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Geological Survey DEPARTMENT OF THE INTEKIOE BULLETIN UNITED STATES r'. GEOLOGICAL SURVEY No. 167 ;/ ' WASHINGTON GOVERNMENT PRINTING OFFICE UNITED STATES GEOLOGICAL STJRYEY CHARLES D. WALCOTT, DIRECTOR t ' ' CONTRIBUTIONS TO CHEMISTRY AND MINERALOGY FROM THE FRANK W. OLARKE CHIEF CHEMIST WASHINGTON GOVERNMENT PRINTING OFFICE 1900 CONTENTS. Page. Letter of transmittal........................................................ 9 ' Prefatory note .............................................................. 11 Experiments relative to the constitution of pectolite, pyrophyllite, calamiue, and analcite, by F. W. Clarke and George Steiger ......................... 13 The constitution of tourmaline, by F. W. Clarke ............................ 26 The colorimetric estimation of small amounts of chromium, with special reference to the analysis of rocks and ores, by W. F. Hillebrand ........... 37 Volumetric estimation of vanadium in presence of small amounts of chromium, with special reference to the analysis.of rocks and ores, by W. F. Hille­ brand ........................................................ '. ........... 44 Distribution.and quantitative occurrence of vanadium and molybdenum in rocks of the United States, by W. F. Hillebrand....................... .... 49 Warning against the use of fluoriferous hydrogen peroxide in estimating ^ titanium, by W. F. Hillebrand ........................ .... ................ 56 '! Mineralogical notes, by W. F. Hillebrand ................................... 57 1. Calaverite from Cripple Creek, Colorado ............................ 57 ( 2. .Tellurides from California........... ............................... 60 / 3. Hessite from Mexico ................................................ 63 - 4. Covellite and enargite from Montana ............................ .... 63 5. Tysonite and bastniisite ......................... .................... 64 6. Prosopite ..................... .^.................................... 66 7. Jeffersonite ............................................... .......... 68 8. Anorthite and epidote ......................... .................... 69 9. Roscoelite .......................................................... 70 10. Mariposite ...... .............................. ...................... 74 ) 11. Two sulphates from Montana........................................ 75 On the chloronitrides of phosphorus and the metaphosphimic acids, by H. N. , t Stokes.................................................................... 77 1. On tri- and tetraphosphonitrilic chlorides ............................ .77 2. On trimetaphosphimic acid and its decomposition products ........... 89 3. On tetrametaphosphimic acid...................... .................. 116 4. The higher chloronitrides ............................................ 124 { 5. The higher metaphosphimic acids .................................... 136 ' On a hydromica from New Jersey, by F. W. Clarke and N. H. Dart on ..*...... 154 The alkaline reaction of some natural silicates, by F. W. Clarke............. 156 The solubility in water of certain natural silicates, by George Steiger ....... 159 Index ...................................................................... 161 5 ILLUSTRATIONS , Page. / FIGS. 1-2. Crystals of sodium trimetaphosphimate.......................... 97 J 3-4. Crystals of tri-silver trimetaphosphimate........................ 103 5-6. Crystals of tri-silver diimidotri phosphate........................ Ill 7. Crystal of hexaphosphonitrilic chloride.......................... 132 LETTER, OF TRANSMITTAL. DEPARTMENT OF THE INTERIOR, UNITED STATES GEOLOGICAL SURVEY. Washington, I). (7., November 4, 1899. SIR : I submit herewith a manuscript entitled Contributions to Chem­ istry and Mineralogy from the Laboratory of the United States Geo­ logical Survey. I have the honor to request that it be published as a bulletin of the Survey. Very respectfully, . F. W. CLARKE, Chief Chemist. Hon. CHARLES D. WALCOTT, Director United States Geological Survey. PREFATORY NOTE. In the following pages there have been brought together a variety of chemical and mineralogical researches, which were carried out in the laboratory of the United States Geological Survey between July 1, j 1893, and July 1, 1899. In one sense the bulletin is a continuation of / the series represented by Bulletins Nos. 9,42,55,60,64, 78,90, arid 113; only, unlike them, it reports no miscellaneous analyses. The latter represent -by far the larger part of the work done in the laboratory; but most of them are published in other form, in connection with the geological investigations to which they relate. Their repetition here is unnecessary. F. W. 0. > 11 CONTRIBUTIONS TO CHEMISTRY AND MINERALOGY. EXPERIMENTS RELATIVE TO THE CONSTITUTION OF PECTOLITE, PYROPHYLLITE, CALAM1NE, AND ANALCITE. By F. W. CLARKE and GEORGE STEI&ER. In a series of investigations by Olarke and Schneider, which were carried out iii the laboratory of the United States Geological Survey between 1889 and 1892,1 a number of reactions were examined which shed some light upon the constitution of several natural silicates. The work then begun was unfortunately interrupted for several years; but it is now resumed, with the hope that it may be pushed considerably further. Two of the reactions studied by Clarke and Schneider were of peculiar interest. First, in the case of talc, it was found that one-fourth of the silica could be liberated by ignition; and that the fraction thus set free was measurable by solution in aqueous sodium carbonate. This reac­ tion suggests that other acid inetasilicates may behave in a similar way, and that we perhaps have a means of discrimination between such salts and other compounds which simulate them. In other words, an acid metasilicate may be experimentally distinguished from a pseudo- metasilicate by the way in which it splits up when .ignited. Evidence bearing upon this supposition will be found in the present paper. The second of the reactions just referred to is that between dry ammonium chloride, at its temperature of dissociation, and various silicates.2 This involves, in part at least, the action of dry gaseous hydrochloric'acid upon the compounds which are studied: and different minerals are very differently attacked. Some are almost completely decomposed, others are affected but slightly; and here again there seems to be a method of diagnosis which deserves further attention. Both reactions suggest the main purpose of the investigation; which is, the fractional analysis of silicates by means of various reagents, in 1 Bull. U. S. Geol. Survey No. 78, p. 11; Bull. No. 90, p. 11 ; Bull. No. 113, p. 27. 2Bull. U. S. Geol. Survey No. 113, p. 34. 13 14 CONTRIBUTIONS TO CHEMISTRY AND MINERALOGY. [BULL. 167. order to gain evidence bearing upon their chemical structure. The evidence, at least, is of value, whether the interpretation of it be right or wrong. Bach fact helps to the ultimate solution of the central problem, the problem of constitution. PECTOLITE. The pectolite which was chosen for examination was the well-known radiated variety from Bergen Hill, New Jersey. The mineral was in long, white needles, and apparently quite pure; but the analysis shows that it contained some carbonate as an impurity. Enough of the material was ground up to furnish a uniform sample for the entire series of experiments, and the work properly began with a complete analysis. The results obtained are as follows: Analysis. v Si02 ........................................... 53. 34 A1203 ............... .......................... .33 CaO ........................................... 33.23 MnO. --..-.-.. ................................. .45 Na.O ........................................... 9.11 Total H2O. ........... .......................... 2.97 C02 . ............... ............................ .67 100. 10 Fractional water. At 105° .....^.... ............................. 0.27 At 180° ........................................ .16 At 300° ........................................ .22 2.32 2.97 <» All of the water was given off at a barely visible red heat; and the figures show that practically all of it is constitutional, a fact which perhaps hardly needed reverification. The analysis gives the accepted formula for pectolite, Does this represent, as is commonly assumed, a true metasilicate? If it does, we should expect that ignition would split off silica propor­ tional to the acid hydrogen, or one-sixth of the total amount. To answer this question several portions, of the pectolite were sharply ignited, to complete dehydration, and then boiled each for fifteen min- CLARKE AND") 6TE1GER. J CONSTITUTION OF PECTOLITE. 15 utes with a solution of sodium carbonate containing 250 grams to the liter. In the extract so obtained the silica was determined} and three experiments gave the following percentages: 8.96 8.67 8.42 Mean, 8.68 One-sixth of the total silica is 8.89 per cent; and the experiments, therefore, justify the original expectation. The belief that pectolite is a metasilicate is effectively confirmed. Upon the unignited pectolite the sodium carbonate solution has a slow decomposing action, both silica and bases being withdrawn. In two experiments fifteen minutes of boiling extracted 2.07 and 2.55 per cent of silica, and by a treatment lasting four days 4.80 per cent was taken out. With water alone similar results were obtained; the action being so rapid, although relatively slight, that pectolite, moistened, gives an immediate and deep coloration with phenol phthalein. By boiling
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