Thermodynamic Aspects of Freeze-Drying: A Case Study of an “Organic Solvent–Water” System
Full article
| Общее |
Language:
Английский,
Genre:
Full article,
Status:
Published,
Source type:
Original
|
| Journal |
Journal of Thermal Analysis and Calorimetry
ISSN: 1388-6150
, E-ISSN: 1572-8943
|
| Output data |
Year: 2017,
Volume: 127,
Number: 2,
Pages: 1593-1604
Pages count
: 12
DOI:
10.1007/s10973-016-6003-8
|
| Tags |
Cryotemperature SEM, DSC, Freeze-drying, Phase diagram, X-ray diffraction |
| Authors |
Ogienko A.G.
1,2
,
Drebushchak V.A.
2,3
,
Bogdanova E.G.
1,2
,
Yunoshev A.S.
2,4
,
Ogienko A.A.
5
,
Boldyreva E.V.
6
,
Manakov A.Y.
1,2
|
| Affiliations |
| 1 |
Nikolaev Institute of Inorganic Chemistry SB RAS,
Lavrentiev Ave. 3, Novosibirsk, Russia 630090
|
| 2 |
Novosibirsk State University, ul. Pirogova 2, Novosibirsk,
Russia 630090
|
| 3 |
Sobolev Institute of Geology and Mineralogy SB RAS,
Novosibirsk, Russia 630090
|
| 4 |
Lavrentiev Institute of Hydrodynamics SB RAS,
Novosibirsk, Russia 630090
|
| 5 |
Institute of Cytology and Genetics SB RAS, Novosibirsk,
Russia 630090
|
| 6 |
Institute of Solid State Chemistry and Mechanochemistry SB
RAS, ul. Kutateladze 18, Novosibirsk, Russia 630128
|
|
Funding (4)
|
1
|
The Ministry of Education and Science of the Russian Federation
|
СП-1144.2013.4
|
|
2
|
The Ministry of Education and Science of the Russian Federation
|
СП-680.2013.4
|
|
3
|
Federal Agency for Scientific Organizations
|
0301-2014-0002
|
|
4
|
Federal Agency for Scientific Organizations
|
0330-2016-0004 (АААА-А17-117122790027-1)
|
Aqueous solutions of glycine and tetrahydrofuran (THF) were frozen under variable conditions and subsequently annealed. The phases that resulted from this process were studied by X-ray diffraction, DSC and cryotemperature SEM. Under conditions achieved in common laboratory freeze-dryers, the THF clathrate hydrate of cubic structure II was formed in near-quantitative yields. The temperature–composition state diagram for the THF–water–β-glycine systems suggests that the critical temperature of the primary drying stage is the temperature of the four-phase peritectic reaction (269 K), and not the temperature of the congruent melting of the THF hydrate in the THF–water system (278 K). Freeze-drying is shown to go much faster if aqueous solutions are substituted for THF–water solutions. This finding is of great importance for practical applications, including pharmaceutical drug formulation.