The purpose of this study was to determine the diurnal composition and concentration of volatile fatty acids (VFA) and to determine VFA composition and concentration differences between stomach compartment 1 (C1) and caecum of alpacas fed grass and alfalfa hay. The study was divided into two experiments. In Experiment 1 (EXP 1), 10 male alpacas (3+ years old, 65 kg BW) were divided into two groups, housed in drylot pens, provided ad libitum water and fed alfalfa (AH) or grass hay (GH) for 30 days. The alpacas were slaughtered and the digestive tract collected, divided into sub-tract sections, weighed and digesta sampled for pH, dry matter (DM) and NDF. Volatile fatty acid composition and concentration were determined on C1 and caecal material. Four adult male (3+ years old, 60 kg BW), C1 fistulated alpacas were housed in metabolism crates and divided into two forage groups for Experiment 2 (EXP 2). Alpacas were fed the forages as in EXP 1. Diurnal C1 VFA samples were drawn at 1, 3, 6, 9, 12, 18 and 24 h post-feeding. There were no differences between forages for tract weight, C1 and caecum digesta DM or NDF. Differences were noted (p < 0.05) for pH between forages and sub-tract site. Volatile fatty acids concentrations were different (p < 0.05) for forage and site, and total VFA was higher for AH than GH (110.6 and 79.1 mm) and C1 than caecum (40.7 and 27.6 mm). Proportion of VFA was significant (p < 0.05) for forage and site, C1 acetate highest for GH (84.8 vs. 74.0 mm) and caecum acetate 83.7 and 76.2 mm for GH and AH respectively. These data demonstrate the level of VFA produced in C1 and the caecum of alpacas and the diurnal VFA patterns. Composition of VFA is similar to other ruminant species.