Determination of the δ34S of low-concentration sulfate in water; RSIL lab code 1949

Techniques and Methods 10-C8

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The purpose of the Reston Stable Isotope Laboratory (RSIL) lab code 1949 is to determine the δ(34S/32S), abbreviated as δ34S, of dissolved sulfate having a concentration less than 20 milligrams per liter. Dissolved sulfate is collected on an anion-exchange resin in the field, eluted in the laboratory with 3 M KCl, and precipitated with BaCl2 at pH 3 to 4 as BaSO4. The precipitated BaSO4 is filtered and dried before introduction into an elemental analyzer (EA) Carlo Erba NC 2500. The EA is used to convert sulfur in a BaSO4 solid sample into SO2 gas, and the EA is connected to a continuous flow isotope-ratio mass spectrometer (CF-IRMS), which determines differences in the isotope-amount ratios of stable sulfur isotopes (34S/32S) of the product SO2 gas. The combustion is quantitative; no isotopic fractionation is involved. Samples are placed in a tin capsule and loaded into the Costech Zero Blank Autosampler of the EA. Under computer control, samples are dropped into a heated reaction tube that combines the oxidation and reduction reactions. The combustion takes place in a helium atmosphere containing an excess of oxygen gas at the oxidation zone at the top of the reaction tube. Combustion products are transported by a helium carrier through the reduction zone at the bottom of the reaction tube to remove excess oxygen and through a separate drying tube to remove any water. The gas-phase products, mainly CO2, N2, and SO2, are separated by a gas chromatograph. The gas is then introduced into the isotope-ratio mass spectrometer (IRMS) through a Finnigan MAT (now Thermo Scientific) ConFlo II interface, which is also used to inject SO2 reference gas and helium for sample dilution. The IRMS is a Thermo Scientific Delta V Plus CF-IRMS. It has a universal triple collector with two wide cups and a narrow cup in the middle. It is capable of measuring mass/charge (m/z) 64 and 66 simultaneously. The ion beams from SO2 are as follows: m/z 64 = SO2 = 32S16O16O; m/z 66 = SO2 = 34S16O16O primarily.

Additional publication details

Publication type:
Publication Subtype:
USGS Numbered Series
Determination of the δ34S of low-concentration sulfate in water; RSIL lab code 1949
Series title:
Techniques and Methods
Series number:
Version 1.0 - May 2006, Version 1.1 - 2007, Version 1.2 - September 2012
Year Published:
U.S. Geological Survey
Publisher location:
Reston, VA
Contributing office(s):
Reston Stable Isotope Laboratory
viii, 35 p.
Larger Work Type:
Larger Work Subtype:
USGS Numbered Series
Larger Work Title:
Chapter 8 of Book 10, Methods of the Reston Stable Isotope Laboratory, Section C, Stable Isotope-Ratio Methods
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