Friday, August 21, 2015

Sulfur of Saturn

The Roman Goddess Ops, 'sweet'-heart (and wife)
of Saturn, Peter Paul Rubens c. 1630,
“Abundance (Abundantia).” [1]
Antonio Neri’s book on glassmaking, L'Arte Vetraria, devotes an entire chapter to making artificial gems. These are made with an especially dense, refractive form of lead glass—what today would be called lead crystal. He made it in small batches, in sealed ceramic vessels; each infused with various metal oxide pigments to give characteristic jewel tone colors.  His secret ingredient for making the finest artificial gems was a material known as "sulfur of Saturn." He writes:
You will have jewels of marvelous beauty in every color, which by far surpass those described above, made with ordinary minium. Because with this true sulfur of Saturn, they will surpass all others by far more than I can write here, as I have seen and made many times in Antwerp.[2]
This "ordinary minium" that he speaks of is one of several oxide forms of lead, also known as 'red lead,' it is bright red or orange in color. As a stable red pigment it was well known to ancient Byzantine and Persian illuminators. [3] It was so popular, in fact, that the word used to describe small intricate pictures 'miniature,' is derived directly from 'minium.' [4] The intricate embellishments in manuscripts ultimately took on the name of the scribes' favorite color.  In glass, minium does not impart red or any other color on its own, but does add 'sparkle' and made Neri's jewels highly refractive to light. 

In the recipe, he uses white vinegar and he reacts it with finely ground minium through a laborious process. The acetic acid in vinegar chemically combines with the minium to form lead acetate, which alchemists called "sugar of Saturn" because it had a distinctively sweet taste (more on that later). [5] Lead (Saturn) could be added to the melt in a number of different forms including acetate, carbonate and various oxides. The heat of the furnace reduces them all and the result is essentially identical glass from any of these sources. The lead acetate has one major advantage that set it apart from the others. Lead acetate is soluble in water and therefore it can easily be purified of contaminants and to a much higher degree. It can be filtered, allowed to stand and decanted after any insoluble impurities settle out.

In other references "sugar of Saturn" and "sulfur of Saturn" are considered synonyms. This is not the case with Neri, for him they are two different substances; the 'sugar' is a precursor for his final product, sulfur of Saturn:
Left in the bottom will be a salt as white as snow, and as sweet as sugar. Repeat the dissolution, and filtering, and evaporation with common water three times. This is the required sugar of Saturn. 
Keep it to calcine in sand in a glass flask or ball in a furnace over a moderated fire for many days. It will further calcine to a color that is much redder than cinnabar, and more finely impalpable than sifted grain flour. This is the required true sulfur of Saturn; purified from the sediment, foulness and blackness that were upon the lead at first. [6]
It would be a reasonable guess that by heating the acetate for "many days" he is reducing it back to minium, its more basic, bright red oxide state, but this time in a greatly purified form.

Unfortunately for his health, in this recipe for sulfur of Saturn, Antonio makes extensive use of heating and evaporation. Even more unfortunate is that in a number of steps he judges the potency of his product by taste. Lead acetate is highly toxic; because it is soluble in water, it enters the bloodstream easily. It attacks the nervous system, accumulates in the bones and can cause organ failure. It is quite likely that by breathing the fumes and tasting crystals of sugar of Saturn, Neri was contributing to his own demise at the relatively young age of thirty-eight. Lead acetate was not the only toxic substance he handled regularly, but it was certainly one of the worst for his health. 

 It does not follow that he was totally ignorant of the risks he was taking. The dangers of heavy metals were recognized from early times. Pliny speaks of the noxious fumes from lead furnaces, and Plutarch opined that lead and mercury mines were "unwholesome and pestilent places." Neri’s own father followed the work of Dioscorides, who wrote that ceruse (lead carbonate), taken internally, could be fatal and that certain sweet wines could adversely affect the abdomen and the nerves.

Ancient Romans discovered that when wine started to turn to vinegar, it could be boiled down in lead lined pots to produce a highly sweet syrup called sapa. A late Roman cookbook made extensive use of sapa, which presumably contained considerable lead acetate. [7] It has been conjectured that  lead laced sapa contributed to poisoning among the Roman aristocracy. While lead acetate is a deadly poison, it is a step too far to imply that it contributed to the fall of the Roman Empire.

[1] Alchemical tradition does provide for an association between the metal lead and the Roman god Saturn. However, there is no such association between 'sugar of Saturn' and either of his consorts Ops or Lua, although Ops, the goddess of abundance (opulence) does rather nicely represent the chemical that made Neri's most opulent artificial gems possible.
[2] Neri 1612, ch. 91.
[3] Chemically, this is Pb3O4, also known as Lead (II,IV) oxide, triplumbic tetroxide. Historically, it was called minium and red lead.
[4] The accepted etymology of ‘miniature’ is from ‘minium,’ but may have been influenced by similar Latin terms such as  minor, minimus, minutus, etc.
[5] Lead acetate comes in two forms; Pb (C2H3O2)4 and Pb (C2H3O2)2, both are toxic; the later variety is soluble in water.
[6] Neri 1612, ch. 91.
[7] “Saba” endures today as a popular grape syrup, albeit without the lead.
* This post forst appeared here on 12 September 2014.

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