Extensive data are presented on the arsenic doping characteristics of Hg1−xCdxTe layers grown by metalorganic chemical vapor deposition using the dopant source tertiarybutylarsine (TBAs). The incorporation of arsenic in the layer is proportional to the II–VI alkyl ratio during TBAs injection. High arsenic concentrations significantly increase the layer dislocation density. Acceptor activation efficiency (taken to be the 77 K carrier concentration divided by the layer arsenic concentration) is ∼50% for a wide range of conditions, but decreases for arsenic concentrations approaching 1018cm−3. For arsenic concentrations below low‐1017cm−3, the 77 K carrier concentration is stable even for sample annealing at 400 °C on the Te‐rich side of the phase boundary. 77 K hole mobility strongly depends on compositionx. Variable temperature Hall effect measurements show that one layer exhibits the expected carrier freeze‐out with an ionization energy of 4.8 meV, but three other layers exhibit a much smaller degree of freeze‐out. Preliminary results using the dopant source triisopropylantimony are also presented.