Arsenic is among the heavy metals commonly found in aqueous environments. Iron oxide is known as an efficient adsorbent for the arsenic. A new synthetic method was applied to provide iron oxide giving a large specific surface area. The mixing method affects the formation of iron oxide. Ultrasonic waves assisted the formation of very fine iron oxide in an organic phase. The synthesized iron oxide is amorphous type with a high surface area of more than 181.3 m2/g. Sorption capacity of the synthesized adsorbent was relatively very high for arsenic and varied depending on the oxidation state of arsenic: a higher capacity was obtained with As(V). Lower solution pH provided a higher sorption capacity for As(V). The competitive effect of co-exist anions such as chloride, nitrate, and sulfate was minimal in sorption capacity of the iron oxide for arsenic.