Investigated empirically through post mortem item-examinee sampling were the relative merits of two alternative procedures for allocating items to subtests in multiple matrix sampling and the feasibility of using the jackknife in approximating standard errors of estimate. The results indicate clearly that a partially balanced incomplete block design is preferable to random sampling in allocating items to subtests. The jackknife was found to better approximate standard errors of estimate in the latter item allocation procedure than in the former. These and other results are discussed in detail. (Author)