AbstractA novel, fast and reliable sample preparation procedure for the simultaneous separation of Sr, Pb, and Nd has been developed for subsequent isotope ratio analysis of sediment digests. The method applying a fully automated, low-pressure chromatographic system separates all three analytes in a single-stage extraction step using self-packed columns filled with DGA Resin. The fully automated set-up allows the unattended processing of three isotopic systems from one sediment digest every 2 h, offering high sample throughput of up to 12 samples per day and reducing substantially laboratory manpower as compared to conventional manual methods. The developed separation method was validated using the marine sediment GBW-07313 as matrix-matched certified reference material and combines quantitative recoveries (>90% for Sr, >93% for Pb, and >91% for Nd) with low procedural blank levels following the sample separation (0.07 μg L-1 Sr, 0.03 μg L-1 Pb, and 0.57 μg L-1 Nd). The average δ values for Sr, Pb, and Nd of the separated reference standards were within the certified ranges (δ (87Sr/86Sr)NIST SRM 987 of -0.05(28) ‰, δ(208Pb/206Pb)NIST SRM 981 of -0.21(14) ‰, and δ(143Nd/144Nd)JNdi-1 of 0.00(7) ‰). The DGA Resin proved to be reusable for the separation of >10 sediment digests with no significant carry-over or memory effects, as well as no significant on-column fractionation of Sr, Pb, and Nd isotope ratios. Additional spike experiments of NIST SRM 987 with Pb, NIST SRM 981 with Sr, and JNdi-1 with Ce revealed no significant impact on the measured isotopic ratios, caused by potential small analyte peak overlaps during the separation of Sr and Pb, as well as Ce and Nd.