Rapid, Accurate, and Reagent-Free Determination of Chlorine Concentration in Glass by Femtosecond LA-ICP-MS/MS with a Scanning Galvo Mirror System Using Hydrogen as Reaction Gas

Abstract

Determining halogen concentrations in inorganic materials is becoming increasingly important to satisfy environmental regulations. However, quantifying chlorine using laser ablation-inductively coupled plasma mass spectrometry (LA-ICP-MS) is challenging, despite the merits of this method. We propose a method for determining the chlorine concentration in glass using femtosecond LA with a scanning galvo mirror system, coupled with tandem ICP-MS (ICP-MS/MS). Hydrogen was introduced into the collision–reaction cell to eliminate mass spectral interferences (quadrupole 1: 35Cl+ (m/z 35) → quadrupole 3: 35ClHH+ (m/z 37)). A 1 × 1 mm2 ablation area was used to minimize sample heterogeneity. Using the proposed method with standard reference materials (SRMs) 610, 612, 614, and 616 (National Institute of Standards and Technology) as calibration samples, we determined the chlorine concentration in BAM-S005-A, a standard glass reference material with a composition similar to that of the SRM 61x series. The determined value of 244 ± 4.5 μg·g–1 (n = 6, average ± 95% confidence interval) is in excellent agreement with the certified concentration (247 ± 33 μg·g–1), demonstrating the high accuracy and low uncertainty of the method. The proposed method enables rapid analysis (within 10 min), and does not require harmful reagents or complicated pre-treatment. This approach can be readily extended to other materials, supporting safer, faster, and more reliable halogen analysis across research and industry settings.