A trace quantitative analysis of barbiturates has been carried out in blood, urine, organs and in gastric and intestinal concents. The amount of sample required for analysis is very small [approximately 400 mul blood]. Extraction is carried out four times with the mixture of acetone and either 1:1]. The preparation of columns, packing and standards has been described. The device used for the analyses [Chrom 3] is furnished with an adjusted feeding block preventing the decomposition of samples in the doser. The column temperature is 190 degrees C, the column packing is Chromaton N-AW-DMCS coated with 3% NPGS and 0.75% trimer acid, detector FID.