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Chemistry Index

Chemical Element Identification Timeline
History of Phosphorus : Introduction and Timeline

History of Science and Technology Index

Characters involved in the Phosphorus Story

Hennig Brand (1630 - c. 1710)
Johann Kunckel (1630 - 1703)
Johann Daniel Krafft (1624 - 1697) and Gottfried Wilhelm Leibniz (1646 - 1716)
Johann Joachim Becher (1635 - c. 1682)
Robert Boyle (1627 - 1691) and his Assistants

Transcripts of Publications (1677 - 1853)

Aerial Noctiluca : Robert Boyle 1680

An Account of four sorts of factitious
Shining Substances : Robert Boyle 1677


A Paper of the Honourable Robert Boyle's,
Opened Since His Death (1692)


Some Observations made upon an Artificial
Shining Substance : Robert Boyle 1677


Extracts from John Evelyn's Diary 1681 and 1685

Experiments made with the liquid and of the solid
Phosphorus : Frederick Slare 1681


Extract from Experiments of the Luminous
Qualities of Amber : Samuel Wall 1708


On the Discovery of Phosphorus and a
Biography of Ambrose Godfrey
Hanckwitz : Joseph Ince 1853


An Extract from "An Account of some
Experiments upon the Phosphorus Urinæ"
by Ambrose Godfrey Hanckwitz 1731

Other Information

The Chemical Equations involved in the Luminescence of Phosphorus

 

 

Accidents in the Laboratory and elsewhere

Boyle describes how is assistant, by this time Hanckwitz, suffered from burns in pursuit of his master's objective (and he obviously was not the only one). Boyle seems more occupied with the evidence of the impurity of the product rather than his assistant's welfare:

(Line 1692) "If our phosphorus be for any time pressed hard between the fingers, or against a board, or some such hard, and not very cold body, it will feel actually and very sensibly hot; and sometimes the degree of heat will be so vehement, as to scorch the skin, as my venturous assistant found several times to his pain; his fingers being almost covered with blisters, raised on them by handling our shining matter: he also complained to me, that, though he had been often burned on other occasions, yet he found blisters excited by the phosphorus, more painful than others; and he is not the only person, who has complained of finding burns made with this matter, to be more tedious and difficult of cure than ordinary ones. But, as our noctiluca was not always made of the same matter, nor with care equally successful; so I observed its disposition to burn, and the degrees of heat, to which it would be brought by motion, to be different; upon which account, I did not find that some portions of it, would produce those higher effects of heat, that others did; besides, these higher effects gradually differed among themselves."

It would seem that Hanckwitz had plenty of battle scars as related by the following passages.

(Line 1728) "To try, whether our phosphorus, which appeared not inferior to that of Mr. Krafft's, would (as his sometimes did) fire gun-powder; we took a little of our shining matter, and having wiped it dry, we put it upon some gun-powder, and with a knife pressed it, and in some sort rubbed it upon the black grains; but found, that though a heat were produced, and sometimes such as would make some of the corns of powder have a bluish flame, yet the mixture would not go off: so that the assistant, to whom I left the care of repeating the experiment, presuming it would not success, scrupled not to hold his head over it, that he might better see what change was made in the mixture; but then, upon a sudden, the powder took fire, and the flame shooting up, burnt his hair.

The same person, not long after, bringing me some newly distilled grains of our noctiluca, covered with some of the shining water; that came over with it, he unluckily broke the glass in his pocket; whereupon the heat of his body, increased by the motion which a long walk had put it into, so excited the matter, fallen out of the broken vial, that it burned two or three great holes in his clothes."

However, Hanckwitz does seem to have sometimes put himself in harm's way:

(Line 1769) "The highest effect of the heat of our icy noctiluca, was casually produced by my assistant; who being desirous to try, whether some that was newly prepared, were good, began to draw letters with it, upon a piece of plank, that had been long used in the laboratory, as part of a stove; and, chancing to press the matter hard upon this board, that the consistent heat of the place had brought to an unusual degree of dryness, he found, to his surprise, that he had not only shining, but burning letters; the lucid matter having actually set on fire those parts of the wood, against which he had strongly pressed it."

 

 

HISTORY OF SCIENCE AND TECHNOLOGY

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Icy Noctiluca : Robert Boyle 1682

The text of Icy Noctiluca used for the extracts shown on this page is available as a PDF through this link that opens in a new window.
The line numbers shown in the text below refer to the PDF.

The first section of this version of the Icy Noctiluca is focused on Boyle's initial experiments and repeats much of the information published in 1680. The second section relates his almost accidental discovery of the Constant Nocticula (solid phosphorus) that he had long searched for.

(Line 793) "The shining matter, contained in our best vials, being, at length, partly wasted in experiments, and partly given away; I thought fit to try, whether by the help of heat, and other motion, our want might not be supplied, until more could be prepared.

In pursuit of this design, I took an old vial, that had long lain by as useless, because the noctilucal matter had been poured out of it into a smaller glass; and having held that side of this vial, to which I perceived some feculent matter stuck, near the fire, until it had conceived a considerable degree of warmth, I removed it into a dark place; and found it to shine vividly ....."

Boyle describes how he entertained visitors with his new Icy Noctiluca or self-shining substance.

(Line 961) "And being one night willing to give a lady, and some other company, the diversion of a new phenomenon; after having opened the vial, and then stoppered it again, I shook it, and turned it so, that, much the greatest part of the liquor having been before poured out, the resident was spread over the inside of the glass, to which its particles stuck, because there wanted liquor enough to wash them down: by this means, those little portions of the sediment being not covered, as usual, with water, but exposed to the immediate contact of the air, shone much more vividly than the luminous exhalations; and the light being tremulous and twinkling, as well as brisk, they seemed to resemble so many little stars in a clear night, and continued this sparkling longer than one would have expected, to the delight of the spectators; for whose sake the experiment was several times repeated, and with success."

He goes on to relate why he chose the name Icy Noctiluca:

(Line 985) ......"And first, though this usually came over in distillation, in the form of many little grains, or fragments, differing, for the most part, from one another, both in bigness (some being of the size of grains of corn, and others of peas, or large cherry stones) and shapes, which most commonly were irregular, yet when the distillation was carried on prosperously, we obtained the desired matter in greater lumps; sometimes as large as small beans, and at others, three or four times as large, but not proportionally thick.

These lumps, whether small or great, were colourless; and usually when held against the light, transparent; so that many bodies placed beyond them at a distance, might be plainly seen through them. And some of the larger appeared so like such fragments of ice, as being thin, are often very clear, and almost quite destitute of manifest bubbles; because of this great resemblance, and for distinction sake, I thought it not amiss to call our consistent self-shining substance, the icy, or glacial noctiluca, or phosphorus."

Boyle and his team then worked to obtain larger samples of the solid phosphorus.

(Line 1028) "The consistent phosphorus is fusible enough. For though in the air it will not be brought to melt, without some difficulty and waste; yet by the help of hot liquors, and even of water itself, it may, with a little dexterity, be dissolved; which is an observation of good use; because, by means of fusion, several fragments, if the matter be pure enough, may be brought to run into one lump; and in that condition may both be the better preserved, and become fit to be applied to some considerable uses, which cannot so well be made of less, though numerous fragments."

Boyle records his observations of his solid phosphorus.

(Line 1042) "....And when this solid noctiluca is held in the free air, though perhaps its superficies be wet, it affords a very vivid light, usually surpassing that of the aerial noctiluca; and this light seems to proceed from, if not also to reside in, the body itself ......"

(Line 1063) ".....For as soon as it is again taken out of the water, (though it have lain very long there) it falls to shine again, even whilst it is yet dripping wet.

And I have sometimes observed, that when I had so large a piece of noctiluca, that I could conveniently hold one half of it under the surface of the water, and the other half above it, whilst the immersed part afforded no light, the extant part shone vividly."

Boyle is pleased to report that his Icy Noctiluca could be used to solve the problem of the unpleasant smell he had been forced to subject his 'delicate spectators' to. He also shows that he gives thought to his expenditure:

(Line 1208) "It has rendered the experiments made with aerial noctiluca much less acceptable, than otherwise they would have been, to the delicate sort of spectators, that the light produced was accompanied by a very unpleasant smell, that effused out of the vial whenever it was unstoppered, to let in the air. But by the help of our icy noctiluca, I found a way to prevent this ungrateful concomitant of our artificial light. For having, in a very small vial, put about a grain of noctiluca matter, and covered it with as much pure essential oil of cinnamon, as would swim less than a finger's breadth above it; we carefully stoppered our little vial, and having warily held the bottom of it against a fire, until the phosphorus began to melt, I suffered it to cool; and then, unstoppering it in a dark place, had the pleasure to see a vanishing indeed, but vivid light. So that, by this means, I could afterwards show the production of light to the nicest persons, adding to the pleasure of a delightful phenomenon, that of a fragrant smell. Because the oil of cloves is more easy to be had good, than the oil of cinnamon, and it is also cheaper, I tried the experiment more fully with that."

Boyle makes sure to protect his own skin when touching his Icy Noctiluca:

(Line 1714) "And accordingly, after having in vain tried to fire paper, by pressing and rubbing some of our phosphorus upon it with a blasé of a knife; I took a piece of fine paper, and having dried, and warmed it at the fire, I put a little of our noctiluca in a fold of it; and rubbing the paper between my hands, though there was thereby produced considerable heat, yet it did not reach to what I desired; but continuing a little while to rub the paper, it on a sudden took fire, and blazed out, so that it would have burned my hand, had it not been guarded by a thin glove, which was thereby scorched, and in part shriveled up. After the same manner, to make the experiment the more certain, I fired another piece of paper."

Boyle finishes his paper with the method he used to make phosphorus (which is much the same as the method he published two years previously). He does seem to indicate that he only used urine in the distillation:

(Line 2027) "I will not positively affirm, that the matter I employed is the very same that was made use of by the ingenious German chymists, in their noctiluca; for some inquisitive men have told me, that the Germans mix two or more distillable materials; whereas I employed but one substance capable of distillation."

Although he admits that he has produced phosphorus from other sources, one of which reads like dried faeces while the third remains a complete mystery:

(Line 2034) "Though the foregoing observations were commonly made upon that substance, which, I guess, to be, at least, the chief employed by the Germans; yet I first thought, and upon my first trial found, that it is possible to make noctiluca of a dry pulverable substance, which, for ought I can guess, was never employed by Mr. Krafft, or those from whom he had his secret. And besides this second sort or phosphorus, we made a third, which was obtained from a material, that never had been either a part, or an excrement of a human body; nor was mixed with anything that had been so."

He follows this with a paragraph worthy of a true alchemist.

(Line 2046) "To name the matter, though ever so explicitly, would not, in my opinion, have sufficed to inform those who would work upon it; for chymists themselves would, in all probability, work, as hitherto, on other occasions, they have done, upon the volatile and saline, which they presume to be the only spirituous and noble parts of the concrete; throwing away the rest as useless and abominable."

Boyle relates that he experimented with fresh urine but the product could not be made to shine. However, he admits that the procedure is complex and that there could have been other factors that affected the outcome:

(Line 2055) "I think fit to give notice, that having employed the material of our noctiluca without previous fermentation or putrefaction, though it was proceeded with after the same manner, with that whereby we obtained our shining substance; and though it afforded a substance, for colour and consistence not unlike our luciferous matter; yet I could not find that it would shine at all. And, indeed, there are so many circumstances that may make the experiment miscarry, that he who shall, at the first attempt, succeed in preparing this liquor, must be a very skillful, or a very lucky operator."

And finally another accident in the laboratory. Boyle puts the blame on the victim for not having listened to instructions and relates how he came to the rescue:

(Line 2185) "But in my absence; the operator, not staying for particular directions, rashly inverted the instrument, without taking care to get away; whence it happened, that as soon as ever the contained liquor, being too plentifully poured out, came to work on the sal-ammoniac, wherewith it usually produces cold, there ensued an expansion or explosion, so surprisingly great, that with a vehement noise the glasses were broken into a multitude of pieces, and much of the mixture thrown up, with violence, against the operator, whereby his hat was struck off, and his face, especially about the eyes, much hurt; whence, immediately, tumors, extremely painful, were produced; which might, also, have been very dangerous, had I not directly caused the parts affected, to be bathed with a solution of Saccbarum Saturni1 in fair water; by which means, within an hour or two, the pain that had been so raging, was taken away, and the fretting oil kept so much as breaking the skin of the tumours that it had raised."

1Saccbarum Saturni = Sugar of lead or lead acetate

 

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