journal article·2025-10Open access

Intralaboratory calibration of the DSC shift-factor approach for melt viscosity determination: A case study on lead metasilicate glass

Danilo Di Genova, Gabriele Giuliani, Sumith Abeykoon, Kajal Dadwal, Suruchi Sharma, Atul Khanna, Alessio Zandonà, Dmitry Bondar, Stefanie Meyer, Laura Calabrò, Serena Dominijanni, Joachim Deubener

Abstract

The differential scanning calorimetry (DSC) shift-factor approach provides a powerful tool for determining the shear viscosity of glass-forming melts across several orders of magnitude. Its accuracy, however, depends on the proper determination of the shift factor ( K ) – a process of establishing K by linking DSC data to viscometry, herein termed 'intralaboratory calibration' – which then connects the fictive temperature to viscosity. In this study, we determine K for lead metasilicate (PbSiO 3 ) glass by integrating conventional DSC, flash DSC, and ball penetration viscometry measurements on samples obtained from the same batch. Raman spectroscopy was employed to verify sample integrity before and after measurements. Our results confirm the applicability of the DSC shift-factor approach, yielding shift factors of K onset = 10.92 ± 0.04, K peak = 9.41 ± 0.08, and K endset = 8.71 ± 0.07. These findings underscore the importance of intralaboratory calibration in refining the DSC-based method for accurate viscosity determination in glass-forming systems.
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OpenAlex topics: Material Dynamics and Properties · Cultural Heritage Materials Analysis · Glass properties and applications

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References (66)

Show source-provided references
1. High rate calorimetry derived viscosity of oxide melts prone to crystallization10.1016/j.jnoncrysol.2020.119992 ↗
2. Viscosity of metallic glass-forming liquids based on Zr by fast-scanning calorimetry10.1016/j.actamat.2021.117370 ↗
3. Kinetic fragility of pure TeO2 glass10.1016/j.jnoncrysol.2020.120595 ↗
4. Boson peak, heterogeneity and intermediate-range order in binary SiO2-Al2O3 glasses10.1038/s41598-018-23574-1 ↗
5. Formation of glasses from liquids and biopolymers10.1126/science.267.5206.1924 ↗
6. Recent progress in microcalorimetry10.1063/1.3051541 ↗
7. Elemental and cooperative diffusion in a liquid, supercooled liquid and glass resolved10.1063/1.4986507 ↗
8. Estimating the viscosity of volcanic melts from the vibrational properties of their parental glasses10.1038/s41598-021-92407-5 ↗
9. Anomalous variation of Boson peak and fragility and their correlations with intermediate-range structure in PbO-B2O3 glasses10.1016/j.jallcom.2017.04.168 ↗
10. Investigation of native oxide growth on zinc in different atmospheres by spectroscopic ellipsometry10.1002/pssa.201100542 ↗
11. Electronic structure and morphology of dark oxides on zinc generated by electrochemical treatment10.1039/C3CP44714F ↗
12. Viscosity of anhydrous and hydrous peridotite melts10.1016/j.chemgeo.2023.121440 ↗
13. Raman spectra of Martian glass analogues: a tool to approximate their chemical composition10.1002/2016JE005010 ↗
14. A chemical tipping point governing mobilization and eruption style of rhyolitic magma10.1038/nature24488 ↗
15. Unravelling the effect of nano-heterogeneity on the viscosity of silicate melts: implications for glass manufacturing and volcanic eruptions10.1016/j.jnoncrysol.2020.120248 ↗
16. A penetration viscometer
17. Medium-range structural order in covalent amorphous solids10.1038/354445a0 ↗
18. A review of the differential scanning calorimetry shift–factor approach: application to Colli Albani melt viscosity and implications for mafic plinian eruptions10.1016/j.jvolgeores.2025.108276 ↗
19. A multispectroscopic structural study of lead silicate glasses over an extended range of compositions10.1016/j.jnoncrysol.2009.12.003 ↗
20. The structure of lead silicate glasses determined by vibrational spectroscopy10.1007/BF00647770 ↗
21. Raman Spectra of glassy PbO–SiO2 system10.1143/JPSJ.36.917 ↗
22. Glass transition temperatures and crystallization kinetics of a synthetic, anhydrous, amorphous carbonate10.1098/rsta.2022.0356 ↗
23. Structure and properties of lead silicate glasses and melts10.1016/j.chemgeo.2017.03.030 ↗
24. Rheology of melts from the colli albani volcanic district (Italy): a case study
25. Viscosity and relaxation of glasses below the glass transition temperature
26. Is the structural relaxation of glasses controlled by equilibrium shear viscosity?10.1111/jace.17622 ↗
27. Flash-DSC provides valuable insights into glass relaxation and crystallization10.1016/j.jnoncrysol.2024.123242 ↗
28. Modelling the viscosity of anhydrous and hydrous volcanic melt10.1029/2021GC009918 ↗
29. The influence of pressure and composition on the viscocity of andesitic melts10.1016/S0016-7037(02)01139-0 ↗
30. The nature of boson peak in Raman scattering in glasses10.1016/0038-1098(86)90854-9 ↗
31. Viscosity of glass-forming liquids10.1073/pnas.0911705106 ↗
32. Raman spectroscopic studies of silicate and related glass structure: a review
33. Viskositäts-Temperaturverhalten des Standardglases I der DGG
34. Infrared and Raman spectra of lead fluorosilicate glasses10.1016/0022-3093(91)90507-3 ↗
35. Structural relaxation and the glass transition
36. Dependence of the fictive temperature of glass on cooling rate10.1111/j.1151-2916.1976.tb09376.x ↗
37. A model of structural relaxation in glass10.1111/j.1151-2916.1971.tb12186.x ↗
38. No title
39. Poisson’s ratio and the fragility of glass-forming liquids10.1038/nature02947 ↗
40. Rheology of nanocrystal-bearing andesite magma and its roles in explosive volcanism10.1038/s43247-022-00573-9 ↗
41. Effects of alkaline earth metal oxides, nickel oxide, and cobalt oxide on the viscosity of lead-metasilicate melts10.2320/jinstmet1952.43.7_625 ↗
42. Normal to abnormal behavior of PbSiO3 glass: a vibrational spectroscopy investigation under high-pressure10.1016/j.jnoncrysol.2022.121614 ↗
43. Cold- and hot-densification of a depolymerized glass: a multiscale vibrational investigation of PbSiO310.1016/j.jnoncrysol.2024.123246 ↗
44. Temperature effects on the structure of lead metasilicate glass, supercooled liquid, crystal, and liquid: vibrational anharmonicity and configurational transformations analyzed by molecular dynamics and Raman scattering10.1016/j.jnoncrysol.2024.122992 ↗
45. Chapter 9. Raman spectroscopy of silicate glasses and melts in geological systems
46. Raman scattering and molecular dynamics investigation of lead metasilicate glass and supercooled liquid structures10.1016/j.jnoncrysol.2018.07.048 ↗
47. Origin of the high-frequency doublet in the vibrational spectrum of vitreous SiO210.1126/science.275.5308.1925 ↗
48. Determination of cooling rates of glasses over four orders of magnitude10.1007/s00410-022-01899-5 ↗
49. A chemical threshold controls nanocrystallization and degassing behaviour in basalt magmas10.1038/s43247-022-00615-2 ↗
50. Correction of thermal inertia on scanning calorimetry10.1016/j.tca.2025.180062 ↗
51. The kinetics of the glass transition of silicate glass measured by fast scanning calorimetry10.1016/j.tca.2019.01.001 ↗
52. Use of the Adam-Gibbs equation in the analysis of structural relaxation10.1111/j.1151-2916.1984.tb19643.x ↗
53. Raman-scattering selection-rule breaking and the density of states in amorphous materials10.1103/PhysRevLett.25.222 ↗
54. Synthesis of PbO·SiO2 glass by CO2 laser melting method10.1016/j.jnoncrysol.2019.119572 ↗
55. Raman spectroscopy study of high B2O3 content lead fluoroborate glasses10.1002/(SICI)1097-4555(199907)30:7<525::AID-JRS412>3.0.CO;2-O ↗
56. Review on grain size effects on thermal conductivity in ZnO thermoelectric materials10.1039/D1RA06133J ↗
57. Relation between inelastic deformability and thermal expansion of glass in its annealing range10.1111/j.1151-2916.1946.tb11592.x ↗
58. Are volcanic melts less viscous than we thought? The case of Stromboli basalt10.1007/s00410-023-02024-w ↗
59. Nanoscale chemical heterogeneities control magma viscosity and failure
60. Raman spectroscopic investigation of evaporated PbO layers10.1016/j.tsf.2005.02.010 ↗
61. Vibrational spectroscopic studies of some lead silicate glasses10.1016/0022-3093(78)90150-3 ↗
62. Characteristic temperatures of enthalpy relaxation in glass10.1016/j.jnoncrysol.2006.11.027 ↗
63. Fictive temperature, cooling rate, and viscosity of glasses10.1063/1.1689951 ↗
64. DSC and Raman studies of lead borate and lead silicate glasses10.1016/0022-3093(93)90470-I ↗
65. Non-stoichiometric crystal nucleation in a spodumene glass containing TiO2 as seed former: effects on the viscosity of the residual melt10.1016/j.jnoncrysol.2023.122563 ↗
66. Reconciling calorimetric and kinetic fragilities of glass-forming liquids10.1016/j.jnoncrysol.2016.11.014 ↗