This document summarizes the analysis of a square glass bottle containing remnants of dried hair dye. The bottle was labeled "Guilmard Eau Sublime" and dated to the late 19th century. Analysis found the black material inside had polymerized over time and no longer contained the original dye ingredients. Infrared spectroscopy detected aromatic, C-N, and N-H bonds, indicating the dye originally contained para-phenylenediamine, a common hair dye ingredient at the time. Simple chemical tests did not identify the material due to degradation over decades. The bottle likely originally held a two-part hair dye system with hydrogen peroxide in a separate container.
This document summarizes the analysis of a square glass bottle containing remnants of dried hair dye. The bottle was labeled "Guilmard Eau Sublime" and dated to the late 19th century. Analysis found the black material inside had polymerized over time and no longer contained the original dye ingredients. Infrared spectroscopy detected aromatic, C-N, and N-H bonds, indicating the dye originally contained para-phenylenediamine, a common hair dye ingredient at the time. Simple chemical tests did not identify the material due to degradation over decades. The bottle likely originally held a two-part hair dye system with hydrogen peroxide in a separate container.
This document summarizes the analysis of a square glass bottle containing remnants of dried hair dye. The bottle was labeled "Guilmard Eau Sublime" and dated to the late 19th century. Analysis found the black material inside had polymerized over time and no longer contained the original dye ingredients. Infrared spectroscopy detected aromatic, C-N, and N-H bonds, indicating the dye originally contained para-phenylenediamine, a common hair dye ingredient at the time. Simple chemical tests did not identify the material due to degradation over decades. The bottle likely originally held a two-part hair dye system with hydrogen peroxide in a separate container.
This document summarizes the analysis of a square glass bottle containing remnants of dried hair dye. The bottle was labeled "Guilmard Eau Sublime" and dated to the late 19th century. Analysis found the black material inside had polymerized over time and no longer contained the original dye ingredients. Infrared spectroscopy detected aromatic, C-N, and N-H bonds, indicating the dye originally contained para-phenylenediamine, a common hair dye ingredient at the time. Simple chemical tests did not identify the material due to degradation over decades. The bottle likely originally held a two-part hair dye system with hydrogen peroxide in a separate container.
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Guilmard Eau Sublime Hair Dye Bottle with Iron Cap
University of West Florida
Artifact: 86D 8 011 076 8E534 Panton Leslie
Analyst: Amanda Vu April 8, 2016
Appearance of Artifact The artifact was a square glass bottle (Fig. 1) of dark brown color with an iron cap. On one side it had raised lettering saying Guilmard Eau Sublime, as shown in Fig. 2. On the inside surface there were remnants of what was believed to be dried hair dye. The iron cap was extensively rusted. The bottle was about 4 inches tall and the square part was about 1 inch wide. Fig. 1 Artifact
Procedure and Results
The solid material inside the bottle was scraped off for analysis. Pieces of patina that also came off were removed as they were a product of glass decomposition, rather than part of the original contents of the bottle. A 0.05 gram sample of the black material was placed in a muffle furnace at 850o C for 8 h. None of the sample remained after this treatment. Separation of the sample by thin-layer chromatography was attempted using a silica plate and ethanol, cyclohexane, and pyridine as eluents but no separation was achieved with any of these. A fluorescence emission spectrum of the sample was also obtained (not shown).
Fig. 3 Infrared spectrum of unknown material
Fig. 2 Side of bottle, showing raised
lettering
Discussion and Conclusions
An early report on hair dyes such as Mrs. Potters Walnut Tint Hair Stain and Eau Sublime noted that these products produced a dark color by reaction of para-phenylenediamine (PPDA) with hy-drogen peroxide. A dire warning was given about a marked lassitude and an obscure general eruption resulting from the use of such hair dyes.1 Earlier work in our laboratory identified PPDA as a component of a Mrs. Potters hair dye sample recovered from an excavation at Sandpoint, Idaho.
The contents of the present Eau Sublime bottle retained none of the original constituents, as they had polymerized through long exposure to oxidative and hydrolytic conditions. Consequently, the simple PPDA test described in ref. 1, namely:
addition of an acetic acid solution of the unknown to a ferric chloride solution producing a violet color;
addition of a few drops of a 1% potassium permanganate solution to the
unknown leading to decolorization and the production of and ammonia smell.
did not produce positive results.
Likewise, when a small amount of the sample was added to acetic acid and the solution was mixed with a drop of aqueous aniline (one drop of aniline per 50 mL of water), and potassium persulfate was added, a blue color (a positive result) did not appear.2 However, infrared spectroscopy (Fig. 3) did reveal the presence of aromatic moieties, CN, and NH bonds in the material: aromatic C=C at 1580-1600 cm1; CN at 1250-1370 cm1; and NH at 34003500 cm1. These are strong indications of the presence of materials that arose from long-term chemical modification of PPDA. It must be concluded that this was the principal ingredient of the dye. The other component, hydrogen peroxide, would have been contained in a separate bottle that was not part of this consignment. 1
Nostrums and Quackery, first edition, vol. 1, Press of the American Medical Association, Chicago, pp. 354ff, ca. 1912 (undated). 2 Feigl, Fritz, Vinzenz Anger, and Ralph Oesper. Spot Tests in Organic Analysis. 7th ed. Amsterdam, London, New York: Elsevier, 1966.
