The solid potassium L-threonate hydrate, K(C4H7O5)·H2O, was synthesized by the reaction of L-threonic acid with aqueous potassium hydrogen carbonate and characterized by means of chemical and elemental analyses...The solid potassium L-threonate hydrate, K(C4H7O5)·H2O, was synthesized by the reaction of L-threonic acid with aqueous potassium hydrogen carbonate and characterized by means of chemical and elemental analyses, IR and TG-DTG. Low-temperature heat capacity of K(C4H7O5)·H2O has been precisely measured with a small sample precise automated adiabatic calorimeter over the temperature range from 78 to 395 K. An obvious process of the dehydration occurred in the temperature region of 364-382 K. The peak temperature of the dehydration of the compound has been observed to be (380.524±0.093) K by means of the heat capacity measurements. The molar enthalpy, △dHm, and molar entropy, △dSm, of the dehydration of K(C4H7O5)·H2O were calculated to be (19.655 ± 0.012) kJ/mol and (51.618 ± 0.051) J/(K·mol) by the analysis of the heat-capacity curve. The experimental molar heat capacities of the solid from 78 to 362 K and from 382 to 395 K have been respectively fitted to two polynomial equations of heat capacities against the reduced temperatures by least square method. The constant-volume energy of combustion of the compound, △cUm, has been determined to be (- 1749.71 ±0.91) kJ·mol^-1 by an RBC-Ⅱ precision rotary-bomb combustion calorimeter at 298.15 K. The standard molar enthalpy of formation of the compound, △fHm , has been calculated to be (- 1292.56± 1.06) kJ·mol^-1 from the combination of the standard molar enthalpy of combustion of the compound with other auxiliary thermodynamic quantities.展开更多
New hydrated potassium hexaborate K2[B6O9(OH)2] has been synthesized under mild solvothermal conditions. The structure was determined by single-crystal X-ray diffraction and further characterized by FT-IR, Rarnan sp...New hydrated potassium hexaborate K2[B6O9(OH)2] has been synthesized under mild solvothermal conditions. The structure was determined by single-crystal X-ray diffraction and further characterized by FT-IR, Rarnan spectra and DTA-TG. It crystallizes in the monoclinic system with space group P21/n, a=0.9036(2) nm, b=0.66052(18) nm, c=1.5997(4) nm, β=91.862(4)°, V=0.9543(4) nm^3 and Z=4. Its crystal structure consists of K-O polyhedra and 1-D stepped polyborate chains constructed by new [B6O9(OH)2]2- fundamental building blocks. 1-D polyborate chains contain 3,8-membered boron rings. Adjacent chains are further linked via H-bonding interactions into 2-D layers. The K^+ cations reside not only between the layers but also in the 8-membered boron rings of the chains, compensating the negative charges of the borate chains and holding the layers together into the 3-D structure through bonding with oxygen atoms of the chains.展开更多
基金Project supported by the National Natural Science Foundation of China (No. 20171036), Education Committee of Shannxi Province (Nos. 01JK229, FF02328 and 2004B 10) and Postgraduate Foundation of China.
文摘The solid potassium L-threonate hydrate, K(C4H7O5)·H2O, was synthesized by the reaction of L-threonic acid with aqueous potassium hydrogen carbonate and characterized by means of chemical and elemental analyses, IR and TG-DTG. Low-temperature heat capacity of K(C4H7O5)·H2O has been precisely measured with a small sample precise automated adiabatic calorimeter over the temperature range from 78 to 395 K. An obvious process of the dehydration occurred in the temperature region of 364-382 K. The peak temperature of the dehydration of the compound has been observed to be (380.524±0.093) K by means of the heat capacity measurements. The molar enthalpy, △dHm, and molar entropy, △dSm, of the dehydration of K(C4H7O5)·H2O were calculated to be (19.655 ± 0.012) kJ/mol and (51.618 ± 0.051) J/(K·mol) by the analysis of the heat-capacity curve. The experimental molar heat capacities of the solid from 78 to 362 K and from 382 to 395 K have been respectively fitted to two polynomial equations of heat capacities against the reduced temperatures by least square method. The constant-volume energy of combustion of the compound, △cUm, has been determined to be (- 1749.71 ±0.91) kJ·mol^-1 by an RBC-Ⅱ precision rotary-bomb combustion calorimeter at 298.15 K. The standard molar enthalpy of formation of the compound, △fHm , has been calculated to be (- 1292.56± 1.06) kJ·mol^-1 from the combination of the standard molar enthalpy of combustion of the compound with other auxiliary thermodynamic quantities.
文摘New hydrated potassium hexaborate K2[B6O9(OH)2] has been synthesized under mild solvothermal conditions. The structure was determined by single-crystal X-ray diffraction and further characterized by FT-IR, Rarnan spectra and DTA-TG. It crystallizes in the monoclinic system with space group P21/n, a=0.9036(2) nm, b=0.66052(18) nm, c=1.5997(4) nm, β=91.862(4)°, V=0.9543(4) nm^3 and Z=4. Its crystal structure consists of K-O polyhedra and 1-D stepped polyborate chains constructed by new [B6O9(OH)2]2- fundamental building blocks. 1-D polyborate chains contain 3,8-membered boron rings. Adjacent chains are further linked via H-bonding interactions into 2-D layers. The K^+ cations reside not only between the layers but also in the 8-membered boron rings of the chains, compensating the negative charges of the borate chains and holding the layers together into the 3-D structure through bonding with oxygen atoms of the chains.