CURRICULUM VITAE

Name : Dr. K. Chandran

Father’s name : Kannan

Date of birth : 13-02-1963

Nationality : Indian

Address for correspondence :

Office	Residence
K. Chandran Scientific Officer Materials Chemistry Division Chemistry Group Indira Gandhi Centre for Atomic Research Kalpakkam – 603 102 Tamil Nadu, India	K. Chandran No. 7, Shenbagam DAE Township Anupuram – 603 127 Thirukalikundram taluk Kancheepuram District Tamil Nadu, India

Telephone No. : 091-44-27482506 (Res.)

091-44-27480098 (Office)

Email id : kchand@igcar.gov.in

kchand63@yahoo.com

Education

2007 - Ph.D, (Industrial Chemistry), Alagappa University, Karaikudi, India

1995 - Post graduation: AIC (Analytical Chemistry), Institution of Chemists (India), Calcutta

1984 – Graduation: B.Sc (Chemistry) University of Madras, Chennai, India

· Ph.D work:

“Thermochemical studies on some sodium alkoxides of relevance to fast reactor technology” under the guideship of

Dr. V. Ganesan, Head, Materials Chemistry Division, Indira Gandhi Centre for Atomic Research, Kalpakkam, India,

Professional Employment

1985-1988 – Chemist, Petrochemical Industry, TEL, India

1988-1997 – Scientific Assistant, IGCAR, Kalpakkam, India

1997- till date – Scientific Officer, IGCAR, Kalpakkam, India

Area of Research

· Main area of research is sodium chemistry related to fast reactor technology. Research includes development of sodium sampling techniques and analytical techniques for metallic and non-metallic impurities measurement present in liquid sodium. Performance testing and calibration of in-house developed electrochemical sensors meant for online monitoring of non-metallic impurities such as oxygen, hydrogen and carbon present in dynamic sodium system. R & D includes testing of electrochemical hydrogen sensor response for sodium-steam and sodium-sodium hydroxide reactions.

· Development of radionuclide traps for fission products and activated corrosion products in liquid sodium system. Synthesis and characterization of radionuclide trap materials.

· Development of sodium cleaning techniques for sodium wetted components using aqueous and non-aqueous methods and their kinetic studies.

· Synthesis: Synthesized sodium alkoxides namely sodium methoxide, sodium ethoxide, sodium n-propoxide and sodium iso-propoxide in pure state in spite of their high reactivity to moisture.

· Characterisation:

Analytical techniques employed: X-ray diffraction, infrared spectroscope, atomic absorption spectroscope, combustion and thermal conductivity methods have been used extensively.

· Property Measurment: Enthalpies of solution of sodium and its alkoxides in various alcohols using solution calorimeter were carried out. Enthalpy of formation and reaction were calculated for the above sodium alkoxides. Heat capacities of sodium alkoxides were measured by DSC technique. Thermal stability and decomposition kinetic studies on sodium alkoxides were carried out by thermo-gravimetric technique coupled with mass spectrometer.

Member of professional body

Life member of Indian Association of Nuclear Chemists and Allied Scientists

Recent Publications

Journal

· Tensile behaviour and acoustic emission in zirconium alloys after thermal aging and sodium exposure

P.K Chaurasia, C.K. Mukhopadhyay, S. Murugan, P. Muralidaran, K. Chandran, V.Ganesan, T. Jayakumar, P.V. Kumar.

J. Nucl. Mater. 322 (2003), 217-227.

· Heat capacity measurements on sodium alkoxides

K. Chandran, R. Venkata Krishnan, A. Gopalan, K. Nagarajan, V. Ganesan

Thermochim. Acta 438 (2005) 107-111.

· Synthesis and characterization of sodium alkoxides

K Chandran, R Nithya, K Sankaran, A Gopalan, V Ganesan

Bull. Mater. Sci. 29 (2) (2006) 173-179.

· Kinetics of thermal decomposition of sodium methoxide and ethoxide.

K. Chandran, M. Kamruddin, P.K. Ajikumar, A. Gopalan, V. Ganesan

J. Nucl. Mater. 358 (2006) 111-128.

· Crystal Structure of Sodium Ethoxide

R. Nithya, K. Chandran, A. Gopalan, K. Sankaran Sastry, V. Ganesan (Accepted by ICDD).

· Crystal Structure of Sodium n-propoxide

R. Nithya, K. Chandran, A. Gopalan, K. Sankaran Sastry, V. Ganesan, (Accepted by ICDD).

· Standard molar enthalpies of formation of sodium alkoxides

K. Chandran, T.G. Srinivasan, A. Gopalan, V. Ganesan,

J. Chem.Thermodynamics 39 (2007) 449-454.

· Thermal decomposition and kinetic analysis of sodium propoxides

K. Chandran, M. Kamruddin, P.K. Ajikumar, A. Gopalan, V. Ganesan

J. Nucl. Mater. 374 (2008) 158-167

International Conferences

· Low-Density Carbon Foam as Radionuclide Trap Material

Prasanta Jana, K. Chandran, V. Ganesan

Int. Conf. on Advanced Materials (ICAM-2008), Feb 18-21, 2008, Kottayam,

pp222-223

National Conferences

· Preparation, characterization and measurement of solubility of sodium ethoxide in ethanol

K.Chandran, P. Muralidaran, V.Ganesan and G.Periaswami

Chemist meet 2002, December 7-8, 2002, Dept. of Chemistry, IIT, Madras.

· Preparation and characterization of alumina foam for radionuclides sorption studies

Prasanta Jana, K. Chandran, V. Ganesan

Annual Chemistry symposium and the first mid year meeting of the chemical research society of India. July 12-13, 2006. Dept. of Chemistry, IIT, Madras.

· Decomposition of sodium ethoxide: A matrix isolation study

K. Sankaran, K. Chandran, V. Ganesan, K.S. Viswanathan

Proc. Nuclear and Radiochemistry Symposium- NUCAR 2007, The Maharaja Sayajirao Uni. of Baroda, Vadodara, Feb. 14-17, 2007.

· Cesium trap developoment studies

Prasanta Jana, K. Chandran, V. Ganesan

12^th biennial symposium on Modern Trends in Inorganic Chemistry (MTIC-XII). Dec 6-8, 2007. Dept. of Chemistry, IIT, Madras.

· Thermal decomposition kinetics of sodium alkoxides - Model independent method

K. Chandran, M. Kamruddin, A. K. Tyagi, V. Ganesan,

Proc. Sixteenth National Symposium on Thermal Analysis (THERMANS 2008),

Feb 4-6, 2008, IGCAR, Kalpakkam. pp 254-256

· Carbon Foam – Synthesis, Characterisation and Thermal Stability Studies

 Prasanta Jana, K. Chandran, V. Ganesan,

Proc. Sixteenth National Symposium on Thermal Analysis (THERMANS 2008),

Feb 4-6, 2008, IGCAR, Kalpakkam. pp335-337

Reports

· Out-of-pile Testing for the Efficiency of Cesium Trap, Report No.: CG/2008/53

· Procedure for Sodium Sampling of In-Sodium Test facility (INSOT)

Report No. : FRTG / SFD - 99136, June 2007.

Ph.D synopsis

THERMOCHEMICAL STUDIES ON SOME

SODIUM ALKOXIDES OF RELEVANCE TO

FAST REACTOR TECHNOLOGY

SYNOPSIS OF THE THESIS SUBMITTED TO ALAGAPPA UNIVERSITY

IN FULFILMENT OF THE REQUIREMENTS FOR THE AWARD OF THE DEGREE OF DOCTOR OF PHILOSOPHY IN INDUSTRIAL CHEMISTRY

By

K. CHANDRAN

Dr. A. GOPALAN Prof., Ind. Chem. Dept. Alagappa University, Karakudi (Co-guide)

Dr. V. GANESAN Head, MCD, CG IGCAR, Kalpakkam (Guide)

INDUSTRIAL CHEMISTRY DEPARTMENT

ALAGAPPA UNIVERSITY

KARAIKUDI 603 003, INDIA

NOVEMBER 2006

Synopsis

THERMOCHEMICAL STUDIES ON SOME SODIUM ALKOXIDES OF RELEVANCE TO FAST REACTOR TECHNOLOGY

To meet the energy requirements of growing economy and considering the fast depletion of conventional sources of fossil fuels in India, alternate and sustainable energy resources are essential. Nuclear fuels are the promising suitable alternative sources of energy. Hence, India has launched nuclear energy programme in a big way to augment the electricity production.

The most important factor for the large scale development of fast reactors is the efficient breeding of new fissile material (²³⁹Pu and ²³³U) from their respective fertile materials ²³⁸U and ²³²Th. These fertile materials (²³⁸U and ²³²Th) are several hundred times more abundant than ²³⁵U and can be converted to fissile material by neutron absorption in a fast reactor. A breeder reactor is designed such that it generates more fissile materials from fertile material than the fissile material it consumes for energy production.

The core in fast reactors is compact compared to that of thermal reactors because of the absence of large amount of moderator and the heat energy produced is very high. It is necessary to have a coolant with excellent heat transfer characteristics and good chemical compatibility with fuel and structural materials to transport the large amount of heat generated in the core. Liquid metals have the most promising coolant characteristics because of their good heat transfer properties. Several coolants such as mercury, potassium and a eutectic mixture of sodium and potassium (NaK) etc have been considered. Among these, liquid sodium has emerged as the most suitable coolant for fast reactors because of its favorable physical, chemical and nuclear properties. In addition, cost consideration makes it a suitable coolant among the other liquid metals and alloys [1].

Components that are in physical contact with liquid sodium in the coolant circuits of Fast Breeder Reactors (FBRs) get wetted with a thin layer of sodium on prolonged exposure and high temperature operation of the reactor. During reactor maintenance, some of these components need to be replaced or maintained periodically. Exposure of such sodium wetted components to air would cause fire hazard and a possible hydrogen explosion as the reaction between sodium and moisture present in air is highly exothermic in nature producing hydrogen gas. In addition to posing problems related to fire hazard, this reaction also adversely affects the mechanical properties of the steel components due to the formation of sodium hydroxide. These problems could be tackled by using suitable solvent to dissolve out sodium under controlled conditions and avoiding residual sodium hydroxide on the component. Several techniques [2] are reported in the literature for removal of sodium. The highly reactive sodium metal can be converted into its less reactive or chemically inactive compound in either aqueous or non-aqueous conditions. Among the non-aqueous methods, several alcohols viz. methanol [3], ethanol [4], Jaysol SS [5], butyl cellosolve [6], ethyl carbitol [7, 8] etc., have been used world wide for sodium removal purposes.

However, there were reports of run-away reactions leading to accident when ethyl carbitol was used for cleaning residual sodium in storage tanks in France [7] and Germany [8]. Understanding the basic chemistry of the sodium-alcohol system would help in avoiding such accidental situations during sodium cleaning process. Measurements of thermochemical data such as enthalpy of formation, enthalpy of solution, heat capacity, thermal decomposition behaviour etc., of sodium alkoxides are useful in understanding sodium-alcohol reactions. The work reported in this thesis addresses the systematic procedure for the synthesis of sodium alkoxides and measurement of thermochemical properties of sodium-alcohol system of interest.

Results

Chapter 1 being an introduction part deals with the development of nuclear energy in India. The importance of fast reactor technology for the effective utilisation of available resources and the choice of suitable coolant for fast reactor, the properties of liquid sodium are discussed. The necessity of sodium cleaning of reactor components and the various methods adopted world wide for this purpose are described in detail in this chapter. The objective of the present work is also highlighted in this chapter.

The experimental facilities and techniques used in the present work are described in chapter 2. The different techniques used for characterisation of sodium alkoxides are the atomic absorption / emission spectrometry (AES), Infrared spectrometry (IR), X-ray diffractometry (XRD) and elemental analysis for carbon and hydrogen. Calorimetry, thermogravimetry and mass spectrometry techniques were also involved in the experimental studies. An inert (argon) atmosphere glove box was used for handling sodium and its alkoxides which are highly moisture sensitive. Enthalpy and heat capacity measurements were carried out using a solution calorimeter and a heat flux differential scanning calorimeter (DSC) respectively. To study the thermal decomposition of sodium alkoxides a thermogravimetric analyzer (TGA) was used. The gases evolved during thermal decomposition of sodium alkoxides were analysed using a quadrupole mass spectrometer (QMS).

Chapter 3 gives the results of synthesis and characterisation of sodium alkoxides, namely, sodium methoxide, sodium ethoxide, sodium n-propoxide and sodium iso-propoxide. The carbon and hydrogen contents of sodium alkoxides were estimated simultaneously by combustion and thermal conductivity method and the values are given in this chapter. The sodium content of sodium alkoxides were estimated by AES and the values are presented in this chapter. The values of sodium in these compounds as estimated by AES are in accordance with the theoretical values thus indicating high purity of these compounds. XRD patterns were collected for all the above mentioned sodium alkoxides. Crystal structure was deduced from XRD data for sodium methoxide, sodium ethoxide and sodium n-propoxide in this work. The lattice parameters ‘a’ and ‘c’ derived for sodium methoxide are 4.3404(12) and 7.412(4) Å, respectively, which are in agreement with the cell constants reported by Weiss [9, 10]. The lattice parameters for sodium ethoxide and sodium n-propoxide are not available in literature. The lattice parameter values of ‘a’ and ‘c’ viz. 4.4215(6), 9.088(24) and 4.3994(9), 12.166(21) Å, respectively are reported for the first time. The selected sodium alkoxides exhibit tetragonal structures with constant ‘a’ parameter while the unit cell is found to elongate along the ‘c’ direction with increase in carbon chain length. The IR spectral data of sodium methoxide and sodium ethoxide are consistent with the literature [11]. The IR spectral data of sodium n‑propoxide and iso-propoxide were reported for the first time.

Chapter 4 gives the details of the measurements of enthalpies of solution of sodium and sodium alkoxides in their respective alcohols. The molar enthalpies of solution of sodium _(Na/ROH) in methanol, ethanol and n-propanol are ‑203.95±1.30, –190.43±1.34 and –180.87±0.84 kJ mol^-1, respectively which are in close agreement with the values reported in literature [12]. Molar enthalpies of solution _(RONa/ROH) of sodium methoxide, sodium ethoxide and sodium n‑propoxide in their respective alcohols are –76.84±0.34, ‑54.84±0.39 and ‑41.90±0.66 kJ mol^-1, respectively. The enthalpy values for sodium methoxide and sodium ethoxide agree with those reported in NBS Table [13]. The molar enthalpy values of solution of sodium n‑propoxide in n-propanol are reported for the first time.

The enthalpies of formation of sodium alkoxides are deduced using the above data and the details of calculation of enthalpies of formation of sodium alkoxides are discussed. The molar enthalpies of formation _(RONa) of sodium methoxide, sodium ethoxide and sodium n-propoxide derived in the present work are ‑366.21±1.38, –413.39±1.45 and –441.57±01.18 kJ mol^-1, respectively. The values for sodium methoxide and sodium ethoxide deduced in this work are in close agreement with those reported by Leal [14] and in NBS Table [13]. The value of enthalpy of formation for sodium n-propoxide is reported for the first time.

The enthalpies of reaction of sodium with alcohols are calculated and the method of calculation is discussed in this chapter. The calculated values of  _(Na/ROH) are –127.11±1.34, –135.59±1.40 and –138.97±1.07 kJ mol^-1, respectively. The present values of enthalpies of reaction in sodium-methanol and sodium-ethanol systems are in close agreement with the values reported in NBS Table [13]. The enthalpy of reaction of sodium with n-propanol was calculated and reported for the first time.

A linear correlation has been found between enthalpies of formation of sodium alkoxides and that of alcohols, enabling the prediction of such data for higher sodium alkoxides when the kinetics of reaction pose difficulties in experimental determinations. The linear expressions are given in this chapter.

Heat capacity measured in the present work for sodium methoxide, sodium ethoxide, sodium n-propoxide and sodium iso-propoxide are given in Chapter 5. Measurements are made in the temperature range of 250-550 K. The C_{p,m 298} values are 65.05, 90.87, 113.52 and 121.20 J K^-1 mol^-1 respectively. The values of heat capacity were fitted in to a polynomial by least-squares method and are given in Table 1. From the heat capacity values, other thermodynamic functions such as enthalpy increments, entropies and Gibbs energy functions of these compounds are derived and reported. It is to be noted that the heat capacity values of sodium methoxide reported by Grenter and Westrum [15] in the temperature range of 10-350 K are the only data available in the literature. The heat capacity of sodium methoxide measured in the temperature range 250-550 K in the present study is 4-6 % less than that reported by Grenter and Westrum [15] in the temperature region 250-350 K. The heat capacity values for other sodium alkoxides are reported for the first time.

Table 1

Heat capacity of sodium alkoxides fitted in the form of polynomial in temperature range of 250–550 K

Compound	Cp, m (250–550 K) (J K^-1mol^-1)	standard error (J K^-1mol^-1)
Sodium methoxide	37.52 + 1.0002 ´ 10^-1T – 2.0311 ´ 10^5 T^-2	0.52 (1)
Sodium ethoxide	61.42 + 1.2247 ´ 10^-1T – 6.2744 ´ 10^5 T^-2	0.59 (2)
Sodium n-propoxide	60.04 + 1.9738 ´ 10^-1T – 4.7697 ´ 10^5 T^-2	0.76 (3)
Sodium iso-propoxide	48.69 + 2.4420 ´ 10^-1T – 2.6535 ´ 10^4 T^-2	0.83 (4)

The variation in DC_p,m as a function of temperature for addition of one –CH₂– group from sodium methoxide to sodium ethoxide and ethoxide to n-propoxide are computed and the correlation is shown in this chapter. It is inferred that DC_p,m for addition of one –CH₂– group can be considered to be same for both the alkoxides. Therefore, from this study the heat capacity values of higher alkoxides such as sodium n-butoxide, sodium n-pentoxide can be estimated.

Studies were made on thermal decomposition of the sodium alkoxides and the results are discussed in Chapter 6. Decomposition studies are investigated using thermogarvimetric analyzer coupled with mass spectrometer (TGA-MS) under non‑isothermal and isothermal conditions. Non-isothermal experiments are carried out at different linear heating rates (3, 5 and 10 K min^-1). In isothermal experiments, the sample was heated at a faster rate to a predetermined temperature close to decomposition temperature with a heating rate of 25 K min^-1 and held at that temperature till completion of decomposition.

The decomposition of sodium methoxide starts above 623 K. The gaseous products formed on decomposition are mainly methane (mass: 16) and minor quantities of ethane (mass: 30) and propylene (mass: 42). However, it is to be noted that Pfeifer et al. [16] have reported that the decomposition of sodium methoxide occurred in steps occurring at 393 and 413 K with ethylene, water and sodium oxide as decomposition products.

The decomposition of sodium ethoxide starts above 573 K which is in agreement with the report published by Blanchard et al. [17]. The gaseous products formed on decomposition are mainly methane (mass: 16) and ethylene (mass: 28) with minor quantities of ethane (mass: 30), propylene (mass: 42) and butylene (mass: 56).

The decomposition of sodium n-propoxide starts above 590 K. The rate of the decomposition is slow up to 625 K and beyond 625 K that decomposition took place at a faster rate. The gaseous products formed on decomposition are mainly propylene (mass: 42), and butylene (mass: 56) with minor quantities of methane (mass: 16), ethane (mass: 30) and very small quantity of ethylene (mass: 28).

The decomposition of sodium iso-propoxide starts at temperatures above 550 K. In this case too the decomposition is slower at the beginning and thereafter faster at the latter period. The gaseous products formed on decomposition are mainly methane (mass: 16), propylene (mass: 42) and butylene (mass: 56) with minor quantity of ethylene (mass: 28). Formation of methane is high when compared to other products, propylene and butylene.

The weight loss observed for the methoxide, ethoxide, n-propoxide and iso‑propoxide of sodium are 6, 24, 29 and 24 wt. %, respectively. The weight loss increases as carbon number increases in the carbon chain. This is due to the presence of an additional –CH₂– group. The formation of higher alkenes and alkanes on decomposition of higher alkoxides may also be due to the presence of additional ‑CH₂– group.

Various techniques such as XRD, IR, AES, elemental analysis and volumetric estimation were employed to characterise the residue after decomposition. The XRD pattern obtained for the residue in the present work is discussed in this chapter. All the peaks in XRD could be identified by comparison with the reported XRD pattern of sodium carbonate and sodium hydroxide [18, 19]. The IR spectra obtained for the decomposition residue of these sodium alkoxides and AR grade sodium carbonate are presented in this chapter. The IR spectral features of residues are in agreement with that of sodium carbonate reported in the literature [11], and gives confirmation that the residue is sodium carbonate. The probable mechanism and kinetics of decomposition of these sodium alkoxides are described in this chapter and are reported for the first time. The generalized decomposition reaction of sodium alkoxides can be represented as

RONa à m Na₂CO₃ + x C + 2m NaOH + y C_nH_2n+2 + z C_nH_2n (5)

where m, x, y, and z are constants. n is the number of carbon atoms present in the hydrocarbon. x = 1.5, 2, 4 and 5 in the case of methoxide, ethoxide, n-propoxide and iso-propoxide decomposition respectively; R= methyl, ethyl, n-propyl and iso-propyl group].

The activation energies derived from Arrhenius plots obtained from isothermal experiments are 187.81±11.22, 150.84±5.32, 151.45±2.16 and 128.07±3.44 kJ mol^-1 for sodium methoxide, sodium ethoxide, sodium n-propoxide and sodium iso‑propoxide respectively. These values are in close agreement with the values derived from non-isothermal method.

Chapter 7 gives the overall summary of the work and the conclusions. Thermochemical properties such as enthalpies of reaction, enthalpies of solution, enthalpies of formation, heat capacity and thermal decomposition behaviour of sodium alkoxides which are essential for the understanding of sodium-alcohol reaction have been studied and the results discussed.

Conclusions

The compounds, sodium methoxide, sodium ethoxide, sodium n-propoxide and sodium iso-propoxide which are extremely moisture sensitive were prepared in pure state. The sodium content as determined experimentally for these alkoxides is close to the theoretical value and high purity for these compounds is witnessed. Crystal structures deduced from XRD data are reported for the first time. IR spectrum of sodium n-propoxide and iso-propoxide are reported.

Enthalpies of formation and reaction of these alkoxides are estimated. The enthalpy of sodium n-propoxide and enthalpy of reaction of sodium with n-propanol are reported for the first time.

Heat capacities of these alkoxides are reported in the temperature range 250‑550 K. Other thermodynamic properties such as enthalpy increment, entropy and Gibbs energy function are also reported for the first time. From these measurements, heat capacity values of higher sodium alkoxides can be estimated.

In general, thermal decomposition of sodium alkoxides starts above 550 K. Saturated and unsaturated hydrocarbons are the gaseous products formed on decomposition of these alkoxides and solid residue consists of sodium carbonate, sodium hydroxide and free carbon. The activation energies of decomposition of sodium methoxide, sodium ethoxide, sodium n-propoxide and sodium iso-propoxide are 187.81±11.22, 150.84±5.32, 151.45±2.16 and 128.07±3.44 kJ mol^-1, respectively. The decomposition temperatures of the alkoxides are well above the boiling point of the respective alcohols and melting point of sodium (normally sodium cleaning is carried out below the melting point of sodium). Hence, this study has demonstrated that the lower molecular weight alcohols can safely be used for sodium cleaning purposes. Any unexpected temperature rise up to 550 K during sodium cleaning process, due to the exothermic reaction in an accidental condition, will not lead to thermal decomposition of the alkoxides. This ensures safety of the cleaning process.

References

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[2]	J.M. Lutton, R.P. Colburn F. Welch, Atomic Energy Review 18, 4 (1980) 815.
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[8]	J. Minges, W. Cherdron, W. Schutz, Short Report of an Accident During Sodium Cleanup with Ethyl Carbitol in a Storage Tank of a Research Facility, IAEA / IWGFR–Technical Committee Meeting on Sodium Removal and Disposal from LMFRs in Normal Operation and in the Frame Work of Decommissioning. 3-7 November, 1997, Aix-en-Provence, France. IWGFR‑98.
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[10]	JCPDS – International Centre for Diffraction Data. PDF-2 database 1999, File 19-1876.
[11]	J. Charles Pouchert, The Aldrich Library of Infrared Spectrum, 3^rd Edition, 1981, p 556.
[12]	M. D. Forcrand, M. Berthelot, Comptes Rendus 101 (1885) 318.
[13]	D.D. Wagman, W.H. Evans, V.B. Parker, R.H. Schumm, I. Halow, S.M. Bailey, K.L. Churney, R.L. Nuttall, The NBS Tables of Chemical Thermodynamics, J. Phys. Chem. Ref. Data, vol.11, Suppl.2, 1982.
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[16]	Pfeifer, Gyulac, Flora, Terez. Magyar Kemiai Folyoirat, 71 (8) (1965) 343.
[17]	J. M. Blanchard, J. Bousquet, P. Claudy, J.M. Letoffe J. Therm. Anal. 9 (1976) 191
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