In the determination of arsenic, attention has recently focused on the speciation of As(III) and As(V). Reversed-phase HPLC can be used to efficiently separate these two arsenic species. When inductively coupled plasma mass spectrometry is used for arsenic detection, an isobaric interference at m/z 75 is caused by the presence of chloride in the sample. These experiments describe the use of hydride generation in conjunction with a polypropylene-membrane gas-liquid separator to completely eliminate the transport of chloride to the plasma. A detection limit of 0.46 ppb for As(III) was achieved with this system. The chromatographic resolution of the system was not compromised by the addition of the gas-liquid separator. A determination of the arsenic content of a NIST urine sample was performed to demonstrate the effectiveness of the chloride elimination.