Design and evaluation of a liquid chromatographic column oven with adaptive and precise temperature control

doi:10.3724/SP.J.1123.2023.11021

Abstract

Abstract:

High performance liquid chromatography (HPLC) is a key analytical technique that is used in a number of fields. Improving the separation efficiency, stability, and universality of HPLC has been a continuing analytical-chemistry focus. In chromatographic separation, factors such as the composition and ratio of the mobile phase, the type of stationary phase, and the dimensions of the chromatographic column significantly affect the separation efficiency. In addition, the temperatures of the chromatographic column and mobile phase are also important for achieving separation. The column oven is usually used to stably control the column temperature in the HPLC separation system. Indeed, highly accurate temperature control ensures superior separation performance, short analysis times, and repeatability. In this study, we innovatively improved the traditional column oven by combining a variety of temperature-control algorithms to deliver continuous and highly accurate temperature control in the wide 4-90 ℃ range, and by exploring a new chromatographic-method development route. Instead of focusing on the complex hardware system, we optimized the software to achieve highly stable and accurate (±0.1 ℃) temperature control. Temperature-control performance was further improved by optimizing the structure of the thermal insulation and employing reliable and environmentally friendly thermal-insulation materials. Additionally, the thermal conduction of the heat-source device is discussed based on the heat-transfer principle with the aim of improving the performance of the column oven. The improved column oven delivered significantly enhanced chromatographic-separation repeatability and stability thereby reliably guaranteeing the development of highly efficient chromatographic analysis methods.

Key words: precise temperature control, algorithm, heat transfer principle, liquid chromatography, column oven

CLC Number:

O658

REN Xingfa, SHAO Fengwei, WU Yong, LIAO Xinming, WANG Zhuo, ZHOU Linjuan, HE Xuhong, ZHANG Weibing. Design and evaluation of a liquid chromatographic column oven with adaptive and precise temperature control[J]. Chinese Journal of Chromatography, 2025, 43(2): 177-184.

Figures/Tables 9

References

[1]	Moldoveanu S C, David V. Essentials in Modern HPLC Separations. Netherlands: Elsevier, 2022: 109
[2]	Liu Z J, Zhao M, Xu F. Chemical Analysis and Meterage, 2008, 17(4): 14
[2]	刘志娟, 赵敏, 许峰. 化学分析计量, 2008, 17(4): 14
[3]	Yang Y. Anal Chim Acta, 2006, 558(1/2): 7
[4]	Guillarme D, Heinisch S, Rocca J L. J Chromatogr A, 2004, 1052(1/2): 39
[5]	Kaczmarski K, Chutkowski M. J Chromatogr A, 2021, 1655: 462509
[6]	An X, Hayat A, Lee J W, et al. J Chromatogr A, 2022, 1665: 462831
[7]	Baba P A, Gettar R T, Magallanes J F, et al. J Chromatogr A, 2007, 1157(1/2): 227
[8]	Kadlecová Z, Kalikova K, Tesarova E, et al. J Chromatogr A, 2022, 1681: 463473
[9]	Losacco G L, Fekete S, Veuthey J L, et al. Anal Chim Acta, 2020, 1134: 84
[10]	Ortak H Y, Demiralay E C. J Pharm Biomed Anal, 2019, 164: 706
[11]	Xing Z F, Cheng H D, Zhang W B. Chemical Engineer, 2008, 157(10): 26
[11]	邢占芬, 成洪达, 张维冰. 化学工程师, 2008, 157(10): 26
[12]	Maisuradze M, Sheklashvilii G, Chokheli A, et al. J Chromatogr A, 2019, 1602: 228
[13]	Coym J W, Roe B W. J Chromatogr A, 2007, 1154(1/2): 182
[14]	Rogeberg M, Wilson S R, Malerod H, et al. J Chromatogr A, 2011, 1218(41): 7281
[15]	Liu G H. Natural Gas Chemical Industry, 2000, 25(6): 46
[15]	刘光会,. 天然气化工, 2000, 25(6): 46
[16]	Zhu S S, Zou P, Lu M N, et al. Infrared Technology, 2017, 39(11): 990
[16]	朱双双, 邹鹏, 路美娜, 等. 红外技术, 2017, 39(11): 990
[17]	Liu H, Fang Y, Su X, et al. Instrum Sci Technol, 2023, 51(2): 109
[18]	Hu K, Li S C, Lu Y H, et al. Mechanical & Electrical Engineering Technology, 2023, 52(4): 90
[18]	胡昆, 李思超, 鲁元昊. 机电工程技术, 2023, 52(4): 90
[19]	Wang Q H, Zhou J, Hou J C. Journal of Northwest A&F University (Natural Science Edition), 2023, 51(11): 144
[19]	王庆华, 周晶, 侯俊才. 西北农林科技大学学报(自然科学版), 2023, 51(11): 144
[20]	Tian L, Zhang B. Electronic Measurement Technology, 2006, 5(4): 197
[20]	田里, 张波. 电子测量技术, 2006, 5(4): 197
[21]	GB/T26792-2019

Application scenario	Room temperature condition	Temperature difference	Instruction
Target temperature>cavity temperature	relatively stable	large	fast heating➝slow heating
	relatively stable	small	slow heating
	slowly rising	large	slow heating
	slowly declining	small	slow heating
Target temperature<cavity temperature	relatively stable	large	fast cooling➝slow cooling
	relatively stable	small	slow cooling
	slowly rising	large	fast cooling→slow cooling
	slowly declining	little	slow cooling
Target temperature≈cavity temperature	relatively stable	minimal	quick switching between
≈room temperature			heating and cooling

Application scenario	Room temperature condition	Temperature difference	Instruction
Target temperature>cavity temperature	relatively stable	large	fast heating➝slow heating
	relatively stable	small	slow heating
	slowly rising	large	slow heating
	slowly declining	small	slow heating
Target temperature<cavity temperature	relatively stable	large	fast cooling➝slow cooling
	relatively stable	small	slow cooling
	slowly rising	large	fast cooling→slow cooling
	slowly declining	little	slow cooling
Target temperature≈cavity temperature	relatively stable	minimal	quick switching between
≈room temperature			heating and cooling

Condition	Operation	Algorithms
A<B	normal heating	heating PID algorithm and dual Peltier following algorithm
A≥B≥D	finely tuned heating	extreme PWM algorithm
B<C	normal cooling	cooling PID algorithm and dual Peltier following algorithm
C≤B≤D	finely tuned cooling	extreme PWM algorithm

Condition	Operation	Algorithms
A<B	normal heating	heating PID algorithm and dual Peltier following algorithm
A≥B≥D	finely tuned heating	extreme PWM algorithm
B<C	normal cooling	cooling PID algorithm and dual Peltier following algorithm
C≤B≤D	finely tuned cooling	extreme PWM algorithm