Many laboratories routinely analyze plant, animal and soil samples with elemental analyzers coupled to isotope ratio mass spectrometers, obtaining rapid results for nitrogen (%N, d 15 N) and carbon (%C, d 13 C) from the same sample. The coupled N and C measurements are possible because of a gas chromatography (GC) separation of N 2 and CO 2 gases produced in elemental analysis. Adding a second GC column allows additional measurement of sulfur (%S, d 34 S) from the same sample, so that combined N, C and S information is obtained routinely. Samples are 1-15 mg, and replicates generally differ by less than 0.1% for d S. An example application shows that the N, C, and S measurement system allows a three-dimensional view of element dynamics in estuarine systems that are undergoing pollution inputs from upstream watersheds. Extension of these GC principles should allow coupled H, C, N, and S isotope measurements in future work. Copyright # 2007 John Wiley & Sons, Ltd.Measuring several parameters together from the same sample is desirable for many reasons, partly to save time, cost and sample, but also because the resulting coupled data allow a multivariate view of scientific problems. This paper describes a new advance in the field of coupled elemental and isotope analysis, adding S analyses to existing systems that already measure N and C amounts and isotopes in routine laboratory settings. Sulfur isotopes are valuable tracers in biogeochemical studies of element cycling on ecological and geological time scales, 1,2 complementing and expanding tracer information gained from N and C isotope measurements. 3 This paper focuses mostly on the added S analyses, and gives practical guidelines on how to make routine these new N, C and S (hereafter NCS) measurements. Laboratory analyses of sulfur are traditionally difficult and performed separately from nitrogen and carbon analyses. [4][5][6][7] Problems encountered with sulfur derive mostly from production of SO 2 gas in elemental analyzers, with SO 2 often reacting with surfaces and behaving in a 'sticky' fashion as it slowly desorbs and moves through combustion systems. Current NC analysis uses a combined elemental analyzer-isotope ratio mass spectrometer (EA-IRMS) system with one gas chromatography (GC) column to separate N 2 and CO 2 gases for sequential analysis. The new main feature of the system described here is use of a second GC column to separate SO 2 from N 2 and CO 2 gases. The N 2 and CO 2 gases pass through both GC columns for N then C measurements, while the SO 2 is only slowly moving through the first column. Upon completion of the N and C measurements, the second GC column is switched out of the gas-handling system, allowing flow rates to increase by twofold, rapidly eluting the SO 2 to the mass spectrometer for S measurements. The system described here complements a recent report of an analyzer capable of coupled H, C, N, and S (hereafter HCNS) measurements, 8 with the main difference that the system described here separates gases with GC and avoids usin...