In this study, zirconia containing refractory samples were decomposed by dilute nitric acid. The chloride ion content in the leaching solution was determined by thiocyanate spectrophotometry. The influences of the leaching method of the sample pretreatment and the coloration condition of the solution to be tested on the test results were studied. The precision test was carried out and the results were compared with those determined by ion chromatography. The results showed that the zirconia containing refractories were boiled with dilute nitric acid to obtain the test solution. The influence of zirconium hydrolysis on determination was removed by centrifugation. The chlorine contents in zirconia containing refractories determined by spectrophotometry have low relative standard deviation (RSD), showing slight testing difference with those determined by ion chromatograghy.