in water
temperature between the sandwich water and the
calorimeter in this test. The temperature of the sandwich
water is close to the room temperature. The precision of
electronia balance (FA1004, Shanghai Precision & Scien-
tific Instrument Co., Ltd.) and microthermometer is,
respectively, 0.10 mg and ± 0.01 C.
The process is: (1) the powdery tested sample is
squeezed into a cylindrical flakes of 1.0 ± 0.1 g about
1 cm in diameter with a tablet press, then put the tablet into
the sample crucible, put 10 mL deionized water in the
oxygen bomb, and fill in excess oxygen to pressure up to
0.3–0.4 MPa before the bomb is sealed. It is important to
connect the ignition wire to the two electrode and make the
ignition wire form the point contact with the tested sample;
(2) fill the outer barrel with water, add 3200 g (25 C)
deionized water to the inner cylinder and fix the inner
cylinder, put oxygen bomb into inner cylinder and connect
ignition device; (3) after setting up the parameters of the
software panel to the temperature constant, click start and
begin to determine the combustion heat Qv. (4) After
temperature is constant, the blender is turn on. The metal
wire is ignited after 6 min, the sample starts combustion
when temperature is quickly raised. Temperature readings
are taken at 30-s intervals after the ignition. After tem-
perature reach at the most height point and continue
10 min, the test could be stopped automatically [9].
Investigation on standard molar enthalpy of combustion, specific heat capacity and thermal…

Theoretical analysis of specific heat capacity Results and discussion

When the specific heat capacity is measured by differential Investigation on the enthalpy of combustion
scanning calorimetry (DSC-60, Shimadzu Corporation,
Japan), the sample is under linear programmed temperature Determination of heat capacity of oxygen bomb
control, the heat flow rate into the sample is continuously calorimeter
measured, equal to the amount of heat absorbed by the
sample, there is a relationship between specific heat The constant volume combustion heat of naphthalene was
capacity and absorbed heat [10, 11] measured by XRY-1C-type oxygen bomb calorimeter to
dH 1 verify the reliability of the calorimeter for the determina-
Cp ¼  ð3Þ tion of combustion heat [13]. Benzoic acid was used to
dT m
determine the heat capacity of the oxygen bomb
where m is mass of the tested sample; Cp is the specific heat calorimeter. According to the literature, the constant vol-
capacity of the sample. In the actual measurement process, ume combustion heat of benzoic acid is 26,460 J g-1
due to the sample size and the limitations of the instrument, [10, 14–17]. The heat capacity of an oxygen bomb
it is difficult to accurately determine the absolute value of calorimeter(c) can be calculated by Eq. (2), the calculation
dH/dT, therefore, often used indirect measurement. First, results are shown in Table 1, and its average value is
place the empty crucible on the sample holder and refer- 2026 J K-1.
ence support to measure a baseline; then, the DSC curves
of both the standard substance and the sample were Determination of standard molar enthalpy of combustion
determined under the same conditions, respectively. The 4cHHm of methionine
specific heat capacity of the sample at any measured
temperature can be calculated by Eq. (4) [12]. The formula for complete combustion of methionine can be
mstd DSCs  DSCb written as following Eq. (5) [18, 19]
Cp ¼   Cp;std ð4Þ
ms DSCstd  DSCb 4C5 H11 O2 NSðsÞ þ 31O2 ðgÞ ¼ 20CO2 ðgÞ þ 22H2 OðlÞ
where Cp, Cp,std, are the specific heat capacities of the þ 2N2 ðgÞ þ 4SO2 ðgÞ
tested sample and the standard sample at the temperature T, ð5Þ
respectively, kJ kg-1 K-1; mstd, ms are mass of the stan-
According to Eq. (2), we can find that the formula for
dard and the tested samples, mg; DSCstd, DSCs are values
calculating the combustion heat of methionine at a constant
of the DSC signal about the standard and the measured
pressure is Eq. (6)
samples in the temperature T, lV; DSCb is the DSC signal
value of the baseline at the temperature T, lV. DH ¼ Qp ¼ Qv þ DnRT ¼ Qv  5RT ð6Þ
According to the laws of thermodynamics, the constant
Measuring steps of specific heat capacity volume combustion heat of a substance at a certain tem-
perature and the specific heat capacity of the substance at
DSC-60 was used to determine the specific heat capacity of
this temperature are known, the standard molar enthalpy of
methionine at a constant pressure, the scanning conditions
combustion at 25 C (298.15 K) can be calculated. If the
were as follows: aluminum reference tank, scan range from
experimental temperature was T K, the standard molar
373.15 to 453.15 K at constant heating rate of 5 C min-1,
combustion enthalpy (298.15 K) is calculated by Eq. (7) on
the flow rate of dynamic dry nitrogen gas was
the basis of Hess’s law [3–5]
40 mL min-1, amounts of the tested sample was about
2.5 ± 0.5 mg. Before the samples were analyzed, the Dc Hmh ð298:15 KÞ ¼ DHr þ Dc Hm ðTÞ þ DHf
DSC-60 was calibrated with indium (purity = 99.99%, ¼ DHr þ Qv  5RT þ DHf ð7Þ
Tm = 429.78 K, DmH = 28.45 J g-1) and zincum (pu- ZT X
rity = 99.99%, Tm = 419.58 K, DmH = 100.50 J g-1)  
DHr ¼ aj cp;j dT ð8Þ
(Japan Shimadzu Co.). Data acquisition and online pro- reactant
298:15
cessing were done with TA-60WS Collection Monitor
software. Z
298:15
X 
DHf ¼ bk cp;k dT ð9Þ
T product

123
 Q. Niu et al.

Table 1 Heat capacity of

Substance Quantity, m/g Temperature, DT/C (3200cw ? c)/J K-1 Thermal capacity, c/J K-1
oxygen bomb calorimeter at
298.15 K Benzoic acid 0.9754 1.392 15,462 2118
0.9821 1.973 15,278 1934
0.9763 1.683 15,370 2026
Average 15,370 2026

where Dc Hm h
and Dc Hm are the standard molar combustion a standard molar combustion enthalpy of substance. The
enthalpy (298.15 K) and the combustion enthalpy at the formation reaction of methionine can be written as fol-
experiment temperature (T K). DHr and DHf are the lowing Eq. (10)
enthalpy of the reactants and products. O2 ðgÞ þ 5CðgraphiteÞ þ 11=2H2 ðgÞ þ 1=2N2 ðgÞ
On the basis of the experiment data in Tables 1 and 2, þ SðrhombÞ
the standard molar combustion enthalpy of methionine is ¼ C5 H11 O2 NSðsÞ ð10Þ
calculated to be - 6661.03 kJ mol-1.
The products of the combustion reaction of methionine
The reliability of the instrument was tested by naphthalene;
are 5CO2(g) and 11/2H2O(l), according to the principle of
as a standard, the average value of standard molar combustion
thermodynamics, the standard molar enthalpy of formation
enthalpy of naphthalene is - 5165.80 kJ mol-1 in Table 2.
for methionine can be calculated by Eqs. (11) or (12) [16]
Compared with the document value (- 5153.90 kJ mol-1) 
[10], the relative error between the experimental value and the Df Hmh ¼  Dc Hmh ðC5 H11 O2 NS; sÞ  5Dc Hmh ðC,graphiteÞ
document value is 0.23% for naphthalene, and the absolute 
11=2Dc Hmh ðH2 ; gÞ
error is 11.9 kJ mol-1. Based on the result of naphthalene, the
ð11Þ
uncertainty of standard molar combustion enthalpy for

methionine can be estimated to be 0.23%. In the same way, the Df Hmh ¼  Dc Hmh ðC5 H11 O2 NS,sÞ  5Df Hmh ðCO2 ; g)
uncertainty of standard molar enthalpy of formation is the 
11=2Df Hmh ðH2 O; lÞ
same as that of standard molar combustion enthalpy.
ð12Þ
Determination of standard molar enthalpy of formation Df Hmh ðCO2 ; gÞ and Dc Hmh ðH2 O; lÞ are - 393.514,
h
Df Hm - 285.838 kJ mol-1, successively, Df Hmh ðO2 ; gÞ,
Df Hm ðN2 ; gÞ and Df Hm ðS; rhombÞ are 0 kJ mol-1 [20].
h h
The complete combustion of organic matters in oxygen The standard molar enthalpy of formation for methionine
atmosphere is easy, but it is difficult to achieve organic was calculated to be 3121.35 kJ mol-1.
substances through elemental direct synthesis. Therefore,
the standard molar formation enthalpy can be calculated by

Table 2 The standard molar combustion enthalpy of methionine at 298.15 K

Substance Quantity, m/g Temperature, DT/C Enthalpy of combustion, Qv/J g-1 4cHm/J g-1 4cHH
m /J g
-1
4cHH
m /kJ mol
-1

Methionine 0.9400 1.416 43,329.1 - 43,320.3 - 43,314.4 - 6462.94

0.9642 1.609 47,995.6 - 47,985.6 - 47,978.9 - 7158.93
0.9625 1.363 40,733.3 - 40,724.8 - 40,719.1 - 6075.70
0.9714 1.526 45,183.6 - 45,174.1 - 45,167.8 - 6739.49
0.9788 1.567 46,046.2 - 46,036.5 - 46,029.9 - 6868.12
Average - 44,648.3 - 44,642.0 - 6661.03
Naphthalene 0.9405 2.503 40,430.6 - 40,435.5 - 40,370.5 - 5166.15
1.0059 2.674 40,386.7 - 40,391.5 - 40,323.0 - 5168.20
0.9842 2.611 40,304.5 - 40,309.4 - 40,243.6 - 5158.02
0.8233 2.181 40,249.6 - 40,254.5 - 40,197.9 - 5152.16
0.7126 1.902 40,555.1 - 40,560.0 - 40,493.2 - 5190.01
0.6813 1.805 40,248.8 - 40,253.7 - 40,197.2 - 5152.08
Average - 40,367.4 - 40,304.3 - 5165.80

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Investigation on standard molar enthalpy of combustion, specific heat capacity and thermal…

Meanwhile, the thermal stability of methionine was

investigated by DTG-60 differential thermal gravimetric
Exo

apparatus. Figure 3 and Table 3 show a series of TG curves

of methionine at heating rates of 5, 10, 15, 20 and
25 C min-1 under a nitrogen atmosphere. From TG
Heat flow/mW Endo

curves, methionine displays one-stage decomposition pro-

cess among 480–715 K; the average percentage of mass
loss was 96.77%. The result that explains the process is an
incomplete thermal decomposition process and is consis-
tent with the decomposition temperature of 280 C
T f = 550.15 K
v h = 5 °C min–1 (553.15 K) reported in the literature [21]. Note that these
200 300 400 500 600 700 800
curves of the mass loss and the endothermic peaks in
thermal decomposition process appear a slight displace-
Temperature/K
ment along with the increase in heating rate b, meaning
Fig. 2 The DSC curve of methionine that the decomposition temperature is affected by the
heating rate b.
200% Compared with the DSC analysis, TG–DTA curves
reveal that the absorb heat of 974.34 kJ mol-1
Exo

150%
(6530 J g-1) at 550.51 K from DSC could be endothermic
amount of melting and decomposition of methionine dur-
1
2
3 4
5
ing heating process.
100%
Mass loss/%
Heat flow/mW Endo

Analysis of specific heat capacity

Tf
0 100 200
Temperature/K
Fig. 3 TG-DTA curves of methionine at different heating rates b: 1.
5 C min-1; 2. 10 C min-1; 3. 15 C min-1; 4. 20 C min-1; 5.
25 C min-1
Thermal stability analysis of methionine
The melting point of the sample can be determined by
DSC-60 differential scanning calorimeter. As can be seen
from Fig. 2, the absorb heat of methionine is
974.34 kJ mol-1 (6530 J g-1) at 550.51 K, and there is
only one endothermic peak.
50%
5
The specific heat capacity of methionine was measured in
the solid state by DSC-60 differential scanning calorimetry,
0%
with sample mass 2.0 ± 0.5 mg, and the temperature ran-
1 234 ges from room temperature to 450 C at the constant
–50% heating rate of 5 K min-1. Each sample was subjected to at
300 400 500
least 3 experiments, and its average was taken as the final
result. In order to determine the reliability of the instru-
ment, the specific heat capacities of benzoic acid and a-
Al2O3 were measured and compared with literature values
[4, 5].The experimental results are shown in Tables 4 and 5
[20]. The average relative deviation is defined as:
 
1 X Cpi  Cpi ;cal 
ARD ¼ ð13Þ
n Cpi
As shown in Tables 4 and 5, the average relative devi-
ations of the specific heat capacities of benzoic acid and a-
Al2O3 by DSC-60 are 0.38 and 0.35%, respectively, and
the absolute error of the specific heat capacities of benzoic

Table 3 TG-DTA basic data

Heating rate, b/C min-1 Initial temperature, Ti/K Finial temperature, Tf/K Peak temperature, Tp/K Mass loss/%

5 480.54 715.23 536.53 99.27

10 480.40 708.37 548.60 96.57
15 480.40 712.69 553.80 96.26
20 480.29 712.61 558.11 94.37
25 480.90 713.21 560.89 97.40
Average 480.51 712.42 551.59 96.77

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 Q. Niu et al.

Table 4 Experimental values and literature values of specific heat capacities for benzoic acid
Temperature/K Heat capacity in Heat capacity in experiment, Average relative Absolute error,
literature, Cp,lit/J g-1 K-1 Cp,exp/J g-1 K-1 deviation, ARD/% Ea/J g-1 K-1

310 1.2471 1.2461 0.08 0.0010

320 1.2852 1.2827 0.19 0.0025
330 1.3232 1.3263 0.23 0.0031
340 1.3611 1.3625 0.10 0.0014
350 1.3989 1.3882 0.77 0.0107
360 1.4372 1.4494 0.85 0.0122
370 1.4767 1.4718 0.33 0.0049
380 1.5169 1.5093 0.50 0.0076
Average 0.38 0.0054

Table 5 Experimental values and literature values of specific heat capacities for a-Al2O3
Temperature/K Heat capacity in literature, Heat capacity in experiment, Average relative Absolute error,
Cp,lit/J g-1 K-1 Cp,exp/J g-1 K-1 deviation, ARD/% Ea/J g-1 K-1

310 0.7994 0.8009 0.19 0.0015

320 0.8188 0.8205 0.21 0.0017
330 0.8372 0.8411 0.46 0.0039
340 0.8548 0.8598 0.59 0.0050
350 0.8713 0.8779 0.76 0.0066
360 0.8871 0.8880 0.10 0.0009
370 0.9020 0.9031 0.12 0.0011
380 0.9161 0.9173 0.13 0.0012
390 0.9295 0.9310 0.16 0.0015
400 0.9423 0.9441 0.19 0.0018
410 0.9544 0.9564 0.21 0.0020
420 0.9660 0.9683 0.24 0.0023
430 0.9770 0.9797 0.28 0.0027
450 0.9975 1.0010 0.35 0.0035
460 1.0070 1.0109 0.39 0.0039
470 1.0160 1.0208 0.47 0.0048
480 1.0247 1.0298 0.50 0.0051
530 1.0626 1.0722 0.90 0.0096
Average 0.35 0.0033

acid and a-Al2O3 by DSC-60 are 0.0054 and Conclusions

0.0033 J g-1 K-1, respectively. The specific heat capacity
of methionine at atmospheric pressure was measured, and
the result is shown in Fig. 4. The relationship between the
specific heat capacity and temperature could be gotten with
the least cube method at solid phase state and represented
by Eq. (14). The linear correlation coefficient (R2) of
Eq. (14) was 0.9944.
Cp ðmethionineÞ=kJðkgKÞ1 ¼0:0002T 2 0:162T
þ32:154ðR2 ¼0:9944Þ
ð14Þ
Using XRY-1C calorimeter, the standard molar combus-
tion enthalpy for methionine was determined to be
- 6661.03 kJ mol-1. The standard molar formation
enthalpies for methionine were determined to be
3121.35 kJ mol-1. The specific heat capacity of methion-
ine was determined using differential scanning calorimetry,
the relationship between the specific heat capacity of the
sample and temperature was obtained from 373.15 to
455.15 K. Using DTA-TG, the decomposition process of
methionine was one stage, the stage is mass loss with
accompanied by endothermic phenomenon so thermal

123
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