Automation and optimization of multidimensional microcolumn size exclusion chromatography-liquid chromatography for the analysis of photocrosslinkers in Cyclotene 4000 series advanced electronic resins

Abstract

Multidimensional chromatography using on‐line, coupled, micro‐column size exclusion chromatography and reversed‐phase high performance liquid chromatography, has been successfully implemented for the quantitative determination of photoinitiator concentrations in photosensitive, interlayer dielectric resin formulations. The actual formulation consists of the prepolymer, aromatic solvent, antioxidant, and a variety of bis‐azide photocrosslinkers. This paper describes the development of an automated system for Micro SEC‐LC, as well as accuracy and precision data for the photoinitiator analysis. The technology is very effective for the analysis of small molecules (e.g. additives) in polymer products, and as such can have wide ranging applicability to other polymer and complex products. The use of microcolumns in the first dimension allows the introduction of the complete fraction containing the components of interest into a reversed‐phase second dimension without deterioration of the separation when using a very strong mobile phase such as THF.

Band broadening in size-exclusion chromatography of polydisperse samples

“…Especially the (off-line) coupling with MALDI is expected to have a great impact on the practice of SEC [8]. Unlike other forms of LC, miniaturization has attracted only marginal interest [9]. In contrast, fast separations by SEC have drawn a great deal of interest in the last few years [10][11][12].…”

Toward microfluidic continuous-flow and intelligent downstream processing of biopharmaceuticals

“…The SEC also can benefit from the discussed methodology by automating the analysis of elution profiles. 155 When purifying protein aggregates or viral vectors, the system can identify peak positions and shapes, facilitating the detection of impurities or changes in the product's quality. If anomalies are detected, the AI system can take corrective actions, such as modifying column temperature or flow rate to improve separation or purity.…”

Contactless conductivity detection of synthetic polymers in non-aqueous size-exclusion electrokinetic chromatography

“…While in the last decade the use of miniaturized liquid chromatography (LC) systems in (bio)chemical and pharmaceutical analysis increased radically, in the field of polymer analysis only a limited number of research groups is working on miniaturized separation systems such as sizeexclusion chromatography (SEC) with microbore or capillary columns [1][2][3][4][5], or size-exclusion electrochromatography [6,7]. In polymer analysis the smaller sample volume is an issue only in exceptional cases [8].…”

“…In polymer analysis the smaller sample volume is an issue only in exceptional cases [8]. Hyphenation with mass spectrometry [2,3] or with another separation technique in a multidimensional system [4] is a more important argument for miniaturization.…”