In the present study the emphasis was given on two points, one is find out the effective extractants solvent and another is method of determination. Importance also was given on extraction ratio between solvent used as extractants and the amount used or dilution of the sample, shaking time and the incubation period on the basis of which after shaking how much time is required for settle down the solution just before titration/determination. The better result was obtained in 45 minutes to one hour after extraction was completed. Among three extractants, determination of elemental sulfur (ES), acetone can be used as an effective extractant for both S-rich fertilizer and soil sample (% recovery values obtained were 99.0 and 97.0% respectively). On the contrary, the % recoveries with toluene and xylene the values obtained from S-rich fertilizer and S-rich soils were 97.0 and 93.0 and 92.0 and 87.0% respectively. Determination was done with titrimetric method. Colorimetric always time consuming, values obtained with spectrophotometer is sometimes variable and expensive due to using of power supply. In titrimetric method where a high degree of accuracy and precision is not required. It is rapid and suitable for routine analysis in laboratories without using specialized equipment.