Analysis of a Meteorite Found at Winslow Arizona

J. A. White

[transcribed by J. Lazio]

[The following analysis was recorded by John Alden White (1873--1963). The copy of his research notes that I have is both undated and appears to be a mimeographed copy. I believe that it was copied by his daughter, Teresa White Zeider. I have attempted to transcribe it as best as I could, but I have had difficulty in reading certain words and, in certain sections, it appears as if a small portion had been erased. Given that he is analyzing the meteorite for elements such as iron, I would guess that the meteorite was an S-type or stony meteorite.]

The meteorite was taken to the Beloit Iron Works and a projecting corner taken off in the pla??. The pla??ings were carefully collected ?? of the least altered ?? and dried. A careful quantitative anlaysis showed that iron, cobalt, nickel, and phosphorus were present.

For the quantitative analysis the methods set down in the Chemical Analysis of Iron by Blair were closely followed. Phosphorus and iron were determined from different weighings. Nickel and cobalt together.

Phosphorus

To determine the phosphrous two amounts of 0.8562 g and 1.0254 g respectively were taken, dissolved in HNO₃ specific gravity 1.42. The solution was evaporated to dryness, the residue picked up with H₂O, NHO₃ and a little HCl. This was again evaporated to dryness to expel the excess of HNO₃. It was again picked up with a little HNO₃, HCl, and H₂O. This solution, which should not exceed 50 or 60 cc, was transferred to an Enemeyer(?) flask of about 250 cc capacity and 100 cc of a standard molybdate solution added; this was heated in a water bath at 40^o for about 4 hours then filtered on(?) a small washed filter and washed through with dilute molybdate solution (1 part H₂O; 1 part solution) until the filtrate gave no test(?) for iron with the filtrate ?? was set aside to see if any further precipitation of ammonium phosphous molybdate takes place. If so it is filtered off and to be added to the marginal amount.

The precipitate of ammonium phospho-molybdate was dissolved by poring 2 or 3 cc strong NH₄ upon it and stirring up well with a fine stream of hot water, allowing the solution to run into the Erlemeyer flask in which the precipitate was first made. See that every particle of the precipitate which may have been left in the origional Erlemeyer flask is removed, run the solution through the same filter as before into a beaker of 100 cc capacity. Wash out the flask with a little hot water and NH₄OH. Use as little as possible to secure complete solution of precipitate. When amount of precipitate is small the filtrate washing(?) should not exceed 25 cc. The ?? the solution was neutralized with strong HCl. If the yellow phosphorus molybdate begins to precipitate, add NH₄OH until it redisolves. Then to the cold alkaline liquid ?? from a burette 10 cc magnesia mixture was slowly added stirring constantly, 4 drops per minute as about the rate of flow. Then ?? one-third of the volume of the solution of strong NH₄OH was added and stirred vigorously. ?? the beaker was placed aside ice code water for some time and ?? the solution stirred several times after the precipitate had begun to crystalize out. It was allowed to stand for four hours, filtered off out to a small ?? filter and washed with dilute NH₄OH (1 part NH₄OH to 2 part H₂O) containing 2.5 g ammonium nitrate to the 100 cc. It was ?? ignited very carefully to burn of (sic) the carbanacous matter and finally heated for several minutes over the blast ?? to volatilize any mobydate acid that may have ?? down with the Mg₂(NH₄)₂P₂O₈. It was cooled and weighed. The crucible was then filled halffull of water and(?) a few drops HCl added and then heated till the Mg₂P₂O₇ was dissolved. The small residue remaining filtered washed ignited and weighed the difference between the two weights in Mg₂P₂O₇ containing 27.836% Phosphorous.

The results are as follows:

  .227
  .214
  .441/2 = .220

Fe

Iron was determined in triplicate

Clean bright plainings(?) were weighted up in three amounts dissolved in HCl sp. gr. 1.20 in a #13 ?? beaker about 20 cc HCl being enough. The solution was then made up to about 250 cc and deoxidized with pure filtered into a procelain dish 10 cc H₂SO₄ added and then titrated with a solution of Potassium Permanganate of ?? strength. Found by titrating a solution of Iron Ammonium protosulphate. 1 cc = 0.0637 g Fe

  94.39
  94.9
  94.5
 ----
 283.79/3 = 94.59

Nickel and Cobalt

About 1 gram was dissolved in 15 cc HNO₃ sp.gr. 1.2 in a small beaker. This was evaporated to dryness and 10 cc HCl added and again was evaporated to expel all HNO₃. HCl was again added and then evaporated almost to dryness, until the solution was like syrup. The solution ws washed into a large Griffin(?) beaker of nearly a liter capacity in a #6 Griffin(?). The solution was made up to about 200 cc and neutralized by the slow addition of a solution of sodium carbonate; the solution being stirred vigorously all the time. When the solution became a very dark red and the precipitate f..ied dissolved slowly the Na₂CO₃ was added 2 or 3 drops at a time stirring the solution well and allowing to stand for a few minutes to see if the precipitate dissolved. When the precipitate remained HCl was added drop by drop the solution stirred and allowed to stand for a few minutes. If it did not clear, more HCl was added in the same manner until the solution cleared up. It is necessary that no more than enough HCl be added than to just dissolve the precipitate.

When the solution was clear of any precipitate a strong solution of sodium acetate was added the solution stirred and boiling water added until the volume was about 700 cc. The solution was then boiled for 10 min. and then the precipitate allowed to settle. The supersaturated liquid was desicated(?) in a large washed filter ... precipitate transferred to the filter and washed two or three times with boiling water.

The filtrate was transferred to a porcelain dish and evaporated rapidly, in which the precipitation was first made by ... of a spatula and that remaining on the filter + spatula was dissolved by pouring on ... hot dilute HCl (10 cc HCl + 20 cc hot H₂O) and allowing it to run into the beaker containing the precipitate. The filter was washed clean with cold H₂O and the beaker containing the precipitate heated until all the ferric(?) acetate was dissolved. The solution was allowed to cool and the precipitation, filtrates, and dissolving of the precipitate proceeded with as before/was done the third time.

The filtrate being poured into the porcelain dish in which the evaporation of the first filtrate was going on.

The precipitation and filtration was again performed and the the filtrate evaporated to about 300 cc and transferred to an #3 beaker.

In this way all the Iron was removed and the filtrate contained all the Nickel + Cobalt.

To the solution was added about 10 grams of sodium acetate and a few drops of acetic acid, the solution boiled and a steady current of H₂S passed through the boiling solution for 10 or 20 minutes to precipitate the Ni + Co. This was filtered out to a small asb... filter washed with H₂S water containing a little acetic acid dried and ig..ted then transferred to a small beaker dissolved in HCl + HNO₃ and evaporated to dryness.

Ni ??

The residue was picked up with a few drops of HCl and cold water. Two or 3 grams of KNO₂ dissolved in as little water as possible and acidulated(?) with acetic acid was added. The Cobalt ws precipitated as the double(?) nitrite of cobalt and potassium. The solution was stirred and set aside for 24 hrs. stirring it occasionally in the meantime.

It was then filtered and the filtrate set aside. The precipitate was washed with water containing sodium acetate and a little free acetic acid.

The filter and precipitate were very carefully ignited in a porcelain crucible so as not to fuse the precipitate. It was then transferred to a #1 beaker and ... with HCl + a little KClO₃. It was then evaporated to dryness undissolved(?) in a few drops of HCl diluted with cold water, about 1 gram of sodium acetate added and the whole boiled for about an hour to precipitate any Fe + Al. These were filtered off and to the filtrate an excess NH₄OH and NH₄HS added and then boiled for fifteen minutes. When the precipitate had settled it was filtered off and washed with water containing NH₄HS, dried and ignited in a platnium crucible. Next a little HNO₃ was added, the crucible heated carefullly and then the solution evaporated to dryness.

Then a few drops of H₂SO₄ were added to convert the sulphide and oxide of cobalt to sulphate and the excess of H₂SO₄ driven off. The crucible + contents was then heated to dull redness for a few moments, coooled + weighed a CoSO₄, which contains 38.05 percent cobalt.

CoSO₄

The filtrate from the double nitrite of potassium + cobalt was boiled and a slight excess of caustic soda added the whole boiled for a few minutes, the precipitate filtered off and washed with hot water.

The nickel oxide on the filter was dissolved in HCl and the solution allowed to run back into the beaker in which it was precipitated and the filter washed with hot water.

The solution was evaporated to dryness on a water bath. The residue was picked up with 3--5 drops HCl + 50 cc H₂O, about 1 gram of sodium acetate added + the solution boiled for about an hour to precipiate any FeO and Al₄O₃ present. These were filtered off + washed with hot water. The filtrate was heated to boiling, a slight excess NaDH added and the solution boiled for some(?) minutes.

The precipitate was filtered off on to a small ashless(?) filter washed with hot water. The filter precipitated ignited cooled + weighed as NiO which contains 78.55 percent Ni.

  1.107
  1.118
  2.225/2 = 1.112

  4.199
  3.636
  7.835/2 = 3.917

Analysis of Troilite found in the Meteorite

Some of the material was finely ground up in an agate mortar and from 0.2 to 0.3 g was taken. This was (intimately?) mixed with 10 grams of a fusion mixture (1 part Na₂CO₃ + 1 part K₂CO₃) and placed in a large platinum crucible.

This was heated careful over a blast ? until the mass was in a state of quiet fusion + perfectly clear. The fusion was ? well up the sides of the crucible and ? about half a gram or less of KNO₃ was added and ? whole fused again. When the fusion had become quiet it was again run up on the sides of the crucible and about the same amount of KNO₃ added and the mass fused again to quiet fusion. It was ? well up the sides of the crucible and placed in a beaker containing about 100 cc of boiling water. When the mass had dissolved the crucible was removed and washed with a small stream of water, allowing the washings to mix into the beaker containing the ?? of iron. The crucible st...? with iron was set aside. The liquid in the beaker was stirred well and the oxide of iron allowed to settle. The supersaturated liquid was decanted off through an ashen filter.

The oxide of iron again stirred up well with hot water and allowed to settle. The supersaturated liquid was decanted off and the crucible filtrates transferred to a porcelain dish acidified with HCl, about 20 cc is necessary, and evaporated to dryness in a water bath. The residue was acidified with HCl and again evaporated to dryness to expel all HNO₃. This residue was picked up with HCl and water transferred to a beaker heated to boiling and barium chloride added to slight excess. If there is an indication of iron present it is best to add a small crystal of tartaric acid before the barium chloride is added to hold(?) up the iron.

The solution was allowed to stand until the precipitate had all settled. The clear super...(?) liquid was decanted off through an ashless filter and finally the precipitate was transferred and washed with water containing a little ammonium acetate. The filter and precipitate were burned throughly in a ?? crucible allowed to cool a few drops of H₂SO₄ added and then heated carefully to expel excess of H₂SO₄. Finally, heating for ten minutes in the heat lamp. It was cooled and weighed up as BaSO₄, which multiplied by 0.1376 gives weight of Sulfer.

While the filtrates (above) were evaporating 10 cc HCl were poured into the crucible in which the fusions(?) was made the cover placed on and the crucible heated carefully. The acid was then decanted through the ashless filter, through which the liquid from iron oxide had been filtered, and the solution with washings allowed to run into the beaker containing the iron oxide. As this did not entirely remove the iron from the filter the paper was treated with a small casinole(?) with hot acid and water. The solution was then poured into the beaker containing the iron. The beaker and solution were heated to dissolve the iron oxide. In case the iron was not all dissolved the solution was run through an ashless filter and the particles of decomposed iron transferred to the paper which was thoroughly washed. The filter and undecomposed iron was transferred to the large platinum(?) crucible with the fusion mixture and heated exactly as in the first place with a less amount of KNO₃.

The filtrate after disolving the fusion being transferred to the evaporating filtrate and the iron oxide and cleanings of the crucible poured into the original solution.

This was then deoxidized with zinc, filtered to take out zinc impurities, H₂SO₄ added and the solution titrated with a solution of Potassium Permaingrate of known strength.

  36.55
  37.44
  -----
  73.99/2 = 36.99

  63.06
  63.1
 ------
 126.16/2 = 63.08

            36.99
            63.08
            -----
           100.07