Abstract
Electroanalytical sensors for point-of-care biomedical or point-of-use environmental sample analysis are gaining popularity due to low limits of detection, ease of miniaturization, convenience, and ability to work with small sample volumes. Since pH must be tightly controlled for optimum electrochemical performance, adjustment of pH in these samples is often a necessity. Yet manual titration is time-consuming and can be especially challenging for small volumes. End point determination can also be difficult. Current commercial automatic pH titrators are generally designed for large volume (>1 mL) batch titrations, while the existing microvolume titrators are semiautomatic at best, still relying on multiple manual steps. To address the gap, we developed an automatic microtitration system suitable for small volume samples. The system was validated using digested whole blood microsamples, successfully demonstrating accurate and rapid pH adjustment for samples as small as 100 μL. The simple modular construction of the system makes it compatible with acid washing for trace metal detection and other cleaning or sample preparation steps. The electrochemical detection of manganese heavy metal in blood at the parts per billion level showed no detectable contamination induced by the system. Ultimately, our simple, accurate, user-friendly automatic microtitration system can be used in the pH adjustment of microvolume samples and can potentially be extended to other pH end point analysis.