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The origin, evolution, and cycling of volatiles on the Moon are established by processes such as the giant moon forming impact, degassing of the lunar magma ocean, degassing during surface eruptions, and lunar surface gardening events. These processes typically induce mass‐dependent stable isotope fractionations. Mass‐independent fractionation of stable isotopes has yet to be demonstrated during events that release large volumes of gas on the moon and establish transient lunar atmospheres. We present quadruple sulfur isotope compositions of orange and black glass beads from drive tube 74002/1. The sulfur isotope and concentration data collected on the orange and black glasses confirm a role for magmatic sulfur loss during eruption. The Δ33S value of the orange glasses is homogenous (Δ33S = −0.029‰ ± 0.004‰, 2SE) and different from the isotopic composition of lunar basalts (Δ33S = 0.002‰ ± 0.004‰, 2SE). We link the negative Δ33S composition of the orange glasses to an anomalous sulfur source in the lunar mantle. The nature of this anomalous sulfur source remains unknown and is either linked to (a) an impactor that delivered anomalous sulfur after late accretion, (b) sulfur that was photochemically processed early during lunar evolution and was transported to the lunar mantle, or (c) a primitive sulfur component that survived mantle mixing. The examined black glass preserves a mass‐dependent Δ33S composition (−0.008‰ ± 0.006‰, 2SE). The orange and black glasses are considered genetically related, but the discrepancy in Δ33S composition among the two samples calls their relationship into question. Plain Language Summary: Using isotopic compositions measured in volatile elements, we can identify the processes linked to isotopic fractionations and ultimately understand processes involved in a planets' evolution. We present sulfur isotope compositions of lunar glass beads from drive tube 74002/1 and demonstrate that an anomalous sulfur source was erupted from the lunar mantle with the orange glass beads. The observed isotopic anomaly has an unknown origin, but it requires a source of sulfur that was photochemically processed prior to its delivery to the lunar mantle and eruption at ∼3.6 Ga. Our results suggest that the lunar mantle is not well mixed with respect to sulfur sources and requires future multi‐disciplinary investigations to reconcile these important observations. Key Points: Orange glass 74002 preserves negative Δ33S valuesThe negative Δ33S associated with orange glass is linked to photochemically processed sulfur in the erupted sourceOrange and black glass preserve different S isotope compositions that calls into question their genetic relationship [ABSTRACT FROM AUTHOR]

High spatial resolution multiple sulfur isotope studies undertaken by multicollector secondary ion mass spectrometry (SIMS) commonly use well‐characterised sulfide reference materials that do not (or are assumed not to) exhibit mass independent fractionation in 33S and 36S, taking advantage of the three‐isotope plot to evaluate the extent of such fractionation in unknown targets. As a result, few studies to date have used a mass independently fractionated reference sulfide to demonstrate accuracy of measurement and/or data reduction procedures. This paper evaluates two mass independently fractionated sulfides, a pyrite from the 3.7 Ga Isua greenstone belt and a pyrrhotite from a 2.7 Ga gold deposit in Minas Gerais, Brazil which may be used to provide additional confidence in the obtained multiple sulfur isotope data. Additionally, the paper presents a method for measuring quadruple sulfur isotopes by SIMS at a comparable spatial and volume resolution to that typically employed for triple sulfur isotopes. This method has been applied to the Isua pyrite as well as to a sample of 2.5 Ga pyrite from the Campbellrand, Transvaal, South Africa previously investigated using SIMS for triple sulfur isotopes, illustrating its potential for quadruple sulfur investigations.©2012 The Authors. Geostandards and Geoanalytical Research ©2012 International Association of Geoanalysts [ABSTRACT FROM AUTHOR]