Lead antimonate yellow, or Naples Yellow, is one of the most common yellow pigments in Western European art. It was used mainly in the period from 1500 to 1850. During the 18th and 19th centuries, a whole range of production recipes was published. However, the early production history of the pigment is not well understood. In this paper, a study of two early production recipes is reported. Under the nomenclature of potters’ yellow, the recipes describe some production details of the pigment. Reconstructions of the historical lead antimonate yellow were made according to these sources. X‐ray powder diffraction (XRPD) was used to examine the reaction products. Our findings show that various types of lead antimonate yellow can be formed, following the descriptions given in the recipes. Some of these types, notably lead–tin antimonate, have been found in earlier studies of authentic works of art. No evidence was found for a locally limited use of this pigment, as has previously been suggested. Documentary and analytical evidence indicates that the knowledge on lead antimonate yellows originates from Middle Eastern ceramic and glass industries. It is argued that the know‐how on the production of lead antimonate yellows has been transferred via the migration of glass artists from the Eastern Mediterranean to Venice during the 15th century.

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A micro‐invasive technique is presented that enables pigment sampling from individual layers of a painting cross‐section by obtaining a furrow 10–50 μm wide of chosen length. Combined with increased sensitivity of lead (Pb) isotope analysis using multicollector inductively coupled plasma mass spectrometry (MC‐ICPMS) equipped with a 1013 Ω resistor or a Pb double‐spike technique, the amount of Pb needed for isotopic analysis is drastically reduced, while maintaining a relative 2 SD precision for 206Pb/204Pb of < 0.02%. The methodology proved able to characterize Pb isotope differences within paint layers.

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