Reliable purity assay of highly hygroscopic trichloroacetic acid for the development of high-purity reference material of NMIJ CRM 4074-a.

Trichloroacetic acid is known as one of the harmful disinfection byproducts with chlorine of tap water and is regulated according to legally binding standards in Japanese Drinking Water Quality Standards. We developed a high-purity trichloroacetic acid reference material, NMIJ CRM 4074-a, with certified purity as a traceability source of standard solution supplied under the Japan Calibration Service System (JCSS). As trichloroacetic acid is hygroscopic, water could be the main impurity. Although all impurities in the sample can be possibly detected by the freezing point depression method (FPD), it was unclear for trichloroacetic acid whether water was detected by FPD owing to evaporation of water from the sample during fusion. Therefore, we confirmed that water in trichloroacetic acid was detected as an impurity by FPD. The procedure was validated from an increment of purity by FPD due to reduction of water content and an agreement of purity by FPD with those by neutralization titrimetry (NT) and mass balance approach (MBA), both methods were based on different measurement principles from FPD. The certified value was determined to be (0.999 ± 0.003) kg kg-1 from the purity assay by FPD and NT, and uncertainties due to the homogeneity and stability of the CRM were included in the expanded uncertainty. The reliability of the certified value was verified by the agreement of purities by FPD, NT, and MBA.