The micro-solid phase extraction of haloacetic acids is a procedure that extracts haloacetic acids from aqueous solution using iron-modified rice husk silica as the stationary phase or sorbent. Rice husks provide an excellent source of silica. The sorbent is prepared by incinerating the husks to produce a powder that is treated with 1.0 M nitric acid for 24 hours to produce rice husk silica. The silica is washed with base, cetyltrimethylammonium bromide is added, and then titrated with a 10% Fe3+ solution to pH 5, which forms a gel. The gel is aged, filtered, dried, and calcined to produce a nitrate-free iron-modified rice husk sorbent. The sorbent is then packaged in porous, heat-sealed polypropylene membrane envelopes and used for extraction of HAAs from water. The HAA analytes are desorbed by ultrasonication in methanol for analysis and quantification.