Liquid wastes from the bioethanol industry bottom rest of the distillation process known as vinasse. High COD content of the vinasse more appropriately treated by the anaerobic process which produce biogas. Anaerobic waste treatment processes produce biogas consisting of methane (CH4) and carbon dioxide (CO2). This research aims to study the influence of fermentation method, feed composition, variations in the initial pH of fermentation 6, 7, and 8, and feed dilution in 1:0, 1:1, 1:2, 1:3, 1:4, 1:5 (Total Solid (TS) 27.865%, 13.93%, 9.288%, 6.96%, 5.573%, 4.64%). Sources of bacteria used is cow rumen fluid and urea as a nutrient. Batch fermentation process is done by measurement of gas every two days using water displacement technique up to gas had not formed. The results of research showed that the methods of without controlling pH on the composition of vinase rumen urea and initial pH 7is the best variable to the total biogas production of 635 ml (8:49 ml biogas / gr COD). The variable dilution feed for diversify TS show that highest biogas production is between the ratio of 1:4 (5.573% TS) and 1:5 (TS 4.64%) in amount of 27.22 to 30.17 mL/g TS.