DEPARTMENT OF THE INTERIOR

BULLETIN

OF THE

GEOLOGICAL SURVEY

3STo. 6O

WASHINGTON

GOVERNMENT PRINTING OFFICE 

1890

UNITED STATES GEOLOGICAL SUKVEY

J. \V. POWELL, DlllECTOK

REPORT OF WORK DONE

IN THE

DIVISION OF CHEMISTRY AND PHYSICS

MAINLY DUKUs'G THE

FISCAL YEAH 1887-'88

F. W. CLARKE, Chief Chemist

WASHINGTON 

GOVERNMENT PRINTING- OFFICE

1890

CONTENTS.

Pago.

Preface.........................................'................... .... ...... 11

The chemical structure of the natural silicates. By F. W. Clarice............ 13

Some nickel ores from Oregon. By F. W. Chirke.... ....................... 21

Natural soda: Its occurrence and utilization. By Thomas Marean Chatard.. 27

Composition ...................................................... ...... 28

Sodium sulphate ......................*............................. 29

Sodium chloride .................................................... 30

Sodium carbonate....... ...................................... ...... 31

Sodium bicarbonate. ...... ............ ...... ............ ...... ...... 34

Sodium sesqnicarbonatc.............................................. 35

Localities and mode of occurrence...................................... 36

Hungary............................................................ 36

Egypt.............................................................. 38

Armenia ............................................................. 39

Venezuela .......................................................... 40

North America.......................... .^.......................... 41

Wyoming. ................................................ ...... 42

Rag town Lakes, Nevada...,...................................... 4C>

Ragtown Soda Works........................................... 49

Mono Lake, California.......................................... 53

Abort Lake, Oregon....................... ...................... 53

Dry deposits.................................................... 55

Owen's Lake, California....... ...... ............................ 57

Owen's Lake Soda Works........................................ 58

Experiments on the evaporation and fractional crystallization of the water

of Owen's Lake...................... ......................... 59

Evaporation .................................................... 59

Fractional crystallization ....................................... 61

Discussion of results ............................................ 65

Fractional crystallization of water of Mono Lake................. 65

Urao..................................................................... 67

Native urao from Venezuela..................................... 67

Native urao from Egypt......................................... 68

True character of Trona, or the native sesquicarbonate .......... 69

Artificial production of sesquicarbonate.......................... 72

Urao from Owen's Lake ......................................... 75

Artificial production of urao; experiments and discussion of results.. .................................................. ...... 78

Analytical methods...................................................... 85

Origin of natural soda............. ....................................... 89

f>
6 CONTENTS.

'Pago. 

Natural soda Continued.

Cause of the red color of alkaline brines ................................. 95

Leaching of alkaline soils and clays..................................... 96

Conclusions............................................................. 99

Analyses of six new meteorites. By J. E. Whitfield.......................... 103

The Rockwood meteorite.......:................................. 103

Chattooga County meteorite. .................................... 106

Tauey County meteorite......................................... 106

Linuville Mountain meteorite ................................... 107

Fayette County meteorite.... .................................... 107

San Bernard! no County meteorite................................ 114

Two sulphantimonites from Colorado. By L. G. Eakins...................... 115

Coefficients of volatility for aqueous chlorhydrie acid. By Robert B. Warder.. 11.9

Experimental method................................................... 120

Calculation of results................................................... 121

Discussion of results............ ............ ...... ...................... 122

Analyses of jade. By F. W. Clarke...................... ............ ........ 123

Miueralogical notes:

1. Petalite from Peru, Me, By.JF. W. Clarke............................ 129

2. Spessartite from Amelia County, Va. By F. W. Clarke. .............. K9

3. Oligoelase from Bakersville, N. C. By F. W. Clarke.................. 129

4. Willemite from Franklin, N. J. By F. W. Clarke............ .... .... 1.30

5. Descloizite from Beaverhea I County, Mont. By. W. F. Hillebrand.... 130 

G. Preliminary remarks on North American urahinites. By W. F. Hilleibrand ..................................... ........................ 131

7. Dumortierite from New York and Arizona. By J. E. Whitfield....... 133

8. Xanthitane from North Carolina. By L. G. Eakins................... 135

9. Triplito from the Black Hills. By L. G. Eakins .'.......,............. 135

10. Kaolin fromGnnuison County, Cob. By L. G. Eakins..---. .......... 130

11. Native gold from Persia. By C. CatleU .............................. 137

12. Pyroxene and serpentine from Montville, N. J. By C. Catlett........ 137

The subsidence of fine solid particles in liquids. Second paper. By Carl Barns 139

A new method of making alloys. By William Hallock....................... 147

Miscellaneous analyses:

Rocks collected by E. D. Irving. .... ... ... .... ...... ...... .............. 149

Novaculite from Marquodfce, Midi........................................ 151

Brick clay from New Ulin, Minu....... ................ .................. 151

Rocks from Mon tana...... ...... ...... .... ............ ...'........... .... 152

Eruptive rock from the Henry Mountains, Utah........ .................. 154

Rocks from New Mexico................. ...... ...... .... ................ 155

Lavas from near Lassen Peak, California.. .............................. 155

Basalt from Mytilene .......... .... ...................................... 158

Inclusion in diorite from Cruger's Station, N. Y.......................... 158

White earth from Talladega, Ala.......... ............ .... .............. 158

Sandstone from Berea, Ohio..................... .... .................... 158

Knox dolomite and residual clay, from Alabama........................... 159

Dolomi te from Tuckahoe, N. Y .......................................... 159

Dolomite marble from Cockeysville, Md. ................................ 159

Marble from Louisiana.................................................. 160

Limestones from Ohio and Indiana ..............'........................ 160

Coqnina, coral, coral rocks, etc.... ...................... ................ 162

Iron and manganese ores.................................. .............. 164

Coal and coke. .......................................................... 169

Efflorescence from Cliff Creek, Colo...................................... 170
CONTENTS. t

Pago. Miscellaneous analyses Continued.

Salt from Hutchinson, Kans............................................ 171

Water from Lincoln County, N. C........................ ................ 171

Water from St. Augustine, Fla.......................................... 171

Water from McLeansborougb, 111........................................ 172

Water from Lebanon, Mo.......... .......... ........ .................... 172

Water from Hominy Hill, Ark. .......................................... 173

Water from near Denver, Colo...................................__.... 174

Water from Matilija Hot Springs, California....-.-...._ ........-........ 174

ILLUSTRATIONS.

Pace.

FiG. 1. Section showing association of gonthitc and quartz................... 24

'2. Section showing association of gcnthito and serpentine.............. 24

3. Section showing association of gcnlhite and serpentine...... ........ 24

4. Apparatus for determination of water..................... .......... 80

5. The Rockwood meteorite...........:................................ 10:5

6. Section of Rockwood meteorite ...................................... 104

7. The Fayctte County, Texas, meteorite............ .................... 109

8. Vein in Fayotte Comity meteorite...................:............... Ill

9. Portion of above vein highly niagu ificd.............................. 113

PREFACE.

The present bulletin, like its predecessors numbered 9, 27, 42, and 

55, contains the results of work completed in the Division of Chemistry 

and Physics during- one fiscal year. Part of the investigations reported were begun in previous years ; and other researches which are 

now under way are reserved for future publication. Still other work 

has appeared, or will appear, in separate bulletins'; so that this issue 

represents only a part of the results obtained during the year which it 

covers.

F. W. CLARKE,

Chief Chemist.

ll

WORK DONE IN THE DIVISION OF CHEMISTRY AND 

PHYSICS IN 1887-88.

THE CHEMICAL STRUCTURE OF THE NATURAL SILICATES.

BY F, W. CLARKE.

In any attempt to discuss the chemical structure of the inorganic silicates we are met at the outset, by difficulties which are partly real 

and partly imaginary. On the one hand we have to deal entirely with 

non-volatile solids, of which, because of their fixedness, we can not certainly ascertain the true molecular weights. They are, furthermore, 

insoluble and, chemically speaking, non-plastic; that is, they yield but 

stubbornly to reagents, so that the changes of which they are structurally capable can rarely be studied in the laboratory. These difficulties . 

are very real. On the other hand, most of the definite silicates are 

natural minerals, and as such are commonly supposed to have a bewildering complexity of constitution. This difficulty is only apparent, not 

real, and is due to several causes. First, few mineral species occur in 

a state of even approximate chemical purity; and secondly, many of 

them, being isomorphous, crystallize together to form seemingly homogeneous bodies to which rational formulae can hardly be assigned. 

Impurities, indefinite crystalline mixtures, and defective analyses account for many apparent complications. Eliminate from any group of 

natural silicates these disturbing conditions, and we shall find in every 

case a simplicity of composition far removed from the complexity which 

is popularly assumed. Even on theoretical grounds we should expect 

simplicity of structure. The mineral silicates are, as a rule, exceedingly stable compounds, while complex molecules are relatively unstable. They are formed in nature under conditions of high temperature, or are deposited from solutions in which many reactions are 

simultaneously possible: circumstances that are strongly adverse to 

any great complications of structure. Finally, they are quite limited in 

number, only a few hundred at most being known; whereas, if complexity were the rule among them, slight variations in origin would produce great variations in character and millions of different minerals

13
14: WASHINGTON LABORATORY. [HULL. GO.

would be generated. That few substitutions occur is presumptive evidence that only few are possible, and hence simplicity of-constitution 

is to be inferred. In fact, we find the same small range of mineral species occurring under the same associations in thousands of widely separated localities, a few typical forms containing a few of the commonest metals being almost universally distributed. The longer the 

evidence is considered the more overwhelming the argument for simple silicate structures becomes. "

Suppose now that for any given silicate the empirical composition 

has been ascertained, how can its chemical structure be determined ? 

We can not measure its vapor density and so deduce its molecular 

weight; but the problem is not therefore necessarily hopeless. Several 

lines of available evidence are open. In some cases the compound may 

be synthetically reproduced in the laboratory, a kind of mineralogical 

investigation in which rapid progress is now being made. Again, the 

constant association of the species with certain others sheds light upon 

its genesis, and still ofteuer its alterations in nature furnish important 

details. An alteration product, despised by the crystallographer, is 

really a record of chemical change, and such products may be of the 

highest scientific interest. lu a few researches they have been produced artificially by reactions which were prolonged for months at a 

time, and so a mass of evidence is slowly accumulating, strictly analogous in kind to that which the organic chemist chiefly depends upon for 

ascertaining the structure of a hydrocarbon. All these lines of evidence are legitimate, and all converge towards truly scientific conclusions. We know that certain silicates originated together, and that 

each, alters in certain definite ways; and from these facts we may draw 

perfectly fair inferences as to chemical structure and deduce rational 

formulae which shall give fuller expression to our knowledge. The evidence for such formulas is less perfect than that at the command of the 

carbon chemist, but it is none the less substantial so far as it goes. It 

is, furthermore, cumulative.

About three years ago, while I was working tentatively at the problem now under discussion, I received for examination certain specimens 

of topaz which were deeply altered upon their surfaces. Upon investigation the alteration product proved to be a variety of muscovite, and a 

study of the empirical formulae of thetwo minerals revealed an unexpected 

relation bet ween them. Further study brought out more extended relations connecting them with several other silicates, and by a natural series. 

of steps I was led to adopt as a working hypothesis the supposition that 

double salts might be regarded as substitution derivatives of normal 

salts. This hypothesis, since then steadily applied to the discussion of 

the silicates, appears to be supported by a weighty mass of evidence, 

and it leads to the development of a series of structural formulae which 

satisfy many conditions. They express and interpret known relations, 

lead to the detection of others, and point out suggestive and profitable
CLABKB.] STRUCTURE OF THE NATURAL SILICATES. 15

lines of research. By these tests any hypothesis must stand or fall, 

and one which, meeting them successfully, has at the same time philosophical significance, may be fairly looked upon as valid.

That the great majority of the natural silicates are double salts need 

hardly be stated, and that a very great number of them contain aluminum is also a commonplace of chemistry. Of the latter some are orthosilicates, and some are meta-cotnpounds; and the problem is to show 

how each series maybe derived from its corresponding normal salt. 

As the orthosilicates are the most important, we may begin with their 

consideration. They represent the maximum of complication and offer 

the greatest difficulties.

Fortunately, the orthosilicate of aluminum Al4(SiO4 ) 3, occurs in nature as the mineral xenolite. This species, which is now well established, was long thought to be an impure variety of fibrolite, Al2SiO5 ; 

and iii their optical properties the two are apparently identical. Fibralite bears the closest of relations to its isonier, andalusite; and to the 

latter, topaz, Al2St04F2, is crystallographically akin. Topaz, as I have 

already stated, alters into inuscovite, Al3KH2 (SiO4 )3 ; and so also does 

eucryptite, AlLiSi04 . To these compounds we may add paragon!te, 

which is merely a sodium mica, and we have at least six silicates, including the normal salt, which are all evidently related to each other. 

That their empirical formulae show little or no connection is due to the 

fact that they do not represent true molecular weights, and on this 

point our fundamental hypothesis gives us a key to the problem. If 

we triple the formulae given for tibrolite, topaz, and eucryptite, the 

substitution theory which I have suggested at once becomes applicable, 

and the derivation of all the others from xenolite is easy. The following structures will make this conception clear:

Si04 -Al 

Al Si04 EAl

Si04 EAl 

Xenolito.

Si04 E(A10)3 

Al Si04 = Al

SiO., =Al 

Fibrolite.

Si04 = (A1F2 )3 

Al SlC-4 E Al 

SiO, E Al

Topaz.

SiO4 EKH2

/

Al Si04 EAl

\

Si04 EAl

Muscovite.

Si04 NaHs

/

Al SiO^Al

\gjo _ AI

Paragonite.

SiO., E Li 3

/

Al SiO4 = Al

\

Eucryptite.

In the second of these formulae the univalent group Al = O is assumed, and in the third we have the corresponding group Al = F2 . 

I think no chemist will regard these assumptions as strained.

Now the foregoing symbols all represent a series of salts derived 

from the first one by various substitutions of a single aluminum atom.
16 v WASHINGTON LABORATOEY. IHULI..OO.

But further replacements are theoretically possible, and the following 

minerals seem to illustrate them :

SiO4 =(A10)» Si04 :

Al Si04 E(AlO)3 AlSi04 EAl SiO.,EAl

Dumortierito. Grossularito.

Si04 E ) 

/ >Ca;,

I Si04 E )

Si04 E Call Si04 E NaH2

/ /

Al SiO4 ECaH Al Si04 ENaH2

Si04 EAl Si04 EAl 

Prehnite. Natrolite.

Dumortierite, which has been little studied, appears to be related to 

fibrolite, and the formulae exhibit a relation. Grossularite, the lime 

alumina garnet, is a common associate of muscovite, a fact which lends 

verisimilitude to the formulae given above. The other two formulae 

represent the known composition of prehnite and natrolite, but whether 

they indicate any deeper relations is not yet proven. They do, however, 

suggest lines of investigation, and so far fulfill a useful purpose. If 

they are true, prehnite should be derivable from garnet, and garnet 

and muscovite ought to be mutually derivable from each other. That 

garnets do alter into micas is already well known, although the exact 

character of the change is undetermined, and the micas involved in the 

reaction appear to be more complex than muscovite.

Returning now to fibrolite, we find that it is a mineral which is liable 

to alter through a process of hydration. Sonic of its alteration products have been described as species, notably under the names worthite 

and westauite, the latter being apparently the final product. Certain 

other species of the same group frequently undergo a sort of degradation into clays, which, unfortunately, are often too impure to admit of 

precise formulation. Still, of the several clays which are certainly 

definite, two seern to fall into series with fibrolite and westanite, as the 

following structures show:

Si04 = (A10)3 OH

Al SiO4'=Al Al SiO4 = Al

Si04 EAl ' Si04 EAl

Fibrolite. Westanite.

OH OH

Al Si04 EH3 Al Si04 EH3

Si04 EAl SiO4 =H3 . 

Kaolinite. Montmorillonite.

Now, suggestive as these formulae are, they represent only a selection 

out of a much larger number, all of which seem to follow essentially
CLAUKK.] STRUCTURE OF THE NATURAL SILICATES. 17

the same structural rule. If the case rested here it would still be a 

strong one, but it becomes even stronger wheu we study some of the 

more complex orthosilicates, and some of tlie silicates containing other 

inorganic acids. In most of the foregoing instances we have one 

aluminum atom linked with three of the orthosilicic groups, making 

a sort of fundamental nucleus to which the other atoms of each molecule are attached. But in many cases we seem to have a semipolymerisation of that nucleus which results in the elimination of one of 

the silicas, leaving a new group of atoms which may be represented us 

follows :

Si04 E

Al S10..E 

Si04 -

Al-Si04 = 

Si04 =

This group, saturated by various bases, seems to exist in many natural 

silicates, notably among the iron and magnesiau micas; and from it 

certain mixed salts, like sodalite and nosean, may be represented as 

derived. Thus, to cite a few examples, we may write:

Al SiO4 = FeH Al SiO., = Al

Si04 = K« Si04 Naa

Al SiO., E FoH Al SiO., E Al

Si04 E FeH Cl

Annite. Sodalito.

Al Si04 = Al Al Si04 IE Al

\ \ *

Si04 Na* , Si04 = Na2

Al Si04 E Al Al SiO4 EE Al

SO4 Na S Na. 

Nosoan. Ultrauiuriuo.

. The last of these four formulae is purely hypothetical and rests upon 

the recognized mineralogical analogies between lapis lazuli and nosean. 

It is, however, a formula which should be capable of synthetic verification, for ultramarine, itself a product of synthesis, yields many derivatives, the formation of which can be systematically studied. Possi 

bly the lines of research followed by Lemberg, in his work on the 

alterations of elacolite, may be fitly applied to the investigation of lapis 

lazuli. As for anuite, I have discussed its relations, together with those 

of the lithia micas, in a previous paper, 1 in which I have also given some

1 Aiuer. Jouru. Sci., Nov., 1880. ' 

BULL. 60 2
18 WASHINGTON LABORATORY. [HULL. GO.

suggestions concerning the part played by fluorine in lepidolite,cryophyllite,audphlogopite. Sodalite and uosean were considered in a still earlier 

paper,1 in connection with cancrinite, nephelite, and other species. It 

is hardly necessary to repeat either discussion here.

Passing now to the metasilicates, we find ourselves, as regards the aluminous salts, at some disadvantage. The normal compound, Al2 (Si03 )3. 

is not known to exist by itself in nature, although certain of its 

derivatives are common. Its formula, however, may 'be written in two 

ways, as follows, and to one of these types some of the double aluminous metasilicates should conform :

i. M.

x,Si03 SiO3

/ \ Al-SiOs-Al.

Which of the two is best sustained by evidence ?

To answer this question we may appeal to several well-known minerals, such as spodumeue AlLi(Si03 )2 , jadeite, AlNa(SiO3 )2 , leucite, 

AlK(SiO3 )2 , and pyrophyllite, AlH(SiO3) 2. All of these can be generalized under one formula, thus :

Si03

XSiO3 R,

which is directly derivable from normal salt No. 1, and is not derivable 

from No. 2. Furthermore, kyanite, an isouier of fibrolite, Al2SiO5 , is 

regarded by Groth and others as a basic metasilicate, for reasons 

which need not be reconsidered here. As such its formula is 

Al2 (SiO3 )O2, which may be derived from either of the formulae for the 

normal compound. But pyrophyllite often occurs as the gaugue of kyanite, which suggests a genetic relation between the two, and so makes 

it highly probable that the latter mineral should be written

Si03

S

Al

\

A/

^

O

rather than as a derivative of the second formula for Al2 (SiO3 )3 . Formula No. 1, then, is the more probable formula for aluminum metasilicate. Two isomers may be possible, bub the evidence so far favors only 

one compound.

'Amer. Journ. Sci., April, 1080
CLABKB.1 STRUCTURE OF THE NATURAL SILICATES. 19

In addition to orthosilicic and nietasilicic acids, at least two other 

silicic acids correspond to known salts. These are the compounds 

H2Si 2O5 and H4Si3O8 . Still more are possible, but it is not necessary to 

assume them in order to account for known minerals. Derived from 

H2Si2O5 we have a few species, notably petalite, AlLi(Si2O5)2 , which is 

the equivalent of spodumene in structure. The other acid, H4 !3i 3 l)8, is 

represented only by .the species albite and orthoclase, ALN"aSi 3Oo and 

AlKSi3O8 respectively. If we triple these formuliB we have structures 

quite analogous to the orthosilicates, in which the normal aluminum 

salt Al4 (Si3O8 ) 3 is the starting point for derivation. Now it is almost 

universally believed, in accordance with the views of Sterry Hunt and 

Tscherraak, that the triclinic feldspars consist of various mixtures between albite and anorthite as two extremes. If our fundamental hypothesis is true, each of these minerals is derived by substitution from a 

normal salt, and the formulse so deduced become strikingly suggestive:

SiO.,= Si 3 08 ^

Al SiO.,~ Al Al Si 3 08 ~ Al

X i - X i " -

Anorthite is the lime salt corresponding to the first formula, and 

albite is the soda salt corresponding to the second. Another comparison 

is even more striking. The four silicates most frequently associated 

with each other in granite veins are muscovite, garnet, albite or orthoclase, and tourmaline. Tourmaline, according to the analyses made by 

Mr. Riggs in the laboratory of the CTuited States Geological Survey, is 

always represented by the general formula R'9B02 (SiO4 )2 , in which at 

least the equivalent of R'3 is present as aluminum. This gives us the 

following quartette of formulae:

Si04 -HKH3 Si04 

Al SiO.,_Al Al SiO.,

SiO4 -::Al SiO, -JAl 

Muscovite. Giimot.

BO, . . 

Al SKV^Ba Al 8i3 08 ;_: Al

SiO, R3 Si 30«;:Al 

Tournialiuo. Ortkocliiso.

The suggestiveness of these symbols can hardly be questioned. All 

four are covered by the one general hypothesis ; and tourmaline, furthermore, is known to alter into muscovite.

Leaving the aluminous salts, the other silicates present few structural 

difficulties. Isomorphous mixtures become perhaps more common, but 

when they are resolved into their constituents relatively simple compounds are found, The commoner bivalent metals form both ortho- and
20 WASHINGTON LABORATORY. f BULL. 60.

inetasilicates, and to them the substitution hypothesis, as a rule, easily 

applies. Only iu the metasilicate series do we find notable difficulties, 

and they may be avoided by the assumption of polymeric molecules. 

Thus, instead of JR/'SiO3 we should write B"2 (SiO3 )2, in which one atom 

of K" becomes replaceable. This conception is by no means new, and 

is indeed quite commonly in use; but I may be permitted to cite one 

item of evidence in its favor. When solutions of calcium chloride and 

sodium metasilicate are mixed, a white precipitate of calcium metasilicate is thrown down. This reaction I have studied under various 

conditions of temperature and concentration, and I find that when the 

precipitated salt is carefully dried over sulphuric acid it has the composition 2CaSiO3 .5H2O. That is, the double molecule Ca2Si2O6 is required in order to avoid a formula containing a half molecule of water. 

By itself this fact is not of weighty importance, but it counts for something in confirmation of the prevalent views.

Concerning mixed silicate molecules, partly ortho- and partly metacompounds, I have nothing at present to say. Such silicates undoubtedly exist, as well as aluminous silicates derived from normal salts of 

magnesia or lime. Nor do I venture to assert that all known silicates 

are as yet interpretable by simple structural means. There are many 

outstanding cases which still seem very obscure, but which I confidently 

expect will be cleared up iu time. The micas, chlorites, and scapolites 

especially need a great deal of further study. Various theories have 

been proposed to account for the composition of these groups, but not 

one is absolutely conclusive and satisfactory. The new method of discussion which I have proposed is yet to be fully applied to these minerals 

but a wider knowledge of their variations is essential to its complete 

application. Whether the method shall be finally established as valid 

remains to be seen, but its results so far at least entitle it to respectful 

consideration. As a working hypothesis the substitution theory has 

value, even though it should be ultimately overthrown.

In conclusion, there is one question to be considered. With the silicates the supposition that double salts are substitution derivatives of 

normal salts appears to work exceedingly well. But how about double 

salts in general *? With such compounds as the sulphates, chroniates, 

tartrates, oxalates, etc., there seem to be few difficulties; but with the 

double haloids, acetates, formates, etc., the case is not so clear. Their 

explanation is troublesome, at least iu accordance with current views 

concerning the valency of their acid radicles; but those views are not 

absolutely incapable of modification. There may be exceptions to the 

general hypothesis of derivation, but chemists are not likely to be satisfied with partial theories, and all double salts ought to come under one 

common law. Toward that ultimate purpose the present paper tends, 

ev<-«> though the road which it opens may not reach the final goal.
SOME NICKEL ORES FROM OREGON.

By F. W. CLARKE.

In or about the year 1881 extensive deposits of nickel silicates were 

discovered in Douglas County, Oregon. In appearance the ores are 

identical with the so-called "garuierite" and "noumeaite" of New 

Caledonia, and many specimens bearing these names have found their 

way into collections of minerals. At present the deposits at Kiddle, 

Oregon, are being worked by the Oregon Nickel Company, and, through 

the kindness of Mr. Will Q. Brown, an admirable series of the ores was 

recently sent to the United States Geological Survey for investigation. 

According to Mr. Brown all the deposits lie at or near the surface, in 

beds from 4 to 30 feet thick. Mining is carried on through open cuts 

or quarries, and no second bed has ever been found underlying the first.

The specimens at ray disposal represent a wide range of appearances. 

They include samples of the country rock and of the associated chromite, 

and the nickel silicates themselves vary much in color and texture. 

The finest specimens are bright apple-green and quite compact, and 

from this they range through duller shades into masses of distinctly 

earthy texture. Most of them are intermixed with oxides of iron and 

with quartz; and even the purest mineral like the garnierite of New 

Caledonia, is seamed with thin sheets of chalcedony. All of the nickel 

bearing samples are much decomposed; and one particularly beautiful 

specimen is distinctly a conglomerate or breccia, having nodules of the 

green ore imbedded in it side by side with pebbles and fragments of 

other material. Like all the nickel silicates which have been so far 

observed in nature, these ores are unmistakably products of alteration, 

and the problem of their genesis is somewhat interesting. For comparison with them I had a suite of the New Caledonia minerals, received 

from Professor Liversidge, and a large series of the genthites from 

Webster, N. C., collected by Mr. W. S. Yeates. All three localities have 

much in common, and the three sets of specimens point clearly to one 

conclusion, which will be stated farther on after the evidence for it has 

been presented.

In composition the nickel silicates from any locality vary widely; 

for the earthy nature of the material renders it impossible to secure 

anything like a homogeneous substance for analysis. The purest

21
WASHINGTON LABORATORY. [BULL. 60.

specimen of the Riddle ore was dark apple-green, compact, and 

amorphous; but so permeated with films ®f silica that a definite mineral 

could not be isolated. With the best material obtainable 1 secured the 

following results, which I give side by side with two published anal. 

yses by Hood, 1 in order to show the variations.

Loss on ignition ...... 

Al203 + Foa03 ........

Si02 ..................

MgO. .................

NiO ..................

Clarkc.

8.87)

6.995 

1.18

44. 73

10.50

27.57

99.90

Hood.

6. 63

1.38

48.21

19.90

23. 88

100. 00

Hood.

7.00 

1.33

40.55

21.70

29. 66

100. 24

Neither lime, sulphates, chromium nor cobalt could be detected. 

Like the New Caledouia garnierite, the fragments of this silicate fell 

to pieces when immersed in water.

Of the New Caledonia silicates many analyses have been published, 

notably by Liversidge and Leibius, Typke, Damour, Gamier, and Ulrich, 

and they vary between widely separated extremes. Not only are there 

the variations due to mutual replacements of nickel and magnesia, 

with a range in the percentage of NiO from 0.24 to 45.15 per cent, but 

there are also great differences in silica and in hydratiou. It is therefore impossible to say whether we have to deal with one nickel salt, 

varying only in its impurities, or with several compounds, although 

the general similarity of the material from different localities renders 

the former supposition the more probable. According to Ulrich2 the 

nouineaite and garnierite consist of a soapstone-like base, with a 

hydroxide or silicate of nickel distributed through it in veins and 

patches; while JDes Cloizeaux3 regards nouineaite as a maguesian 

hydrosilicate impregnated with nickel oxide. The latter view, however, 

is hardly probable, especially when we consider the origin of the minerals ; and Typke4 has cited evidence against it. The prevalent opinion, 

that we have to deal with one or more definite hydrosilicates of nickel, 

is best sustained by careful comparative study of the specimens, even 

though the salts may not be obtained pure or positively formulated. 

The reciprocal variation of nickel and magnesia in more than twenty 

published analyses excludes from further consideration the idea that 

the nickel is present to any great extent as hydroxide. For temporary 

convenience we may use the well-recognized name "genthite" generically, and apply it to all the nickel silicates from the above-named 

localities.

'Mineral Resources of the United States, 1883. 

s Amer. Joiirn. Sci., Third series, vol. 11, p. 235. 

a Bull. Soc. Miu., 1, 29. 

'Chein. News, 34. 193.
CLABKE.] SOME NICKEL ORES FROM OREGON. 23

Of the "country rock" surrounding the Oregon, bods one large, clean, 

fresh specimen was received. This was subjected to analysis, and also, 

through the kindness of Mr. J. S. Diller, to careful microscopic study. 

The olivine separated from it by Mr. Diller was analyzed also, although 

the material was not absolutely free from enstatite and chrornite, aud 

both analyses are here presented together.

SiOa ..................

AlzOj.................

Crs03 ................

reaOs....... ..........

FoO ..................

NiO...... ....... ......

MnO. .................

CaO ..................

MgO...... ............

liock.

4. 41

41. «

.04

.76

0 25

.10

.55

43. 74

09.80

Olivino.

.57

42.81

.79

2.01

7.20

.26

45. 12

99.30

It will at once be seen from these data that the rock contains nickel, 

and that the olivine separated from it contains even a larger proportion. 

This fact-suggests a probable source of derivation for the nickel in the 

altered beds of ore, and this view is maintained by the microscopic investigation. Concerning the latter, Mr. Diller reports as follows, discussing both the rock and the genthite:

The high specific gravity and dark yellowish green color of the country rock with 

which the genthite is associated at Riddle, Oregon, at ouco suggests that it belongs 

to the peridot!bes, and such it is proved to be by investigation. It is aholocrystalline 

granular rock, composed essentially of olivine and enstatite with a small percentage of accessory chromite and magnetite. The olivine predominates, so that the 

enstatite forms less than one-third of the mass. Both of these minerals are clear and 

colorless, but may be readily distinguished by their cleavage aud optical properties. 

They are allotriomorphic, i. e. not bounded by crystallographic planes, and do not 

contain prominent inclusions, excepting a few grains of chromite and magnetite aud 

fine ferritic dust. Notwithstanding the comparatively fresh condition of the rock, to 

which, according to Wadsworth, the name Saxonite may bo applied, it is completely 

permeated by a multitude of cracks filled with serpentine resulting from alteration. 

Quartz also results from the motasoinatic changes in the saxouito, aud wherever the 

genthite occurs it is always associated with either quartz or serpentine.

The genthite from Oregon varies in color from green to pale apple or yellowish 

green in reflected light, and is compact with a faint suggestion of fine granular structure. Generally it is dull, but where most compact and traversed by a series of 

minute fissures or seams of quartz it has a decidedly waxy luster. Under the microscope it usually appears to be an aggregation of irregular grains which have in transmitted light a pale yellowish green to coffee-brown color, and a peculiarly clouded 

waxy aspect. Where the grains are very thin the genthite may bo said to be transparent aud isotropic, but the majority of them are only translucent. In the narrow 

seam of genthite lying between seams of quartz the former is indistinctly fibrous 

and feebly double refracting ; but its system of crystallization could not bo definitely 

determined. In small veins it is free from grains of other minerals, but elsewhere it
24 WASHINGTON LABORATOEY. [HULL. 60.

is very intimately commingled with quartz. The relation of the two minerals is 

shown in the accompanying Fig. 1, in which the shaded portions (3) are genthite,

FIG. 1.-Genthite and quartz.

and the clear ones (4) are quartz. The commingling of the two minerals is so intimate as to make it evident that both were deposited from solution in circulating waters. Veinlets of quartz are frequently found cutting across those of geuthite, and in 

general it appears to be true that the latter mineral was laid down first, although it 

is probable that both were precipitated at about the same time. Although the purest 

genthite is to be found with quartz, the mineral is more commonly associated with serpentine ; and this relation is a most important one in its gonetic significance. The accompanying Fig. 2 represents the edge of one of the larger veins of geuthito (3),

FIG. 2. Genthite and serpentine.

with numerous veinlets or fissures extending out into the serpentine (2). The tributaries are abundant on both sides of the vein. Fig. 3 shows a vein of genthite (3) in

Fia. 3. Genthite find serpentine with oxide of iron.

the serpentine (2), which envelopes small masses of residuary oxide of iron (1), left 

by the decomposing olivine. The area represented is only 0.64 of a millimeter in
cunKR.1 SOME NICKEL ORES l^ROM OREGON. 25

diameter and contains no oiiviuo ; but loss than half a millimeter from the boundary 

of the vein much oliviue still remains, although deeply coated with oxide of iron and 

serpentine. The branching starting from the vein of geuthite, together with the 

manner in which the arms gradually fade away into the serpentine at once suggests 

the source from whic"h the genthite has been drawn. The geuthite and serpentine 

are thoroughly intermingled, but the former is generally present in such small quantities as to be overlooked unless it is the object of special research. It occurs in the 

serpentine directly connected with the grains of oiivino from which the serpentine 

has been derived, and there is every reason to believe that the genthite came from 

the same source.

Ill order to secure completer confirmation of the idea that the nickel 

of the greater silicate deposits is derived from the alteration of nickeliferous olivine, Mr. Diller, at my request, also examined specimens from 

Webster, N. C., and from New Caledonia. Concerning the Webster 

genthite Mr. Diller reports that 

It is almost identical with that from Oregon, excepting that it is not so thoroughly

intermingled with quartz. The relation of the genthite to the serpentine and the 

olivine at the Webster locality is exactly the same as at Riddle. The rock at Webster differs slightly from that at Riddle in containing a smaller proportion of enstatite, and belongs to the peridotites to which the name "dunyte" has been applied.

He also finds the New Caledonia mineral to be identical with genthite 

in its physical properties, and says:

Under the microscope it varies from pale yellowish green to light coffee-brown, 

and is either completely isotropic or exhibits only faint aggregate polarization. Like 

the genthite of Oregon it is deposited in layers and cavities thoroughly intermingled 

with quartz, and in the same thin section may be seen serpentine with traces of oiivino and eustatite so disposed as to clearly indicate that the serpentine, noumcaite, 

and other secondary products have resulted from the alteration of peridotite.

This observation confirms the earlier one of Des Cloizeaux (loc. cit.) 

who stated that tfie noumeaite was imbedded in a serpentine rock 

which appeared to be derived from olivine, and which contained crystals of the latter mineral plentifully disseminated through it. A similar suggestion is made by Mr. H. J. Biddle, 1 who regards the nickel of 

the Webster deposits as an original constituent of the olivine rock, and 

cites an experiment of Mr. Gr. B. Hanna, who found 0.15 per cent, of 

nickel oxide in a chrysolite from Waynesville, N. C.

So far, the case appears to be clearly and conclusively settled as to 

the origin of the nickel silicates under discussion. Nickel is almost 

always present in small quantities in olivines, and T. Sterry Hunt, in 

reporting genthite from Michipicoten Island2 calls attention to the fact 

that the metal is rarely absent from the serpentines, steatites, diallages, 

and actinolites of the Quebec group. Nevertheless, one other possible 

source of nickel must be noticed. Both, 3 in speaking of the genthite 

from the chrome mines of Pennsylvania, attributes it to the alteration 

of nickeliferous chromite; and the almost universal association of the

1 Mineral Resources of the United States, 186(>. 

2 Report Geol. Survey of Canada, 1863, p. £>U(i. 

3 Allgem. und Chern. Geologic, vol. i, p. 225, 1879.
26 WASHINGTON LABORATORY. ,lBm>i,60.

latter mineral with genthite, renders the view deserving of attention. 

But it must be remembered that chromite alters with great difficulty, 

while olivine decomposes with extreme ease; and moreover the genthite from Oregon contained no chromium, although that metal was 

diligently sought for. Furthermore, Mr. Diller examined some of the 

chromite from the Eiddle mines, and found that although it was penetrated by crevices filled with secondary minerals containing genthite, 

the chromite itself showed no evidence of alteration.

Concerning the other silicates of nickel, described under the names 

of pimelite, alipite, conarite, rottisite, refdanskite, etc., little need here 

be said.. Some of them are probably similar in origin to the better 

known genthite, although the conarite and rottisite, which contain 

small amounts of sulphur and arsenic, probably came from nickeliferous 

sulphides. For the other minerals above named there is too little 

evidence upon record to warrant any serious attempt at discussion.1

1 A full discussion of tbe nickel silicates from Now Caledonia maybe found in" 

Professor Liversidge's work, entitled "The Minerals of New South Wales, etc.," published by Triibner &Co., in 1888.
NATURAL SODA; ITS OCCURRENCE AND UTILIZATION.

By THOMAS MARE AN CHATARD.

The enormous consumption of carbonate of sodium in consequence 

of the great variety of uses to which it is applied in manufactures and 

in daily life, has made its artificial production one of the most thoroughly 

studied branches of chemical technology. The valuable work of Lunge, 1 

which is the standard authority on this subject, gives the history of this 

industry from its slender beginnings to its present vast expansion and 

shows what energy, ability and capital have been expended in the 

course of its development.

Of the many methods proposed for the manufacture of carbonate of 

sodium, but two, the Le Blanc and the ammonia processes, have fulfilled 

practical requirements and are, at present, contending together for the 

mastery of the field. So sharp is this competition that in many cases 

the Le Blanc process can live only through the demand for its byproducts the soda obtained yielding little or no profit and if the 

problem of the utilizatio n of the chlorine in the waste liquors of the 

ammonia process be ever economically solved, the former method must 

soon become a. thing of the past.

Before the discovery of the Le Blanc process the only sources of carbonate of sodium were barilla, or the ashes of certain plants, and a 

small amount of "troua" or "natural soda" obtained from Hungary 

and a few African localities. The principal use of soda is in the manufacture of hard soaps, which, in default of this alkali, can be made by 

adding common salt to the "soft soap" produced by saponification of 

fats by means of the potash-lye obtained by the leaching of wood ashes. 

The addition of salt causes the soap to curdle, the sodium of the salt 

replacing the potassium of the "soft soap" while the residual liquid 

contains chloride of potassium. Such was the method of soap-making 

followed at that time, but the increasing cost of potash and of barilla 

gave a powerful impulse to the artificial soda manufacture which abroad 

has now become the most important branch of chemical industry.

.'Sulphuric Acid and Alkali, by George Lunge. Ph.D., three vols., London, 1880.

27
28 WASHINGTON LABORATORY. [BULL. GO.

Nature has been bountiful in giving us, within our boundaries, 

sources of soda which await the union of capital and technical skill 

to become valuable producers of national wealth. These sources of 

natural soda are the alkaline lakes and "dry deposits" situated in 

that section of the country lying between the Rocky Mountains and 

the Sierra Nevada, known as the " Great Basin." JVI^auy are well k nown, 

having been described by the various Government expeditious and 

surveys; while some are too weak, too impure, or of too little extent 

to have a prospective value, others promise good results to well-directed 

practical development. To aid this, the present investigation has 

been undertaken by the United States Geological Survey.

This work naturally falls into two divisions the collection and arrangement of previously existing knowledge and a study of the technical questions involved. As the literature of the subject consists of but 

few articles, most of which are to be found only in journals inaccessible 

to those more particularly interested, it has been deemed advisable to 

bring together, in a compact form, the information we possess concerning foreign localities, both as to their nature and the work done in connection with them. In regard to the study of the technology of the 

subject, it must be understood that this has its special difficulties, since 

laboratory experiments on a small scale, no matter how carefully conducted, can rarely reproduce the condition existing in large masses 

of such material, while the influence of the climate is also a very potent 

factor. For these reasons a portion of the work was done in the field, 

and more was contemplated, but unforeseen circumstances have prevented the complete prosecution of this plan, and the results so far obtained are published in order that others may be induced to take up 

the work and develop it on a practical scale.

COMPOSITION.

" Natural soda," so called to distinguish it from the soda produced 

by artificial processes, is the residue obtained by the evaporation of 

alkaline waters, without the aid of artificial heat. It is composed of 

sodium carbonate and bicarbonate, in varying proportions, mixed with 

impurities, mainly sodium chloride and sulphate. In comparing natural sodas from different localities we shall find that they vary widely in 

composition, so that a process of manufacture developed in one locality, 

and yielding there a very pure and cheap product, may fail completely 

when applied without proper modification to the material from another 

place.

The problem to be solved is the economical production of commercial 

sodium carbonate by the appropriate treatment of the natural soda, 

and the means to be employed are, in the main, solution, evaporation 

and fractional crystallization. By fractional crystallization we mean a 

methodical stoppage of the crystallizing process by removal of the remaining solution or " mother liquor " from the " crop " of crystals so far
CHATAUD.] NATURAL SODA. 29

obtained. This "first crop" may be either the desired material in a 

purer condition than it was in the original solution or may consist 

mainly of impurities which we wish to remove.

As the first step in this study it is necessary for us to know the nature and properties of the salts composing natural soda, not only 

when they are pure, but also when in combination with each other, 

since the properties and reactions of each salt are modified by the presence of the others in its solution, and the extent of this influence is 

generally proportionate to the relative amounts of the salts present.

The substances to be considered are, therefore, sodium sulphate, 

chloride, carbonate and bicarbonate, and in. describing them only those 

characteristics which seem to be of interest in this connection will be 

mentioned, since the text-books of chemistry, notably the work of 

Lunge already mentioned, give all needed general information with sufficient fullness.

SODIUM SULPHATE.

Sodium sulphate Na^SC^, or anhydrous sodium sulphate, is found in 

nature as the mineral Thenardite. Combined with ten molecules of 

water of crystallization or Na2SO4 10H2O, it forms the mineral Mirabilite. Both of these minerals, as also the artificial sulphate, are soluble 

in water, and the solution on being evaporated yields, according to the 

temperature and other conditions, either anhydrous salt or salt with 

seven or ten molecules of water of crystallization.

The composition of these salts is as follows:

Na2 0 ........... 

<sn

HsO.. ...........

Anbydroua.

43. 07

100. 00

With 

7H?0.

23.13 

29.85

47.02

100.00

With 

lOHjO

19.26 

24.84

55. Ul

100. 00

Of the two hydrated salts, the one with 10 H2O is generally known as 

crystallized Glauber's salt, and is formed when the solution is evaporated 

under ordinary conditions. It forms large transparent crystals which 

effloresce in the air, falling into a white powder and losing all of the 

water if the'air is sufficiently dry. If, however, the solution is made 

strongly alkaline, by the addition of sodium carbonate, and evaporated 

at ordinary temperature, the crystals then obtained are anhydrous.1 

That the sulphate is under such circumstances anhydrous is also shown 

by the numerous analyses of mixed salts given in this paper, notably those 

on pages 63, 64, as the amount of water there found is insufficient for 

even the salt with one molecule of water of crystallization or Na2SO4 , 

H2O, said by Thoinseu2 to be formed under such conditions.

1 Schulz-Sellack: Jonrn. fiir prakt. Clietn., series 2, vol. 2, p. 459. 

2 Thomsen: Ber. Deutsch. Cliem. Ges., vol. 11, p. 2042.
30 WASHINGTON LABORATORY. IBULL.CO.

The solubility of this salt in water increases with the temperature, 

100 parts of water at 0°(32° F.) dissolving 5.02 parts Na2SO4, while at 

33° 0(91.4° F.), the point of greatest solubility, 50 parts Na2SO4 are dissolved. As different observers give different results it is well to state 

at this point that the solubility of a salt at any given temperature 

depends on whether we take the salt in its anhydrous condition or as 

combined with water of crystallization. The experiments of Loewel1 

show this very clearly for sodium sulphate, and it is also true for 

sodium carbonate. Of course the figures are only true for pure solutions j if other salts are present such as chlorides and carbonates the 

question becomes very complicated. The results obtained by the series 

of experiments on the evaporation of Owens Lake water, to be described 

later, may, however, aid us in forming correct conclusions, but so far we 

can only say that, from a practical point of view, the sodium sulphate 

which is always present to a greater or less extent in all alkaline waters 

and dry deposits is a most unwelcome guest, being of itself comparatively worthless, but by its presence greatly complicating any process 

devised for the extraction of the valuable carbonate. As will be seen 

later it is deposited to some extent with the "first crop" of crystals, even 

when this crop represents but a small portion of the total salts in solution, and, unlike sodium chloride, it has a distinctly deleterious effect 

upon the quality of the product. It must, therefore, be the aim of the 

manufacturer to prevent, or at least to control, its deposition as far as 

practicable, and to attain this result careful and judicious work will be 

necessary.

SODIUM CHLORIDE.

Sodium chloride (NaCl) or " common salt," contains 39.39 per cent, 

sodium and 60.61 per cent, chlorine. It crystallizes in cubes which, 

when the crystallization occurs on the surface of the solution, usually

unite together to build up the well-known " hopper forms." The crystals formed on the bottom are generally incompletely developed, but 

sometimes, and this is particularly the case when certain other salts are 

present, the cubes are perfectly formed, transparent and very bright. 

Other crystal forms and modifications have also been observed.

One hundred parts pure water at 0° 0 (32° F.) dissolve 35.59 parts 

NaGl, aud this solubility is but little increased by a rise in temperature 

as at 30°0 (86° F.), only 36 parts are dissolved. Even at the boiling point 

of the saturated solution 109.7° 0(129.5° F.) it contains but 40.35 parts. 

This peculiarity of solubility is of great importance in the practical 

treatment of the natural soda, since it renders the removal of the 

chloride a comparatively easy matter, the rate of deposition of the salt 

being but little influenced by changes of temperature of the solution.

If deposited with the crop it has no other effect than to reduce the 

percentage of alkali, and therefore the market value of the product,

1 Loewel: Ann. Ckim. et Phys., series 3, vol. 49, p. 32.
CMATAUD.] NATURAL SODA. 31

while its presence in the solution up to a certain proportion appears to 

have a distinctly beneficial action as causing a more complete and satisfactory crystallization of the first crop.

The influence of chloride of sodium on the solubility of carbonate of 

sodium will be shown under the latter head by the tabulated results of 

experiments undertaken to determine it.

SODIUM CARBONATE.

Sodium carbonate or sodium mouocarbonate Na2CO3 is composed of 

Carbonic acid, CO-2 

Molecular 

weight.

62.0

44.0

106.0

Per 

cent.

58.53

41.47

100.00

It is an opaque white salt of a specific gravity of 2.5, and melts at a 

moderate red heat, losing a small portion of its carbonic acid, this loss 

occurring even when the salt is heated and cooled in a stream of dry 

carbonic acid. When fused in a crucible over an ordinary flame the 

loss of weight at a red heat is about six-tenths of 1 per cent.; as the 

heat increases so does the loss, so that at a yellow heat up to 1.75 per 

cent, is lost, but this is regained as the material cools, so that the final 

loss is that at a red heat. If the salt is fused in a current of air or of 

steam, the loss is continual and proportioned to the degree and duration of the heating, experiments giving a loss as high as 2.05 per cent. 1 

A solution of sodium carbonate, if boiled, undergoes a small but continued loss of carbonic acid, and the same loss occurs if the solution is 

placed in a vacuum at ordinary temperatures. (Jacquelain.)

Sodium carbonate dissolves in water with evolution of heat. From 

its solution it crystallizes with 1, 2, 3, 5, 6, 7,10 and 15 molecules of 

water; (1) according to the temperature of the solution, and (2) according to whether the solution, prepared at a boiling heat, in cooling down 

is freely exposed to the air or not.

Of these hydrates the monohydrate (Na2CO3H2O), is found in nature 

as the mineral thermonatrite j " the trihydrated salt (Na2CO3,3H2O), 

according to Schickendantz, is found as an afflorescence in dry places 

of the beds of rivers in the Cordilleras; "2 while the decahydrate 

(Na2CO310H2O), which is the ordinary " crystal soda " of commerce, has 

been found native by Olzewsky.3 The anhydrous carbonate Na2CO3 

also seems to occur, as Kayser4 describes an incrustation which hadevi1 Scheerer: Ann. d. Chemie u Phann., 116, p. 129; Mallard: Ann. de Chimie, series 

4, vol. 28, p. 89 ; Jacqnelain: Ann. de Chimie, series 4, vol. 32, p. 193. 

2 Lunge: Sulphuric Acid and Alkali, vol. 2, p. 277. 

8 Olzewsky: Journal fiir prakt. Chemie, vol. 102, p. 375. 

4 J^ayserj W.: Liebi^'s Jahresbericht der Cheraie? 1850, pp. 759? 821,
32 WASHINGTON LABORATORY. [BULL.60.

deutly been formed by the weathering of the clay slate upon which it 

was found. His analyses of both slate and incrustation are given and 

are interesting as bearing on the problems of rock decomposition and 

as showing one of the ways in which " natural alkali" is produced.

Slato.

SiO*....... ................................................ 49.87

M^O3 ...................................................... 26.41

Fe20:3 ..--.. ........... .................................... 6.95

MusOs ..................................................... 1.21

CaO ....................................................... 2.10

MgO.. ............ ........................................ .87

K20 ................................................'....... 2.96

NaaO......................... .............................. 1.61

Snlphur.............. ...................................... .39

Carbon .................................................... .65

H2O ....................................................... 7.05

BaO.. .............. ........................................ tr.

100. 27 

Incrustation.

Fe.CO:,...................................................... .19

MgCO3 ........................................... .......... 3.32

CaCOii-............................... ..................... 1.81

Na«2C03 ..................................................... 92.07

H^O ................. ...................................... 1.85

99.24

Sodium carbonate is most soluble, according to Mulder, in pure water 

at 32.5° C (90.5° F.), the solution then containing 59 parts Na2CO3 to 

100 parts water, or 37.10 per cent. Hence a solution which has deposited crystals at the boiling point (105° C 221° F.) redissolves them 

while cooling till the temperature sinks below 32.5°C, wbeu recrystallizatiou begins. The solubility varies very greatly with the temperature; thus at 15.5°C (60°F.) the saturated solution contains 14.53 per 

cent, at 31.3°G, 30.04 per cent, and at 32°0, 31.78 per cent.

The presence of sodium sulphate or chloride decreases the amount of 

carbonate which a given amount of water can dissolve, and as the 

nature and extent of this influence is of importance in studying the 

conditions attending the separation of the carbonate from the natural 

deposits and solutions, all of which contain chlorides usually in larger 

proportions than carbonates, three series of experiments have been 

carried out and the results are given in the following table.

In series A the KaCl was dissolved in water and the solution was 

made up to 50cm3 . The Na^COs was then added and the whole shaken 

vigorously, the shaking being repeated at intervals throughout the day. 

The graduated cylinders containing the solutions were allowed to 

stand till the next morning, when the mother liquors were filtered from 

the deposited salts, a perforated crucible with asbestos felt being used 

for this purpose.
CHATABD.] NATURAL SODA. 33

The volume and temperature of tlie filtrate were noted, and 25 cm3 

were taken for the determination of the specific gravity. This portion 

was then diluted with water to 1000 cm3 , and of this dilute solution 

portions of 50cm3 each were taken for the determinations. These portions as well as the 1000 cm3 were in all cases weighed, and the results 

given have been calculated by the factors so found.

In series B the operations were the same, except that the Na2UO3 

was dissolved first, the KaCl being added, in portions of 2.5 grains 

until a permanent deposit was formed, while for series C a saturated 

mother liquor of Na2003,10H2O \Vas employed, 50cni3 being taken for 

each portion.

Sones 

No.

Al....

A2....

A3....

A4-...

A5. . . .

A6....

Bl....

B2....

B3....

B4....

B5 . . . .

01....

C2....

C3....

C4....

C5....

C6....

Iii 50cm5.

Ka Cl.

grains.

Saturated .

12.5

10.0

7.5

5.0

2.5

Nn,C03

graind.

12.5

10,0

7.5

5.0

2.5

Saturated.

.. do......

...do......

...do......

...do ......

...do......

Na2CO3

added.

5.0

10.0

15.0

17.5

20.0

22.5

NaCl

added.

12.5

12.5

15.0

15.0

17.5

none ....

5.0

7.5

10.0

12.5

15.0

°C.

34.0

35.5

32.5

33.0

33.0

33.5

35.0

35.5

32.3

32. 5

33.0

31.3

30. 0

29.5

29.5

30.0

30.0

Sp. G.

1.245

1.294

1.314

1.329

1.340

1.352

1.309 '

1.281

1. 261

1. 237

1. 217

1. 3287

1. 3435

1. 3114

1. 3139

1.3140

1. 3204

Per cent. 

Na2C03.

7.88

7.92

14.83

14.87

18.34

18.36

22.30

22.26

26.36

26.36

29.34

29.31

16.67

16. 66

14.01

13. 99

10.48

10.48

7.14

7.15

3.67

3.68

30.07

30.02

20.59

26.60

19. 41.5

19. 417

18.59

18.60

18.81

18. 84

19.29

19.30

Averago.

7.90

14.85

18.35

22.28

26.36

29. 325

16. 665

14. 00

10.48

7.145

3.675

30. 045

26. 595

19. 416

18. 595

18. 825

19. 295

Per cent. 

Nad.

21.26

21.24

17.29

17.24

14.39

14.37

10.54

10.51

7.01

7.02

3.42

3.42

15.46

15.45

17. 38

17. 39

19. 67

19.65

21. 41.

21.. 43

24.07

24.06

7.20

7.27

13.08

13.08

14.62

14.62

14.48

14.46

14.17

14.15

Average.

21. 125

17. 265

14.38

10. 525

7.015

3.42 .

15. 455

17. 385

19.665

21.42

24. 065

7.205

13.08

14/02

14.47

14.16

Total 

per cent, 

of salts.

29. 150

32. 115

32.73

32. 805

33. 375

32.745

32. 120

31.385

30. 145

28. 565

27. 740

30. 045

33. 860

32. 496

33. 215

33. 395

33. 455

Bull. 60-
34 WASHINGTON LABOEATOKY. [BULL.60.

In each of the experiments here tabulated, with the exception of 01 

there was a considerable deposit of salts consisting of a mixture, in 

varying proportions, of the two salts employed, and the composition of 

the deposit can be calculated by tho difference between the amounts 

originally taken in each case and those in solution.

It will be observed that in the A series the point of equilibrium in 

the percentages of the two salts in solution lies between A2 and A3, 

probably near to the point where equal weights of NaCl and Na2CO3 

would be taken. This is substantially proved by Bl where 12.5 grams 

of each salt were used and the amount of Na3CO3 was 1.21 per cent, 

higher than that of the NaOl.

The salts, however, do not appear to dissolve in proportion to the 

amounts taken, the variations being greatest in the A series where 

the Na2CO3 was added to the solution of the KaCl; whereas in the B 

series, the !Na 2CO3 was first dissolved and the NaCl added the variations are much smaller. We may therefore conclude that if a mixture 

of these two salts is treated with an amount of water insufficient for 

complete solution, the amount of each dissolved will be approximately 

proportionate to the quantity present but that the approximation is not 

very close.

Series 0 shows the effect of the addition of increasing proportions 

of TsTaCl to a saturated solution of Na2CO3 . 50cm3 of this solution at 

31.3° C. weighs 66.3424 grams and contains 19.9224 grams Na2CO3 , or? 

as given in the table, 30.0i5, per cent. The table shows that the addi. 

tion of 7.5 grams NaCl gave the best result, but as some of it remained 

in the deposited Na2CO3 , a less quantity might have been advantageously taken, say 6.64 grams or one-third of the weight of the Na2CO3 

in solution. Had this been done we should probably have had little 

more Na2CO3 left in solution and that deposited would have been purer. 

If the amount of NaCl is increased, the excess as shown, remains uudissolved and the character of the solution suffers but little change. 

The practical bearing of these results will be more apparent when we 

come to that portion of this paper treating of urao or the combination 

of sodium mouocarbonate with sodium bicarbonate.

SODIUM BICARBONATE.

Sodium bicarbonate, NaHOOs, contains 

Per cent. 

Soda, NagO............. .... ................................ 36.94

Carbonic acid, CO; ............ ............................. 52.36

Water, H3O................................................ 10.70

100.00

It is formed by the action of CO2 on 3Ta 2CO3 , hence is always produced 

when a solution of the latter salt is exposed to the air. At the ordinary 

pressure of the atmosphere the reaction is a slow one, but if pure CO2 

at a pressure of 30 pounds to the square inch is used the conversion i§ 

rapid.
CHATAKD.] NATURAL SODA. 35

The salt occurs in monocliuic tables usually combined into crusts. It 

has a somewhat alkaliue taste; if entirely free from Na2CO.-) it does not 

change turmeric, but reddens blue litmus. The best test for its purity, 

according to Hager,is calomel; 0.5 grain calomel mixed with 1 gram 

NaHCO;t and 1.5 gram water and shaken up does not blacken in 24 

hours in the absence of monocarbonate, but in its presence it turns 

more or less gray. In moist air or if moistened with water the salt 

loses CO2 , the more quickly the higher the temperature. Hence if a 

solution of bicarbonate is heated the bicarbonate is gradually destroyed 

and mouocarbouate remains, which has an important bearing upon the 

problem of the economic treatment of natural soda.

NaHCO3 i.s much less soluble in water than Na2CO3 , 100 parts of 

water at 15.5°(60°F) dissolving only 8.9 parts or 8.17 per cent. The 

solubility is much diminished by the presence of sodium chloride or 

sulphate, or a mixture of both. A saturated solution of sodium chloride dissolves hardly any of the salt, a fact of great importance, since 

upon it is based the ammonia process for the manufacture of soda.

SODIUM SESQUICABBONATE.

Sodium sesquicarbonate, Na4H2C3O3 , so called because the old dualistic formula was (NaO)2 (CO2 ) 3 is described in all chemical works which 

treat the subject of the sodium carbonates at all fully. It is said to 

exist in nature as a mineral to which the name trona has been given 

and lias been prepared artificially by E. Hermann 1 and Wiukleiv5 

Other chemists also claim to have obtained it. It represents a combination of one molecule of Na^CO;, with two molecules of NaHCO3 or 

Na2CO3 ,2NaHCO3 , which may also be written Na4 H2C3O9 . My own experiments, which will be given in detail further on, not only failed in reproducing this salt, but also throw considerable doubt upon its actual 

existence as a definite chemical substance, and not as a mixture of the 

two carbonates accidentally formed in these proportions.

There is, however, a very definite combination of the two carbonates, 

which occurs, as will be shown, widely distributed in nature and which 

bears the mineral name urao. This salt is composed of one molecule 

of sodium monocarbonate and one of sodium bicarbonate, plus two 

molecules of water of crystallization, or Na2OO3 , ]SaHCO3 +2H2O, or 

Na3HG2Oc, 2H2O. It is very easily produced artificially, in a well crystallized condition, and is most important in this connection, since by its 

chemical behavior it gives the key to a rational economic process whereby the natural sodas can be made available for use in the arts.

For this reason it will be made the subject of a special section of this 

paper, but before taking it up we will briefly consider the principal localities of natural soda throughout the world and the character of the 

salts produced by them. In this manner a better idea of the extent

1 E. Hermann: Jour, fiir prakt. Chemie, vol. 26, p. 312. 

8 Winkler; Bacliner's Report, far Pliarm., vol. 48, p. 215.
36 WASHINGTON LABORATORY. [BULL.60.

and difficulty of the problem can be obtained, while a mass of matter 

at present scattered through the various journals is brought together 

for comparison.

LOCALITIES AND MODE OF OCCURRENCE.

As a dry climate is the prime factor for the formation of deposits of 

natural soda, or of concentrated waters heavily charged with it, and as 

such climatic conditions exist in many parts of the world, there are numerous places where this material has been found or may reasonably 

be looked for. A complete list of these occurrences is not available, 

nor would it have any special value, and in speaking of the foreign localities only those will bo described where the material is being utilized 

or where the local conditions are of interest for comparison with our 

home sources of supply.

HUNGARY.

In Hungary natural soda is found in many places, especially near the 

town of Szeged in. 1 It occurs as an efflorescence on the surface of moist 

places, the snow-white crust often extending for miles. The crude soda 

or "szekso" is collected by scraping the surface, the best time for this 

operation being the early morning before sunrise, particularly in the 

spring and when much dew has formed, as the material collected during 

the day is considered to be poorer in salts. As the crust is thin and 

much of the soil is gathered with it, the product is a grayish white 

earth; this is sold to the refiners, whose only test for its value was, at 

the date of the description, the sharpness of the taste. Moser 2 gives 

the following analysis of the szekso as gathered:

Soda, Na»0 ............^ ................ .................... 8.03

Potash,K,0................................................. 3.12

Lime, CaO. ................................................ 2.72

Magnesia, MgO ............................................. Trace.

Alumina, AlaO:). ............................................ 2.33

Sulphuric acid, S03 ......................................... 3. 48

Silica, Si02 .................................. .............. 1.04

Water, H2O ................................................ 15.50

lusoluble (sand, etc.). .... .................................. 54.99

Carbonic acid, C02 .... ...................................... 8.79

100.00

Iii the refineries the earth is leached until the soda taste is no longer 

perceptible, giving a dark-brown solution containing sodium carbonate, 

sulphate, and chloride; this is evaporated to dryness and calcined, the 

mass being ultimately heated to complete fusion, and, when partly cooled, 

drawn from the furnace. The product when cold is broken up and sent 

to market.

1 Wcruer: A. Jour. f. pr.ikt. Chemie, vol. 13, 1838, p. 127. 

-2 Moser: Liebig's J&hres.bericlit, 1859, p. 812,
CHATAHD.] NATURAL SODA. 37

Schapringcr1 gives the following analyses of two samples of this soda. 

No. 1 is said to have been made by evaporating the teachings and drying the product in the air, while No. 2 is said to have been obtained by 

calcining No. 1:

Soclinm carbonate, N.iaCOs.-..

Sodium aulphate, Na^SOj ..... 

Calcium carbonate CaCOa .....

W'ltcr

No. 1.

28.87 

31.00

.rs

.39

39. 04

.10

100. 00

No. 2.

40. 25 

53.93

.45 

l.f.4 

1.45

2.09

.29

100.00

It is difficult to understand these analyses, si nee No. 1, if air-dried, 

could not contain the amount of water here given, and if calcined 

could not yield a product of the composition of No. 2 which is, at best, 

very impure and of but little value. The analysis of the szekso shows 

no chlorides, which is also remarkable, when we consider the origin of 

this soda, which has been discussed by Szabo and Moser.2 According 

to them the sandy soil contains a large proportion of soda minerals 

which decompose through the joint action of carbonate of lime, water, 

and air. The lime furnishes carbonic acid to the soda which is dissolved 

in the water with which the ground, in winter, is saturated. As the 

summer approaches and the ground becomes warmer, the decomposition 

increases, while the water rising to the surface and there evaporating 

leaves its salts behind.

Owing to the rude methods of refining, with consequent variations 

in composition, and the increasing cost of collection, the Hungarian 

soda has not been able to compete with the artificial product, and now 

supplies only a limited local consumption in the manufacture of the 

celebrated Szegediu soap. Its history, however? is interesting, since 

we have in the West many occurrences of soda similar to those of 

Hungary, and it would seem at first sight as though they could be 

utilized; but if in a country of such low wages as Hungary the cost of 

collection is too great we can hardly look for much success in attempting similar processes at home, unless we can find deposits comparatively 

pure and of considerable thickness. In default of such, we can expect 

satisfactory results only from the waters of the soda lakes, in which 

nature, having performed the leaching process, has collected and concentrated the salljs.

1 Schapringer : Dingier, Polyt. Jour., vol. 18l>, ]>. 49.r>.

2 Szabo, J., and Moser, J.: Wagner's Jahrcsbcr., 1862, p. 223.
38 WASHINGTON LABORATORY. [BULL.60.

EGYPT.

The soda lakes of Egypt have been described by D'Arcet1 and by 

Eussegger.2 They are nine in number, in the Desert of St. Macarius, 

sixty miles northwest of Cairo and about thirty3 miles from the Nile, 

and are situated in a small valley running northeast and southwest. 

The largest, Nehel6, is five miles long by one-and-a-half wide, with a 

maximum depth of 20 feet. On the eastern side of the valley are 

a number of weak brine springs (some, indeed, being fresh) which feed 

these lakes in which, having no outlet, the concentration is continual, 

varied only by the annual rise and fall. Eussegger observed that the 

lakes rise when the Nile is falling and fall during its rise, and ascribes 

this partly to the rains which occur during the decrease of the river 

and partly to the supposition that the rise of the river is sufficient to 

overflow the divides of the clay formation which underlies the desert 

sand, and the water then flows through the sand to the lowest points 

of the valley in which are the lakes. As, however, it takes much time 

for the water to travel that distance, the lakes are not reached, and 

therefore do not rise, until the end of the high-water season.

The surface of the country is the desert sand, under which is a layer 

of blackish-gray clay, 20 feet thick, resting upon a tertiary sandstone. 

This clay is strongly impregnated with chloride of sodium and carries 

much gypsum, the quantity of both salts being much greater in the 

lower than in the upper part; it also contains much carbonate of lime. 

The gypsum is either scattered in single crystals through the whole 

mass of the clay, or, especially in the lower part, interstratitied with 

it in thin layers intermixed with desert sand and common salt, forming 

a kind of gypsum sandstone.

The lakes, formed by the leaching out of the soil, are therefore strong 

solutions of chloride of sodium containing in addition varying proportions of carbonate and sulphate of sodium. During the dry season, 

the smaller lakes dry up entirely, leaving on the bottom a salt crust of 

the composition of the entire lake 5 the larger lakes, on the other hand, 

do not dry up, but, as they become more concentrated, deposit salt crusts 

the composition of which depends upon the percentage of carbonate of 

sodium in the water.

In some of the lakes, bottom deposits are said to have gradually formed whose 

upper portion, 16 feet thick, consists essentially of sodium chloride, whilst the lower 

one, 17 feet thick, contains sodium carbonate. The above mentioned crusts, which 

are 15 to 18 inches thick, are pushed off by means of poles and spades, spread out to 

dry on the banks, and carried in baskets to the Nile, whence the salt is shipped to

'D'Arcet: Corr.ptes reuclns, September, 1845, vol. 10. Dingier Polyt. Jour., vol. 

98, p. 159. 9

2 Russegger: Karsten's Archio, vol. 16, 1842, p. 380.

3 Lunge: Sulphuric Acid and Alkali, vol. 2, 1880, p. 285 gives "five mites" as 

the distance from the Nile. He also quotes "Landerer, Waguer's Jahresb. 1858, p. 

68," in this connection, but the volume for that year does not seem on examination 

to have anything by this author or on the subject.
CHATAHD.] NATUEAL SODA. 39

other parts. It is called " latroni" in the Levant and in Greece ; the Egyptians use 

it to soften their very hard drinking water by precipitating its lime and magnesia 

salts, the water being afterwards filtered. Its principal use is in Crete for soap 

making. From Alexandria yearly about 2,500 tons are exported.'

This soda has been analyzed by Eeray,2 who describes the sample as 

bright gray, crystalline, effloresced on surface, slowly soluble in cold 

water, more rapidly in hot, leaving a little residue partly soluble in hydrochloric acid. The analytical results are as follows:

Sodium chloride, NaCL. .... ...............---....--...---- 8.1GO

Sodium sulphate, Na2SO,( ....................... ............ 2.147

Sodium silicate, NazSiOs........---.........---...---..----. .288

Sodium sesquicarbonate, NaJ^CsOo-........................ 47.292

Sodium carbonate Na2C03 .................................. 18.430

Calcium carbonate CaC03 ............................. ...... .200

Water..................................................... 19.GB9

Insoluble.................................................. 4.100

100.292

ARMENIA.

As described by Abich,3 the lakes of the Araxes plain in Armenia 

lie in the volcanic region of Ararat and show a great variety of composition. The lake of Tasch-Burun is situated on "the most distant of 

the lava masses which have broken out at the northwestern base of 

the Great Ararat," and its water carries 6.66 per cent, of salts, mainly 

sodium chloride as shown by analysis No. 1. Analysis No. 2 gives 

the composition of the crusts which are deposited on the shore in hot 

weather; these attain a thickness of a half-inch and are of a reddish 

color.

Other lakes are found southeast of Little Ararat among the volcanic 

lavas of this mountain. One of these lakes, remarkable for the reddish 

color of its water, lies on the left side of the valley close under the 

steep declivities of the greatest heights of the Gundusdag range which 

is formed of sandstone, dolomite, slates, and limestone and is broken 

through and shattered by a red quartz-porphyry. The surface of the 

country is a whitish clay, supporting a strong growth of soda plants.

The shore of tliis lake, which is about a mile in circumference, is very 

soft, so that walking is difficult, and is covered with crusts of a hard 

reddish salt having a laminated fracture. The crusts extend out upon 

the surface of the lake and portions are floating upon it, so that the 

whole looks as though it were about to freeze. Soundings showed that 

crusts had also formed on the bottom, apparently covering the whole of 

it. The water contains 30.63 per cent, of salts, the composition of which 

is shown by analysis No. 3, while No. 4 is the composition of the bottom 

crusts, and No. 5 of the floating portions.

1 Lunge: Sulphuric Acid and Alkali, vol. 2, p. 286. 

2 Eemy: Journal fur prakt. Chemie, vol. 57, p. 321. 

3 Abich: Jour, filr prakt Chemie, vol. 38, p. 4.
40 WASHINGTON LABORATORY. [BULL. 60.

The heavy bottom crusts are described as being composed of successive layers, each of which is a very solid radiated aggregate of crystals; 

the red coloring matter is deposited between the layers, which adhere 

closely together. The floating crusts have nearly the same composition 

and structure, but the layers are much thinner and the salt is almost 

white. The analyses are remarkable as showing that not only the sulphate but also the carbonate has crystallised almost free from water. 

Abich concludes that this is due to the formation of a "double salt" of 

sodium sulphate and carbonate, for which he proposes the mineral name 

"inakite." in the vicinity of this "red lake," are a number of small 

pools of a wine-yellow color, but without salt crusts. The water of one 

of these contained 34.74 per cent, of salts of the composition of analysis 

No. 5. Other lakes are mentioned in the original paper, but the waters 

were poorer in sodium carbonate and sulphate and richer in sodium 

chloride.

Sodium carbonate, NajC03 ......

AVater.HsO... ..................

No.l. No. 2.

Tasch-Burun.

Water.

14.71 

10.36 

74.61

99.68

Crusts.

22.91 

16.05 

51.49 

9 88

100.33

No. 3. No. 4. No. 5.

Red Lake.

Water.

12.08 

18.18 

69.73

99.99

Crusts.

Bottom.

18.42 

77.44 

1.92 

1.18

99. 90

Floating.

16.09 

80.56 

1.62 

.55

98.82

No. 6.

Yellow 

poo!.

Water.

68.90 

15.55 

15.50

v 99.95

The views of Abich as to the mode of formation of these salts will 

be given in the section treating of the origin of natural soda.

OCCURRENCE OF URAO IN VENEZUELA, SOUTH AMERICA.

This locality is described by Palacio Faxar1 as being in a valley named 

La Lagunilla in the province of Maracaibo, 48 miles from the city of 

Merida. In the center of this valley, the soil of which is said to consist of limestone, lies a little lake which in the rainy season has a length 

of 210 meters and a breadth of 106. Although its greatest depth is 

not over 3 meters, it never dries up entirely even in the driest seasons. 

The water is yellowish-green, has a soap}r feel, an alkaline taste, and a 

peculiar smell. During the hot season a salt crystallizes on the bottom. 

This salt, called urao, is collected every two years by the Indians of the 

neighborhood, who obtain from 100,000 to 160,000 pounds, according to 

the demand, which is for the manufacture of wo, a dried extract of tobacco used by the natives as a stimulant.

'Faxar: Ann. de Chimie, ser. 2, vol. 2, p. 432. Also, Pogg. Aun., vol. 7, p. 101.
CHATARD.J NATURAL SODA. 41

The Indians obtain the salt by diving for it, and the peculiar manner 

in which this is done is thus described by Boussingau.lt: 1

To collect the nrao, the Indians make an excavation on the bottom of the lake, 

several meters in extent, and plant therein a stake 14 to Hi feet long, the upper end of 

which reaches above the surface of the water. When this is accomplished an Indian 

resting upon this stake places the end of a second ono upon the deposit and holds it 

at a certain inclination. As soon as this is done, a second Indian glides down the 

inclined stake, plunges beneath the surface of the water and after the lapse of a few 

minutes returns with a portion of the salt. According to tho information we have 

received, tho deposit of nrao, which is not very thick, is covered by a layer of material'contaiuiug crystals of calcite. Above this is a hod of ooze, one meter in thickness.

The excavation spoken of in the beginning of this extract is apparently made for the purpose of removing these upper layers ; the crystals 

of so-called calcite were later shown to be gay-lussite Na2CO;j,CaCO.i-f 

5H2O; and the inclined pole is used to enable the diver in such a dense 

solution to reach the bottom. Concerning this water, Boussingault very 

curiously says: u The water of the lake is only slightly saline; animals 

drink it with pleasure."

As the water is necessarily a strong alkaline mother liquor, often 

completely saturated, it is evident that this statement is incorrect. 

Faxar (loc. cit), more accurately says of the divers: " Their death is inevitable if they swallow a certain quantity of the water."

He also says that the action of the water reddens the hair of the divers.

The Urao is described by Boussingault as " crystallized in prismatic 

needles arranged in radiating masses; a little softer than calcite. Taste 

alkaline; does not effloresce." His analysis is as follows:

Carbonic acid, CO2 -........................................ 39.00

Soda, NaaO ................................................ 41.22

Water, H2O ............................................... IS.80

Impurities................................................. 98

100.00

NOKTH AMERICAN LOCALITIES.

The various exploring and surveying expeditions sent by the Government into the region of the Great Basin have to some extent examined and reported upon the alkaline deposits and lakes lying within 

the range of their labors. Private prospectors, also, recognizing the 

future value of these salts, have not overlooked them, especially when the 

rapid development of the borax industry caused every accessible saltflat or marsh to be scrutinized and tested for that substance. In this 

way natural soda has been found in many places, but the absence of the 

necessary transportation facilities has, until lately, rendered any plan 

for the utilization of the soda a matter of the future.

Within the past few years the railroad facilities through this region 

have greatly increased and are continually extending, so that some of

'Boussiugault: Ann. de Chimie, ser. 2, vol. 29, p. 110.
42 WASHINGTON LABORATORY. [BULL. 60.

the more promising localities are within easy reach. The consumption 

of soda in this country is already great and steadily growing larger, 

and it remains for technical skill, supported by capital, to develop these 

resources and to convert a hitherto valueless, even obnoxious, material 

into a source of wealth. That this can be done there is no reasonable 

doubt; that it will be done should not be doubtful to any one who 

knows the activity and enterprise of our people. The advantages flowing from a successful prosecution of such an undertaking are reaped 

not only by the operators, but also by the entire section of country in 

which the work is carried on, and as, except in some favored .localities, 

nature has not been bountiful to this region, well-directed art must extend its aid.

The expense of the necessary preliminary investigations is considerable, but without these capital can hardly be expected to take any 

decided steps. A great deal of information, in the aggregate, has been 

gathered by various observers, but scattered as it is through various 

publications it is not readily available. It has therefore been deemed 

advisable to bring this knowledge together so that we may have a proper 

starting point for future work.

In proceeding to describe the localities within the boundaries of the 

United States only those concerning which we have reliable information will be considered, and it will be found that their number and 

variety are great enough to furnish types for any others which future 

investigators may bring to notice.

Wyoming. Along the line of the Union Pacific Eailway in the Territory of Wyoming are several places where natural soda is found. The 

best description of these is the following, from a paper on " Glass Materials," by Jos. D. Weeks, published by the Geological Survey in the 

"Mineral Eesources of the United States, calendar year 1885" :

The soda property generally kno\vn as the "Union Pacific Lakes" lies about 13 

miles nearly due soutb of Laramie and is reached by a branch of the Union Pacific 

Railway. The property embraces some 2,000 acres, including five "lakes," in all 

but one of which the soda is solid. The lakes are connected, and seem to drain one 

into another. All of the soil near Laramie is more or less impregnated with the sulphate of soda, and the common sources, it is believed, are springs, water from which 

bears large percentages of soda salts.

The physical condition of the soda in the lakes varies much with the season. In 

wet years the soda is almost fluid, while in dry years, in all but one of the lakes, it 

is solid and in this one it occurs as a saturated solution. In the solid lakes the soda 

contains many thin layers of mixed clay and soda. Analysis of a sample of this mixture shows:

Analysis of deposits of soda salts at Laramie, Wyo.

Per cent. 

Iron, lime magnesia.'....... ............................... 22. 33

Alumina, soda, hydrochloric and sulphuric acids.......... 40. H^

Silica ..................................................... 36.85

Organic matter .......................... .. ».............. traces.

100.00
CHATATU).] NATURAL SODA. 43

The soda when taken pure contains large quantities of water, which fact interferes 

seriously with its employment in the manufacture of sodium hydrate.

Its composition only varies slightly, and the following may be taken as typical 

analyses:

Average analysis of soda deposits near Laramie, Wyo.

Water ................

No. 1.

Per ct. 

44.55

54. 98

.47

100. 00

No. 2.

Per ct. 

41.41

04.79

3.80

100. 00

No. 3.

Per ct. 

31). 78

59. CO

.50

100. 00

These lakes are the only one.s from which soda is being takeu for use. 

The soda works near Laramie were built by the Uiiiou Pacific Railway and leased 

to Mr. Howard Hinckley. The process used is the old " black ash," with stationary

furnace. The capacity of the works is about 2 tons of sodium hydrate per day. The 

capacity of the furnace is 3£ tons of sodium sulphate per day. Rescref nod coal, from 

the Rock Spring Mine is used and the limestone necessary is obtained near Laramie. 

The " black balls," formed of the fused soda, coal and lime, are broken up and 

washed in fouv lixiviating pans, and the liquor is then taken to two settling vats. 

Thence it is drawn to the " causticizer," which is a large circular tank in which are 

two perforated vessels containing caustic lime, around which the solution of sodium 

carbonate is agitated. After the causticisiug the liquor is passed through three long 

circular iron settlers. The clear liquor is then drawn to the " V-pan," where waste 

heat is used to aid the evaporation of the solution. The slightly concentrated liquor 

is then drawn to the " boat pan," which is set upon the reverberatory furnace. The 

evaporation is then continued as long as possible, and the now concentrated solution 

is then drawn to another room iuto the " finishing pot." This is a large cast-iron 

pot set directly over a furnace. Here all remaining traces of water are driven off at 

a low red heat. The hydrate, at this stage is generally black and small quantities of 

niter are added to the fused mass to whiten it. The hydrate is then ladled into sheetiron vessels and shipped. Some of the Laramie caustic soda has been used by the 

Denver Soap Company, which reports favorable results from its use. Tho works at 

Laramie are not well adapted to the most economicalhandling of the soda. Improvements are now being made by which the number of men employed will be greatly 

reduced and the composition of the " black balls " be made more uniform.

When the soda works were first begun it was supposed that the natural occurrence 

of the material as a sulphate, rendering unnecessary the reduction of the chloride to 

the form of a sulphate, would greatly decrease the ultimate cost of the caustic soda; 

but it was found that the very large quantity of water present in the soda as it comes 

from the lakes, more than offset, by the trouble and delay it cost in the furnaces, the 

gain in the natural form of the soda.

Tho Laramie works produced from July to January, 1885, about 30 tons of caustic 

soda. Defects in the plant have caused great delay and loss of some of the caustic 

soda, and it has been decided to close the works until alterations nosv being made 

can be completed. Tho lessee of the works states that good reports of the caustic 

soda have been made by users of it.

Tho "Donney" soda lakes are situated about 18 miles southwest of Laramie and 

are three in number covering, with the land included, approximately 520 acres. In 

one lake the deposit is 11 feet thick ; in the others it is 5 to G feet. The soda from 

these lakes is similar to that from the Union Pacific lakes and there seems to be an 

underground connection between the two groups. In boring an artesian well near
44 WASHINGTON LABORATORY. [BULL. 60.

these lakes to prospect the underlying strata, a brine was obtained which upon analysis showed 

Analysis of brine from near tlie Donney Lalces.

Sodium chloride .... 

Sodium sulphate....

Grains per 

gallon.

2002.0

777.2

Per cent.

2.80

1.10

The large percentage of salt is very curious, as only traces of it are found in these 

lakes.

The soda deposits in Carbon County are situated in the Sweet Wa'er valley, near 

Independence Rock, and are nearly 50 miles due north of Rawlins. These deposits 

contain both carbonate and sulphate of soda, and are generally known as the " Dupont Lakes." The lakes are four in number, and vary from 6 to 2,000 acres in area, 

and are held by United States patents in the name of L. Dupont. There are five 

claims known as the "New York Soda Mine," 160 acres; the "Philadelphia," 80; 

the " Omaha," 20; the " Wilmingtou," 160, and the " Wilkesbarre," 20. The Omaha 

soda mine includes 20 acres, of which 5 are covered with carbonate and sulphate of 

soda, mixed with a little chloride of sodium and sand blown in from the surrounding 

soil. Several bore-holes were put down and show an average thickness of about 6 

feet.

Amount of JVffl3 C03 contained in the samples. 

No. 1, 3£ feet from surface............ ............ per cent.. 24.62

No. 2, surface...... ............ ...... ...... ...... per cent.. 41. 55

No. 3, surface near shore......................... per c<; u t.. 32.42

No. 3, water...... ............ .... ....... pounds per gallon .. 1. 33

A fused sample showed 52.23 per cent, of carbonate of soda. A fuller analysis of 

a sample taken from the surface showed:

Analysis of surface soda from Carbon County, Wyo.

Moisture.................................................... 9.01.

Insoluble................................................... 2.61

Sulphate of soda.... ............ .................. .......... 25.75

Chloride of sodium............................ ............. 2.13

Carbonate of soda....... .................................... 30.62

Bicarbonate of soda......................................... 30.09

100.21 

Another sample from near (ho surface contained 56. 3 per cent of water:

Analysis of dry salt.

Per cent.

Chloride of sodium .. ........... ...... ............ .......... 0. 65

Sulphate of soda......... ........................ .......... 59.29

Carbonate of soda...... ..................................... 27.60

Insoluble matter. .......................................... 1.20

The variations and the proportions of carbonate and sulphate of soda are shown 

by the following table, the samples having been dried:

Samples.

Five feet bnlow surface ..... 

Do....................

Surface ................ ..

NaCl.

Per cent, 

0.070 

0.32 

0.81.

Per cent. 

64.05 

C5. 08 

17. 02

Per cent. 

15.60 

1C. 70 

80. CO
CHATAKD.) NATURAL SODA. 45

The Wilkesbarre claim is about ono mile westof the Omaha, and the soda is insolation. Samples of this solution showed by analysis:

Per cent.

No. 1, Na3C03 grains per gallon ......................3,728=6.39

No. 2, Na.2C03 grains per gallon ......................4,905=8.40

The Wilmington claim is located one-quarter of a mile west of the Wilkesbarre, 

and covers 160 acres. The soda here is also in solution. Its depth has never been 

determined. It has been sounded with a 40-foot rope without finding bottom in the 

center. A sample of this solution contained 2,343 grains per gallon (4.01 per cent.) 

A sample which had crystallized out by cold, when dried showed:

Chloride of sodium......:.................................. 1.83

Sulphate of soda........................................... 39.04

Carbonate of soda........ .................................. 59.00

Insoluble matter........................................... 9.23

The New York and Philadelphia are both upon one lake, which is solid, and is 4 

miles west of tho Wilmiugton. Two bore-holes have been put down in this lake.

One, at a distance of 50 feet from the shore, showed4 feet of soda; the other, at a distance ot 230 fooc from the shore, passed through 14 feet of solid soda without touching bottom. Three samples taken from this lake showed as follows:

Chloride of sodium

Sulphate of soda ........

No. 1.

1.83

71.37

3.10

22. 82

9U.12

No. 2.

2.04

44.77

5.00

47. 50

99. 31

No. 3.

2.52

72.40

5. 10

19.03

99.05

Fifteen miles from these soda deposits good limestone, containing 2 per cent of magnesia, occurs in the Snminoe mountains. Near the limestone is a good 8-foot vein of 

coal. A comparison of the analyses from the Donnoy and Union Pacific lakes and 

those of the Dnpout lakes show how much greater the percentage of carbonate of 

soda in the latter is. The Sweet Water country is still out of the reach of transportation, and imr.il a railway is built in this direction these soda deposits must remain 

undeveloped.

' The Wyoming occurrences are typical sulphate deposits, and in many 

respects resemble those of Armenia, already described. Although they 

all contain more or less carbonate, yet, so far as we now know, it is not 

possible to extract the carbonate economically by natural crystallization processes. Under the most favorable circumstances the use of artificial heat is necessary, and, as stated above, the native sulphate, owing 

to the large proportion of water, has no advantage in point of cost and 

ease of working over the artificial. Careful and systematic study and 

experiment will doubtless, however, develop a good commercial method 

for the treatment of this material, since fuel can be easily obtained at a 

steadily decreasing cost, and transportation facilities are becoming 

greater.

Proceeding westwardly from the Wyoming deposits one finds numerous occurrences of salts more or less alkaline in character. Descriptions 

and analyses of many of these are given by King 1 and Russell; 2 but

'King: Gcol. Expl. 40th parallel, vols.'1 and 2.

?Jttissell: (Jeol. Hist, of Lake Lahontau U- S, Greol, Survey, Mon, No, U,
46 WASHINGTON LABORATORY. [BULL. 60.

most of them are only thin efflorescences or incrustrations, and, so far 

as we know, none have auy commercial value until we reach

The soda lakes at Ragtown, Nevada.-The&Q remarkable alkaline lakes 

or ponds are described at length by King in the work just cited, 1 also 

by Russell, Monograph, 11, pp. 73-80. From the latter report the following extracts are taken:

On the Carson desert, about 2 miles northeast of Ragtown, are two circular depressions that are partially tilled with strongly alkaline waters and known as the Soda 

Lakes or Ragtown Ponds. * * * The larger lake is 268.5 acres in area. * * * 

The rim in its highest part rises 80 feet above the surrounding desert, and is 1G5 feet 

higher than the surface of the lake which it incloses. The outer slope of the cone is 

gentle, and merges almost imperceptibly with the desert surface ; but the inner slope 

is abrupt, and at times approaches the perpendicular. A series of careful soundings 

gives 147 feet as the greatest depth of the lake. The total depth of the depression 

is therefore 312 feet, and its bottom is 232 feet lower than the general surface of the 

desert near at hand.

The walls encircling the lake exhibit well exposed sections of stratified lapilli 

mingled with an abundance of angular grains, kernels and masses of basalt, some of 

which are 2 and 3 feet in diameter, and scoriaceous, especially in the interior. * * * 

The form of the cones and the nature of the materials of which they are composed 

leave no doubt this is a crater ring, viz, a low cone of eruption containing a large 

crater. That the cones were not formed during a single eruption, but have a long and 

complicated history, and are perhaps suhlacustriue in their origin, is shown by the 

alternation of ejected and sedimentary materials in the crater walls.

" The smaller lake," according to Hague, " in most of its features, 

bears a close resemblance to the one just described and from which it is 

separated by a narrow ridge only an eighth of a mile wide. It has the 

same crater-like basin, but the banks are not more than 60 or 70 feet in 

height and the lake, even in spring, is scarcely more than one-filth of 

a mile in diameter. There is no supply of fresh water from the surface, 

and at the time of our visit, in August, the water was much more deuse

than in the larger lake. Over a great part of the surface was found a 

thick incrustation of trona strong enough to bear up a man, under which 

is a greenish slime and occasional pools of water. One characteristic 

feature of the shore is the green and purplish tints of .the moist sands, 

which, upon being dried, present the usual earthy colors."

The trona from the small soda lake, upon being subjected to analysis 

yielded the following: 2

Sulphate of soda..................... ...................... 0.99

Chloride of sodium.. ......,................_............... 1.10

Carbonate of soda.... ...... .... .... .... .... .... .... .... .... 66.27

Water and free carbonic acid.......... .... ................ ; 28.83

Insoluble residue........................................... 2.81

100.00

!Vol. 1, p. 510 513; vol. 2, p. 746 750.

2 Hague: King's Rep. 40th Parallel, vol. 2, 1877, p. 749. Russell (op. cit., p. 73., 

note) says: " The smaller lake (in 1882) had been so changed by excavation and the 

construction of evaporating vats that its original form had been destroyed. Its surface is 20 feet higher thau the larger lake and 65 feet below the general desert surface. 

The highest point ou the crater rim is 80 feet above the bottom of the depression."
0

CHATAHD.] NATURAL SODA. 47

Hague also says of these lakes (op. cit., p. 746): " they lie below the 

level of the plain, in which are probably ancient craters, and are not 

observed until just before reaching the brink." King (op. cit., vol. 1, 

p. 512) considers " that during the period of the occupancy of this region 

by Lake Lahontan * * * these crater-like lakes were points of 

extremely powerful springs deriving their great activity from volcanic 

sources," and gives his observations at Mono Lake, to which we shall 

refer later.

Russell, on the ofcher hand, says (p. 74):

The hypothesis that the craters were formed by the actiou of extremely powerful 

sublacustriue springs, as advanced by King, would not account for the nature of tho 

material forming the crater walls, nor the presence of the numerous volcanic bombs 

that depress the strata on which they rest. If tho cavities owed their origin to 

springs of very great magnitude rising in the bottom of Lake Lahontan, it is evident 

that the outflowing waters \vould have cut channels of overflow when the lake evaporated to a horizon below the rim of uncoilsolidated material that surrounded them; 

but the crater walls are now continuous and unbroken by stream channels. On the 

other hand, had the springs become extinct before the evaporation of. the lake, the 

cavities they formerly occupied would be buried beneath lake beds. This, as our 

observations sho\v, is not the case, but both the inner and outer surfaces of the cones 

are free from lake sediments. The latest additions to the cones must have been of 

post-Lahoutau date. * * * There are no streams either tributary to or draining 

these Jakes; their total water-supply, excepting the small amount derived from direct 

precipitation, is derived from subterranean sources. Around the immediate shores of 

the larger lake there are a number of fresh-water springs; the largest of these is 

situated on the northern border of the basin and issues from a small fault at an elevation of about 15 feet above the water surface. As the lake is 50 feet below the level 

of the Carson River at its nearest point, we may safely look to this stream as the probable source of tho water-supply, which reaches the craters by percolation through 

the intervening marls and lapilli deposits. The bottom of the lake is a continuation 

of the slope of the inner walls of tho crater, * * * is a fine black tenacious mud, 

having a strong odor of sulphuretted hydrogen. When exposed to the air for some 

time this material loses its inky color, and shows itself to be of the same nature as 

the fine dust-like lapilli that form a large part of the crater walls. The organic 

matter impregnating these sediments is evidently derived from the millions of brine 

shrimps (Artemia gracilis) and the larvae of black flies that s\vann in the dense 

alkaline waters.

My own observations in the summer of 1887 were confined to the 

technical aspects of the manufacture of sodium carbonate as carried on 

there, and the short time at my disposal did not allow me to take more 

than a cursory view of the formation, but I have little doubt that Mr. 

Russell's conclusions are correct, since they are supported by what may 

be seen at both Mono and Owen's Lakes.

The details of the manufacture of soda at these lakes are of great 

interest, since, as they differ so greatly in composition, an entirely different method must be employed for each.

The water of the larger lake collected in 1867 was analyzed by O. D. 

Alien (King's Rep., vol. 2, p. 747), and two samples, collected in 1882 

by Mr. Russell in the central portion of the lake at the respective depths 

of 1 foot and JQQ feet, were examined by me, My results, given below,
48 WASHINGTON LABORATORY. [BULL. 60.

agree very well, but differ from those of Alien mainly in that he reports 

the existence of sulphides, while I was unable to find any. If, as is very 

probable, Alien's sample was shipped to him in a keg, the presence of 

sulphides is easily accounted for by the reduction of sulphates by the 

action of the wooden vessel, since every sample of alkali water sent to 

this office in kegs has shown decomposition with resulting sulphuretted 

hydrogen, while the same material shipped in glass, as were Mr. Bussell's waters, was free from it.

The variations in composition between the water at 1 foot and that 

at 100 feet may in part be due to the fact that the mother liquors of the 

soda works are run back into the lake. These mother liquors are.poorer 

in carbonate and richer in chloride than the original water, and may in 

the course of years have changed the composition of the upper part of 

the lake.

The results are stated in grams per liter,1 and the hypothetical combinations between the constituents are such as they may reasonably 

be expected to form. The columns of percentages show the relation of 

the constituents to each other, and will be found of practical value.

Specific gravity at 19.8° C.

Chlorine, Cl.. ...... ...............

Hydrogen (iu bicarbonatos) 11 ....

No.l (Ifoot).

1.0995.

Weight.

.304

.270 

2. 520 

45. 840

.314 

45. G(JO 

.10. 8.0 

2. 100

1 ri '{T!

5. 583 

.179

129. Oil

Percent.

.24 

.21 

1.95 

35. 53 

.24 

35.41 

8.37 

.1.08 

11.89 

4.34 

.14

100. 00

No. 2 (100 foot).

1.0983.

"Weight.

.310 

.270 

2.070 

44. 270 

.3.7 

44. 270 

10.593 

2.117 

15. 128 

5. 501 

.188

125.044

Percent.

.25 

.21 

. 2.13 

35.23 

.20 

35.23 

8.43 

1.09 

12.04 

4.38 

.15

100. 00

1 The statement of results of analyses of such waters as so many grammes to tlie 

liter is preferable to the usual method of stating them as so many parts per thousand 

or per million. Any one handling such material necessarily measures his solutions 

hy volume and his products by weight. The metrical system is used throughout as 

in every respect more practical for the manufacturer, being not only a decimal system, 

but also giving an instantaneous conversion from measure to weight, and vice versa, 

without the labor of calculation. As small variations are sometimes met with in the 

tables found in ordinary hooks, we give the following as the best for comparison: 

A liter of pure water at 4°C = 1000 grammes = 1 kilo = 2.2046 lbs.= .264131U. S.

gallons, 1000 kilos = 1.10-23 ton (2000 Ibs.). 1U. S. gallon = 3.786 liters. 

1 meter = 39.3708 inches. 1000 liters = 1 cubic uieter.

The specific gravity of a liquid is the weight of a liter in grams. Thus a liter of 

Ragtown water, specific gravity 1.0995, weighs 1099.5 grams and a cubic meter 

1099.5 kilos,
CUATAltU.l NATURAL SODA.

Hypothetical combination.

Magnesium carbonate, MgC03 ....

Sodium, bi-borate (borax) Na-^O;.

Sodium bicarbonate, NaHCOs. ....

Ko. 1.

Weight.

.304 

.945 

4.808 

71.521 

19.170 

.400 

10. 8G8 

14. 989

12<J. Oil

Per cent.

.24 

.73 

3. 73 

55. 44 

14.80 

.31 

13.08 

11.61

100. 0(1

No. 2.

Weight.

.310 

.945 

5. 094 

68. 957 

18. 800 

.423 

15. 484 

15. 031

125. G44

Percent.

.25 

.75 

4.00 

54. 88 

14.90 

.34 

12.32 

12.44

100. 00

The Ragtown Soda Works. Mr. Russell's monograph contains an excellent map of the two lakes, drawn on so large a scale that the evaporating vats and their arrangements are clearly shown. He also gives 

many details of the manufacturing processes employed.

Two sets of works were in operation at the "Big Lake" in 1887, one 

belonging to Griswold & Bpperson, the other to Smith & Alien. Both 

works use the same process and the evaporating vats are alike. Owing 

to the narrowness of the beach it was necessary to build the vats in the 

Avater, which was done by running out levees at right .angles to the 

shore and connecting the ends of these by a main dike, thus forming 

rectangular compartments, which by use gradually became practically 

water-tight. Along the shore back of the vats runs a ditch, which is 

kept filled with lake water, and from this the vats are filled as needed.

Certain of the vats are used as "crystallizers," the rest as "evaporators." At the beginning of the season all are filled with lake water, 

and as this concentrates it is drawn from the evaporators into the crystallizers, so as to keep the latter at the proper depth about 12 to 15 

inches. ' As fast as this is done the evaporators are filled up with lake 

water from the ditch. In concentrating the brine gradually becomes a 

deep red (see page 95) and when it reaches 30° Baum6 crystallization 

usually begins. From this time on, the crystallizers must be carefully 

watched lest the soda as it forms should be too much contaminated 

with sulphate or chloride. There is no simple means of detecting the 

formation of sulphate, but when common salt forms it crystallizes in 

minute glistening cubes upon the surface of the brine. A sudden lowering of the temperature generally has this effect, which must be remedied 

by drawing off a part of the mother liquor and supplying its place 

with concentrated brine from the evaporators or even with lake water. 

This drawing off is, of course, only necessary if the vat is already full, 

otherwise the concentrated brine or lake water is added directly to the 

vat in sufficient quantity to re-dissolve the NaCl.

The crystallization process is allowed to go on in this manner until 

the sheet of crystals at the bottom of the vat has grown thick enough 

Bull. 60 4
50 WASHINGTON LABORATORY. [BULL. 60.

to be easily gathered or " lifted," say one-half inch to 1£ inches. The 

mother liquor is then drawn off into the lake, and the crop lifted and 

stacked up to drain. As this soda is made during the summer it is 

known as " summer soda," and is the product of the Big Lake. This 

is the material called in King's report "trona," but is in reality "urao," 

as will be shown by the analysis on page 52. In the process of gathering the crystal sheet is broken up into cakes, which are a hard and 

compact aggregate of crystals sometimes well0 formed.

When the crop is drained it is heated in a furnace to remove the 

water of crystallization and the excess of carbonic acid, and is then 

sacked and shipped as "soda ash."

The furnace is a single hearth reverberatory, the hearth bed being 

made of iron plate. The fire gases pass over the charge to the end of 

the hearth, then through two side flues, one on each side, under the iron 

plate, back to the bridge wall, thence return through, a center flue to 

the end of the hearth, where the stack is placed. The soda is dumped 

through an opening in the top of the arch onto the hearth, and is 

spread out evenly and heated for three hours, and then stirred from 

time to time until it is entirely dry. The furnacing as there practiced 

is a very simple operation, as the material parts with its water readily, 

and does not fuse, or even sinter, unless the heat is too high, and this 

is easily prevented by a little care in the stirring. In regular operation 

nine charges are worked off in a week; the fuel is sage-brush, gathered 

in the vicinity. Annual production about 450 tons, but this could easily 

be made much larger.

The operations at the Little Lake are conducted on an entirely different 

principle. The lake, as described in King's report, no longer exists, but 

the present appearance of the place is well shown in Russell's map. 

In the center of the depression there were at the time of my visit (1887) 

four large but shallow pits, besides a shallow pool somewhat larger, and 

filled with fresh water from the small springs which issue from the 

sides of the crater. Two of the pits are used as crystallizers and are 

supplied from the others, which contain a lye of about 12° to 13° 

Baum6. The lye is formed by the gradual solution of the "ledge" or 

deposit of crystallized sodium carbonate which exists in the bottom. 

No analysis of this ledge has so far as is known ever been made, and in 

consequence of the work which has been done it is difficult to obtain 

specimens. That material which was dug out for me had a close resemblance to dirty ice, although at one time it could be obtained in masses 

of considerable size and quite clean. Its appearance and the nature of 

its solution leave no doubt that it is a natural "crystal soda" or Na2CO3 

]OH2O in a comparatively pure condition.

The solution of this deposit, owing to the small amount of bicarbonate 

present, yields but little " summer soda." The concentration therefore 

continues, more lye beiug added from time to time until cold weather
CHATAKD.] NATURAL SODA. = 51

sets in. Usually by January the lye is sufficiently concentrated and 

chilled, resulting iu a copious crystallization of "winter soda" or 

Na2C03 , 1.0H2O, which is deposited on the thin layer of summer soda on 

the bottom of the vat.

When no more crystals appear to form, by which time the deposit is 

10 or 12 inches thick, the crop is lifted and carefully stacked preparatory to the drying process, the most delicate part of the work. The 

10H2O salt contains 63 per cent, of water, and parts with most of it 

with great ease and rapidity, so that if heated to 33°C. (90°F.) it melts 

in its own water of crystallization and becomes a liquid. In drying 

the crop great care must therefore be exercised lest the material 

should become liquid and much of it be lost.

The crop is therefore kept in the stacks until the approach of warm 

weather, when it is broken up and spread iu a layer two or three inches 

deep on the drying floors, which are covered with light sheds open at

the sides. The material is turned over from time to time and the lumps 

broken up. When the drying is completed the product is a thoroughly 

effloresced white powder, in which the summer soda appears as small 

pieces of thin cakes. The annual product amounts to about 300 tons.

Before giving the analyses of the products of the two lakes, a few* 

words of comparison between these two processes will aid much in 

giving a clear understanding of the meaning conveyed by the analytical figures.

The analysis of the water of the Big Lake has already been given. 

Though no analysis of the deposit of the Little Lake can be furnished, it 

is evident that it must give a solution much poorer in chloride and 

sulphate than the first locality. Let us see why this must be so.

When Hague visited these lakes in 1868 they had never been worked, 

and were therefore in their original condition. From the Little Lake he 

collected the material of which the analysis is given on page 46. On 

the shore of the Big Lake there were " large fields of dazzling white 

carbonate of soda," a sample of which was examined by O. D. Alien 

with the following results:

Water, H20................................................ 19.90

Insoluble residue........................................... .80

Sulphuric acid, SCv....................................... .73

Chlorine, Cl................................................ .98

Carbonic Acid, CCv............ ..i........................ 36.8G

Soda, NaaO................................................ 40.55

99.82 

Deduct oxygen = Cl........................ ................ .22

99.60

The deduction of oxygen=Cl is made because the whole of the Na is 

calculated as oxide Na2O, whereas that part combined with 01 is present

as Na,.
52 WASHINGTON LABORATORY. [BULL. 60.

To compare these two analyses, let us calculate the hypothetical combination of this last analysis and place it side by side with the first 

one, in which the 28.83 per cent, of CO2 and H2U have been divided into 

the constituents, so that the full theoretical amount of Na2CO3 is supposed to be present. If the theoretical amount of NaHCO3 be taken, 

the results will be found to vary very slightly.

Sodium carbonate, Na 2C03 ...... 

Sodium bicarbonate, NaHCOs . . . 

Water, H20- ....................

Big 

Lake.

.80

1.29

1.61

45.05 

34.66 

16.19

99.60

Little 

Lake.

2.81

on

1.10

44.25 

34.90 

15.95

100. Ou

If we were to deduct the insoluble matter from each of these analyses and recalculate them we should find but little difference between 

the two samples, which will be referred to later in the section treating of 

urao. They evidently represent the first and purest crystallization 

of the " summer soda" from the two lakes.

At the Big Lake, however, the process must stop at the point where 

this crystallization is obtained, while at the Little Lake the process is 

allowed to goon and the " winter soda" is collected with the summer 

product. Eussell procured samples of the " market soda" from each 

of these lakes, but neither of them seems to have been correctly taken, 

as the Little Lake soda contains too large a proportion of summer soda 

and the Big Lake material is the result of attempts, which naturally 

failed, to make winter soda at that place.

Silica, SiOz...... ................

Sodium carbonate, Na2C03 ......

Water, HsO .....................

Big Lake.

F. W. Taylor.

44Q

.011

.038

.040

2 im

49. 437

40. 714

7.118

100. 000

Little Lake.

Chatard.

.27

3

Q1

5.10

52.20 

25.05

14. 16

100. 09

These two analyses are valuable for comparison in this connection, 

although in the first one the acid CO2 of the NaHCO3 was not determined,
NATURAL SODA. 53

being included in the H2O which was evidently determined by difference. The chilling of the solutions would not materially increase the 

deposition of NaCI, but would greatly increase that of Ka2SO4 , hence 

the solution of the Little Lake must contain much less of the latter 

salt than the other water, the analysis of which has been given.

The combined product of the two lakes, as has been stated, is about 

750 tons per annum. The Little Lake has nearly reached the limit of 

its annual capacity, but the Big Lake might without great expense yield 

far more. With proper working the two lakes should yield 1,500 tons 

per annum.

Mono Lalce, Mono County, Cal. A very extensive description of this 

locality is given by Mr. I. C. Eussell in his article " Quaternary History of Mono Valley," in the Eighth Annual Beport of the U. S. Geological 

Survey, and I can only repeat what I have elsewhere said " that this 

large body of water, of a composition so favorable to utilization, is, for 

practical purposes, inaccessible and that the high altitude and consequent shortness of the evaporating season would, under any circumstances, render the success of any industry established there very doubtful. 1 The composition of the water is, as shown by the annexed analysis, 

very similar to that of Owen's Lake, which will be considered directly, 

and the same methods of economic treatment would apply to both, but 

owing to the reasons given above, there is little prospect that any extended use of the water of Mono Lake can ever be made.

The sample analyzed was collected by Mr. Eussell in 1882 and was 

taken at the depth of one foot, on east side of lake.

Specific gravity, 1.045 at 15.5°.

'SiOz .......... 

K...... .......

Fa............

Ca...... ......

Mg ...........

(Al2Fca )03....

so.............

C03 ...........

B4 07. .........

Cl.... .........

H...... .......

In 1 liter.

.0700 

90 14

1 0 fiflfvO

.0200

.0551

.0030

0. 6720

13. C903

.1600

12. 1036

nroo

53. 4729

Per cent.

.12 

1.79'

Of» Q1

.037

.10

. 005

12. 480

25. 6L

Oft

22.64

.10

100. 00

Hypothetical 

tion.

Si02 ..... .... 

(AbFo2)Os....

CaCOs ........

MgCOs.......

DfiuKiOT.......

KC1...........

Nad. .........

ya-jSOa .......

NftjiCOs.......

NtiHCOs ......

COt71pO8i-

.0700

.0500

. 2071

1.83G5

9. 8090

18. 3550

53. 4729

Per cent.

.13

.09

.39

3.44

34. 60

18.45

34.33

8.20

100. 00

Abert Lalce, Oregon. This lake, situated in southeastern Oregon, may 

in time become of considerable importance, for though at present far 

distant from railroads and hence unavailable, yet with proper transpor1 Chatard, Aril. Jour. Sci., ser. 3, vol. 36, p. 148.
54 WASHINGTON LABORATORY. [BULL. 60.

tation facilities the water could be utilized. The subjoined analysis of 

the water shows it to be the best suited for solar evaporation of all the 

lakes of the Great Basin, since, though not as concentrated as some 

others, the relation of the constituent salts is such that simple evaporaration should give a very pure product. Summer Lake, not far distant, 

is supposed to have a similar composition.

Both lakes have been described by I. C. Eussell 1 and by H. T. Biddle.2 

Mr. .Russell's paper contains the following analysis of the waters of 

Abert Lake, which shows a very large percentage of potash (loc. cit. 

p. 454).

Sp. G. , 1.02317.

Silica in solution . . 

NaCl...... ........

KC1. ..............

KzSOj ............

Grams 

in liter. .

0.065 

7.219

8.455

9.921

Sp.G., 1.02317.

K,C03 .-.-.. ...... 

MgC03 ...........

Grams 

in liter.

10. 961 

.006

27. 357

From what is known of geological chemistry and the phenomena of 

rock decomposition, it is safe to say that no lake of this composition, 

or containing such a large proportion of potash, could be formed, but 

if such an occurrence should ever be discovered, the rock decompositions yielding such a solution must necessarily be entirely different from 

all those so far observed. It is due to my friend Dr. Taylor, who made 

the analysis in 1882, to state that when, some years later, his attention 

was called to this matter he at once recognized the unlikelihood of such 

a composition, but as the balance of his sample had not been preserved 

and he was unable to find the figures of his analyses, he could not 

rectify the error, which is probably only a simple arithmetical error of

calculation in the estimation of the alkalies.

Mr. Biddle collected and examined a sample of the water of Abert 

Lake, and being unable to verify Dr. Taylor's results sent me the residue 

of his sample, which was examined with great care to settle the doubt. 

The sample was " collected by H. T. Biddle at middle of west side of lake, 

one foot below surface, 30-40 feet from shore, September, 1887." The 

total quantity at my disposal was about 200cm.3 , an amount too small 

for any extended research, but sufficient for all practical purposes. For 

each determination, 25crn.3 = 25.7792 grains were taken.

Specific gravity, 1.03117 at 19.8°.

'Russell: Geological Reconnaissance in Southern Oregon, Fourth Annual Report 

U. S. Geological Survey, p. 435 et seq. 

2 Biddle, H. T.: Am. Jour. Sci., 3d ser. vol. 35, p. 475.
CIIATARI).] NATURAL SODA.

Si02 ................

'K.... ...............

Na. .................

cSOs- ............. ...

10 . ..................

cC02 . ................

10. ..................

01...................

Contents in 25 cm3 .

A.

. ooo:i

.0133 

.3074 

.0148 

. 0030 

. 1.755 

.0015 

.3305

B.

. 0053 

.0136 

. 3071. 

.0140 

. 0029 

. 1757 

.0610 

.3360

Average.

. 00580 

.01345 

. 36725 

. 01470 

. 00295 

. 1.7560 

. 06155 

. 33655

la I 

liter.

. 232 

.538 

14. G90 

.588 

.118 

7.024 

2.4.62 

13. 402 

.058

39. 172

Per 

cent.

.59 

1.37 

37.51 

1. 50 

.30 

17. 91! 

6. 28 

34. 67 

.1.5

100. 00

Si02 ........

KC1. ........ 

NaCl....... 

N:i2S04 .... 

NaiCOa-..-. 

NaHCOi....

Hypothetical 

composition.

.232 

1.027 

21.380 

1. 050 

10. 611 

4872

39. 172

Per

cent.

.59 

2.62 

54. 58 

2.68 

27.09 

12. 44

100. 00

This analysis shows, as would be expected, that the water of Abert 

Lake does not differ materially from tbat of any other alkali lake so far 

discovered. Its low percentage of sulphate is its greatest merit, since, 

as will be shown under the section treating of Owen's Lake, it is of all 

the impurities the most difficult to remove and the most deleterious 

when present.

Dry deposits in the United States. With the exception of Owen's 

Lake, the foregoing are the only lakes which have a prospective value 

for the alkali industry, although there are many others which are 

alkaline, but are too dilute for profitable working. There is, however, 

another class of alkali occurrences which may in time become available, though at present of minor importance. These are the so-called 

dry deposits left by the desiccation of shallow lakes formed in the wet 

season by the drainage of the surrounding country, but drying up more 

or less completely during the summer, leaving an incrustation of salts 

often of considerable extent, though usually of no great thickness.

In the region of the Black Eock Desert and adjacent parts lying 

between Abert Lake and the line of the Central Pacific Railway there 

are many places which furnish such salts. The following analyses will 

give an idea of their composition: 

No. 1. Soluble portion of incrustation from near Black Rock Point, Black Eock

Desert. Chatard. I. Russell, Monograph Xf, U. S. Geological Survey, p. 231. 

No. 2. Quinn's River salts. 0. D. Alleu. King, 40tli Parallel Survey, vol. 2, p. 791. 

No. 3. Hardin City salts, O. D. Alien. King, ibid., p. 792.

SiO*....-.. .............

TTPl

Nad.... ..............

NaiSO4...... .......... 

NajCOs ...............

No. 1.

2.18

1. 3!)

59. 3;>

27. 05 

9.06

100.00

No. 2.

*1. P2

t8. 57

85. 27

1.75 

2. 59

10U. 00

No. 3.

18.47

27. 55 

52.10

98. 12

* Residue. I Water.
56 WASHINGTON LABORATORY. [HULL. 60.

The next five are also from King's 40th Parallel Exploration, and 

show the general character of the alkaline incrustations of eastern and 

central Nevada. In each case the amount of H2O necessary to form 

NaHCO3 has been added and the analysis calculated to 100 per cent, 

for comparison.

No. 4. Ruby Valley, Nevada (Woodward), vol. 1, p. 503.

No. 5. Valley of Deep Creek, Utah (Woodward), vol. 2, p. 474.

No. 6. Antelope Valley, Nevada (Woodward), vol. 2, p. 541.

No. 7. Hniuboldt Valley, Nevada (Woodward), vol. 2, p. 594.

No. 8. Brown Station, Humboldt Lake (Woodward), vol. 2, p. 744.

KS S04 ..............

Na2S04 .............

NaCl ...............

NajC03 .............

NaHC03 ....-.....--

Na2B407 ............

No. 4.

2.79

28.32

2.11

58.69

8.09

100.00

No. 5.

4. 68

17.43

38. 01

25.12

14.76

100. 00

No. 6.

1.88

33.31

24.51

25.95

14. 35

100. 00

No. 7.

4.42

7.24

48.99

3G. OL

3.34

100. UO

No. 8.

49.67

20.88

7.02

11.13

11.30

100.00

At many localities in western Nevada and in that portion of California east of the Sierra, incrustations of like character occur. Of these 

perhaps the most important are the soda lakes in Long Valley, California, 

lying southeastwardly of Mono Lake. The country is highly volcanic 

and the rocks are in many places much decomposed, having upon them 

efflorescences and incrustations. There are many w,arm springs, the 

waters of which flow into the lakes. These are several in number, connected together, with a drainage during the wet season into the headwaters of Owen's Eiver. The shore shows in most places a salt crust 

around the margin, but in the hurried visit I paid this locality in the 

summer of 1886, I had no time to make a more particular examination, 

especially as the lakes are the deepest portions of extensive morasses, 

which in the winter are completely flooded. In the vicinity are large 

stretches of playa covered with thin sheets of alkaline salts, which are 

said to grow to the thickness of two or three inches on the approach of 

cold weather, when the material is gathered for the use of the mills at. 

Bodie. A little to the north of the lakes is a so-called "hopper," a depression in the plain resembling on a small scale the Little Lake at 

Eagtown. The deepest part is filled with a small pool on which is a 

salt crust which covers the remainder of the bottom. The alkali from 

this place is also collected. Were there any facilities for transportation Long Valley might be made to yield a considerable amount of soda 

annually.

There are many other localities in this region, but further enumeration would be useless as the entire country is volcanic in its character,
CHATAUD.I NATURAL SODA. 57

and so far as there is auy drainage the water flows into Owen's 

Lake.

"Owen's Lake. By far the most important natural source of soda is 

Owen's Lake, Inyo County, California, both on account of its magnitude 

and of the facilities for carrying on extensive operations.

It was visited by a party of the Wheeler Survey in 1875, and is 

described in the reports of Lieutenant Birnie and Dr. Oscar Loew, 

published in " Report of 0". S. Geographical Surveys west of the 100th 

Meridian, 1876," pp. 130-135 and 189-190. Both in the summer of 1886 

and of 1887 I spent some time at the lake, and as the Inyo Development 

Company has begun the manufacture of soda at Keeler, a small village 

on the shore of the lake at the terminus of the Carson and Colorado 

Railroad, every needed facility for observation and experiment was 

most courteously extended.

Loew (loc. cit.) states that the greatest length of the lake is 17 miles,

its greatest width 9 miles, and greatest depth 51 feet. The total surface is given by him as nearly 110 square miles, and from his analysis 

of the water he calculates the total contents of the lake in sodium carbonate as 22,000,000 tons, and suggests the utilization of this great 

chemical treasure.

The lake lies between the Sierra Nevada on the west and the Inyo 

range on the east and has no outlet, the lowest point of the rim of the 

valley to the southward being, as I am informed, about 50 feet higher 

than the present level of the lake. On the western side several small 

streams from the Sierra make their way to the lake, but the greater 

portion of the water supply is furnished by the Owen's Eiver which 

empties into the lake at its northern end. This, according to Loew, is a 

stream about 30 feet wide, 2 feet deep, with a velocity of about 5 miles 

an hour. It was my intention to collect accurate data concerning this 

river, as well as to get samples of the water taken at different points 

so as to determine the origin of the carbonate in the lake, but circumstances have prevented the prosecution of this part of the investigation.

As would be naturally expected the lake is somewhat higher in the 

spring than in the autumn, but its average depth suffers but little 

change, hence the evaporation from its surface seems to be at present 

about equal to the amount of water received from all sources. As the 

valley lies between two high ranges of mountains, and is open to the 

north and south, there is usually a good breeze through the greater 

part of the twenty-four hours, thus much increasing the evaporation 

which may safely be taken as about 5 feet in the year, though experiments give a larger result.

On the eastern side, the valley slopes gradually from the foot-hills to 

the lake. The shore is covered in most places with a strong growth of 

salt grass, though there are extensive sandy flats which are bare.
58 WASHINGTON LABORATORY. [BULL. 60.

In the lake itself are large quantities of a sort of " algous or fungoid 

plant, floating in small globular masses of a whitish or yellowish green'' 

(Loew). This collects in patches upon the water and becomes black 

with the clouds of "alkali flies" or ephydra which settle on it. In 

addition to the larva of these flies the water swarms with the artemia.

A carefully selected sample of the water of this lake taken September 17,1886, gave me the following results. All the determinations 

were made in duplicate, the duplicates agreeing very closely. Specific 

gravity, 1.062 at 25°.

Si02 ..........

K. ............

C.i............

Mg. .......... 

FetaOi ..-.--...

Ala03 .. .......

SO... ..........

KtO7 . .........

CO,.. . ........ 

Cl. ............

H...... .......

Inl

liter.

220

j 54.4.

28. 500

.014

.005

7. 505

19.398 

19. 344

.063

77. 098

For

cent.

oo

2. 13

36.96

.02

.02

9.73

49

25.16 

25.09

.10

100.00

SiOz ............

(AJ2Fe2)03......

(CaMK)Co3......

^tuB-iO? ........

KC1 ............ 

Nad ...........

Na2SO4 ........

KaaCOa-. .......

NaHCOs. .......

Hypothetical 

composition.

99ft

.038

ncr

.475

3.137 

29 415

11.080

R 71 C

77. 098

Per

cent.

90

|.»

.03

4.07 

. 38. 10

14.38

34.95

7.40

100. 00

Oiven's Lalce Soda Works. The works of the Inyo Development Company begun in the winter of 1885-'86, had so far progressed by the summer that a small amount of crude soda was produced. Lack of experience on the part of those in charge caused, however, many delays and 

disappointments, and it was not until the summer of 1887 that, under 

the management of Mr. Frank Gray, formerly of Eagtown, a fair start 

was made.

There are now nearly 15 acres of vats, mostly well made. The 

slope of the ground is such that the vats can be, in general, arranged 

in two lines so that the upper ones can be used as evaporators, the 

lower as crystallizers. By the method introduced by Mr. Gray the lye 

is allowed to concentrate in the crystallizers, more concentrated solution 

from the evaporators being added from time to time, till a sufficient 

quantity of the first crop is formed. This first crop is, however, comparatively soft and mushy owing to the small size of the crystals, so 

the mother liquor is drawn off; clear, well-settled lake water is added in 

sufficient quantity to redissolve the crystals and when this is done as 

completely as practicable, the vat is then filled up from the evaporators. 

By this means a new solution is obtained, containing a much smaller
CHATARD.I NATURAL SODA. 59

proportion of chlorides and sulphates than the original lake water, and 

the crystals obtained from it are much larger and purer. The crystallization is allowed to go on, with additions from the evaporators until 

the cooler weather begins, when the soda is lifted.

The cake is then two or more inches in thickness, and if proper care 

be taken during its formation it should be quite clean and contain but 

little sulphate or chloride. An analysis of a sample of the crop of 

1887, a good specimen but not better than could be made on a large 

scale with experience and judicious management, is given on page 76; 

" best specimen," while the " crude " is the undissolved first crop.

The process of furnacing this material so as to convert it into soda 

ash is very simple and easy, since the water and acid CO2 is driven out 

at a temperature but little above 150° 0. (300° F.), and no fusion takes 

place. If the material represented by the "best specimen "be thus 

heated it would give an ash containing 97.77 per cent, Na2C03 , while 

the " crude " treated in the same manner would yield a 94 per cent. ash. 

When we consider that these favorable results have been obtained in 

the infancy of a process, without special skill or experience, it is not 

unreasonable to expect that, under proper technical management and 

with suitable arrangements and appliances, a product averaging OS.per 

cent. JSra2CO3 can be made regularly and in large quantities, at this 

locality.

The calculation of Loew shows that this lake contains 22,000,000 

tons of Na2CO3 , and if we make the moderate estimate that onehalf of this amount can be extracted from it, and consider the natural 

advantages of climate and of the character of the shore which in many 

places is well adapted for the location of extensive works, there seems 

to be no reason why, in time, a large and flourishing industry should 

not develop there.

The small amount of the annual rain-fall and the very great annual 

evaporation resulting from a long season of very warm and dry weather, 

are extremely favorable. No experiments determining the annual 

excess of evaporation over precipitation, have been made in this region, 

but we have reason to think that it is not less than 7 feet per annum. 

The experiments now to be detailed show a much greater rate, but as 

they were carried on in small vessels fully exposed to the rays of the 

sun, the daily loss is, of course, far larger than would occur when an 

earth vat of large size is used for the purpose.

EXPERIMENTS ON THE EVAPORATION AND FRACTIONAL CRYSTALLIZATION OF THE WATER OF OWEN'S LAKE.

These investigations were made during the summer of 1880, for the 

purpose of obtaining information needed for the devising of manufacturing methods suitable for such waters.

Evaporation. On September 6, noon, a granite-ware pot 7£ inches
60 WASHINGTON LABORATORY. [BULL. CO.

interior diameter, 6 inches deep, with straight sides, was filled 5finches 

deep with lake water, specific gravity 1.057 at 18.3° (05° F.) The pot then 

contained 8£pints, the measurement of depth being made by sliding arule 

along the side of the vessel until the lower end of the rule just touched 

the water. By having a thin strip of metal bent over the edge of the 

vessel the measurements can be made very closely. By using short 

hydrometers the specific gravity of the solution could be readily taken 

without disturbing the liquid.

Date.

Sept. 6

Sept. 7 

Sept. 7 

Sept. 8

Sept. 8 

Sept. 9 

Sept. 9

Sept. 10 

Sept.' 10 

Sept. 11 

Sept. 11 

Sept. 12

Hour.

12 m .....

7.30 a. ra. 

5.30 p. m. 

8.40 a. ni.

4,35p.m. 

7.45 a. m. 

4.15 p. m.

8.25 a. m 

5.15 p. ra. 

7.50 a. m. 

5.15 p. ra. 

8.3d a. m.

Depth to 

surface.

Inches. 

i

* 

u 

n

2

2£ 

2£

n

3 

3& 

3* 

3&

LOS9.

Inches.

i 

I 

«

fl 

i

i 

i

k 

A

& 

i

Specific 

gravity.

3.057 

1.07

1.077 

1.082 

1.090 

1.093

1. 103 

1.110 

1.120 

1.127 

1.138

Temperature.

65° F.

i873°TT 

co°

15.5°

71°

21. 7° 

82°

27. 8° 

75.50

24°

85°

29.4° 

71°

21.7°

850 

29.40

67.50

15. 8° 

840

28. 9°

740

23. 3°

Remarks.

t Filled pot ; water filtered and 

I clear.

! Slightly whitish deposit at edge 

of liquid. Liquid slightly 

turbid.

(A. minute surface crystalliza- 

 i tion observed, probably CaCOg. 

[ Liquid more turbid.

Hot wind ftora south.

r Liquid quite turbid. A thin 

< granular precipitate 011 bot- 

[ torn and sides of vessel.

The concentrated solution was at this time transferred to a smaller 

granite-ware pot 6£ inches wide, 5£ inches deep. The surface of the 

solution was 2£ inches below edge of pot, and, as the capacity of the 

vessel had been carefully measured for successive depths, the volume 

of the solution was 3£ pints. The granular precipitate which adhered 

to the large pot consisted of CaCO3 with a little Fe2O3 .

As the original solution measured S£ pints there was a loss of 5 pints, 

or 58.82 per cent., in bringing it to 1.138 (18° B.) at 23.3° (74°F.). When 

the liquid reaches 1.096 (13° B.) it begins to deposit its CaCO.-j, the 

maximum of deposit being at about 1.130-1.138 (17°-18° B.). No 

increase of deposit was observed after the latter point was reached.
CHATAKU.] NATURAL SODA. 61

.Date.

Sept. 12

Sept. 13

Sept. 13

Sept. 14

Sept. 14

Sept. 15

Sept. 15

Sept. 16

Sept. 10

Hour.

4.45 p. m.

7.35 a. in.

4.45 p. m .

8.20 a. in.

5.00 p. m .

9.00 a, in.

4.30 p. ni.

8.45 a. in.

4.35 p. ni.

Depth.

Inches. 

2ipo

2J

3

3i

3£

318

3J

35

4

Loss.

Inches.

 fa

A

TO

'IB

.A

ft

ft

 &

ft

Specific 

gravity.

1.150

1. 105

1.175

1.190

1.215

1.232

1.250

1.260

1.273

Temperature.

89°

31. 07°

64° 

17. 78°

84.5° 

29/1°

72° 

2~272°

85° 

29. 44°

750 

24°

87.5° 

2379°

770 

250

100° 

37. 78°

llemarks.

Incipient crystallization.

Crust formed.

At 8.45 a. m., the solution measured 1§ pints. Hence during the 

concentration to the crystallizing point the liquid lost 6f pints, or 80.4 

per cent, of its bulk, or 5 volumes of Owen's Lake water at the specific 

gravity and temperature above given are reduced to one volume when 

crystallization begins. From these figures the proper relation between 

the evaporating and the crystallization surface is at once obtained. As 

should be expected the daily loss diminishes as the solution concentrates ; the total time of evaporation was nearly ten days, the average 

loss one-half inch per diem, maximum loss one inch, minimum one-fourth 

inch. Observations on earth vats, although roughly made, indicate an 

average evaporation of one-fourth inch in twenty-four hours under the 

same circumstances.

The rapid heating of the solution as soon as a crystal crust had 

formed on the surface is also worthy of notice.

Fractional crystallization. The following experiments were made in 

order to determine the character and composition of the successive crops 

of crystals obtained by the continued evaporation of a portion of Owen's 

Lake water, until the point is reached when the sun's heat is no longer 

sufficient to drive off the water except with great slowness; or, in other 

words, to observe the gradations and extent of a practical soda evaporation.

September 3, 11.30 a. m. Five quarts of filtered, partly concentrated 

lake water were put into each of two granite-ware pans, which were then 

placed in the sun. The water had a specific gravity of 1.135 at J^, the 

10 quarts, so taken, being equivalent to 25 quarts of original water.

September 5, 8.30 a. m. The solution in each pan had deposited a 

small quantity of a fine granular precipitate, while a few stout acicular
62 WASHINGTON LABORATORY. [BULL. 60.

crystals were floating on the surface. Solution pan No. 1, 1.282 j No. 

2, 1.270, both at ^ 5. Filled up pans with filtered water from vat, specific 

gravity 1.19 at gj^, adding to each 3 quarts, equivalent to 7£ quarts original water. The total amount in the two pans was therefore equivalent 

to 40 quarts of lake water.

September 6, 7.30 a. m. Both pans showed a large crop of crystals 

on bottom, while the liquid was turbid, with small crystals floating in 

it. Specific gravity of both solutions, 1.250 at ~^.

September 7. Both pans had a stout crust with large deposit.

3.45 p. m. Poured off mother liquor from both pans and drained 

crystals. The crop Al weighed 1£ pounds when dry. The combined 

mother liquors measured 5£ quarts and had a specific gravity of 1.312 at 

j]!^. This was put in one of the pans and allowed to evaporate.

September 8. The solution was covered by a thin crust, with a considerable deposit of minute crystals on bottom.

September 9. Poured off mother liquor from second crop, A2, 

which weighed 1 pound, and drained the crystals thoroughly. Mother 

liquor 1.312 at g.

September 10, 8.30 a. m. Pan showed a considerable deposit of fine 

granular salts with thin crust on surface.

September 11, 8.30 a. m. Drew off moth'er liquor and secured third 

crop, A3., which was highly saline to taste, and weighed three-fourths 

of a pound. The mother liquor had a specific gravity of 1.315 at ^r-fjjs.

September 12, 5 p. m. The solution was covered with thin, floating 

crusts, and its temperature was 3^5, while the same thermometer exposed

for five minutes to the direct rays of the sun showed barely 5? another 

solution; B, of about 1.29 showed ^^0 .

The evaporation of this concentrated solution was very slow, so it 

was undisturbed until the 18th, when, as no further reduction in volume 

could be observed, the mother liquor was poured off, leaving the fourth 

crop A4. It had a specific gravity of 1.327 at ^J.

To observe the effect of cold at this stage, the vessel containing the 

solution was surrounded with ice. After four hours, at a temperature 

of 74j-°5 a large deposit of a slushy material, looking like wet snow, was 

obtained. This crop, A5, was collected and placed in a pan to dry, but 

speedily melted in its water of crystallization, afterwards becoming a 

dry cake on the bottom of the pan. The mother liquor had a specific 

gravity of 1.300 at j|^5, and was preserved for analysis.

The salts so obtained were analyzed with the following results, to 

which is prefixed an analysis of a sample of the crude soda made at 

the works in that year :
CHATAUD.J NATURAL SODA. 63

Sp. gr. mother liquor. . . . J

Water at 120° C., H20 ..... 

Water at red boat, H20 . . .

Chlorino, 01..... ..........

Soda, MazO. ........ '.......

Potash, EiO....... .......

Deduct 0-C1.. ...........

Crop 

1886.

1.280 

(80° JT.)

~23.~82~ 

.33 

1.55

.18

.14

.01

.01

.01

1.07

2. 30

33.04

37.91

.32

100. 75 

.53

100. 22

Al.

1.312

(80. 50)

17.10 

.54 

.078

.032

.01

.07

.01

1.795

4.84

33.98

' 41.87

.68

101. 15

.78

100. 37

A2.

1.312 

(77°)

firbT

.41

O KI".

. 015

.02

.00!)

14.33

21.81

46.93

.71

104. 33 

4.91

99.42

A3.

1. 315

(79.20°)

3.57 

.29

97

.03

.009

15.05

28. 81

9 67

48.47

.72

106. 64 

C.49

100. 15

A4.

1.327 

(96.6°)

2.37 

.24

.05

.01

10.70

37 r>9

7 9<;

48.69

.76

108. 66 

8.75

99.91

A5.

1.300 

(57°)

10.53 

.92

*1. 14

.10

AO

13. 01

24.93

47.29

1.85

103. 07 

2.93

100. 14

l' Boric acid,

Hyiwthetical combination.

HsO .....................'.

Si02 ......................

AhOa...... ...............

(CaMgJCOs...... ........

KC1...... .................

NaCl...... ................

NiuS04. ...................

NaaC03 ...................

NaHCOs ..................

Crop 

1880.

20.87

.18

.14

.01

.04

.51

3.51

1 SO

40.87

30.65

100. 22

Al.

14. 51

.078

.032

.055

.01

.14

1.07

7.44

3.18

43.75

30.12

100. 37

A2.

4.33

^

1 .09

1. 12

35. 06

22, 84

10.53

99. 4 T

A3.

3 <T!

.00

1.14

45.59

18.19

100. 17

A4.

2.24

( .05'

< .01

1.2L

60.99

19.01

12.51

O QQ

99. 91

A5.

11.03.

.1C

.02

2.93

19.10

5 7ft

4 09

2.01

100. 14
64 WASHINGTON LABOKATOKY. [BULL. 60.

Another series of crystallizations was made at the same time (series 

B). In this, the first crop, Bl was collected when the mother liquor 

stood at a specific gravity of 1.285 at ^|^; second crop, B2 with mother 

liquor of 1.325 at ^^ ; third crop,B3, mother liquor of 1.323 at ^ and 

B4 under the same circumstances as A5. *

H;,0at 120° C.......

H20 at red boat.....

Si02 ................

AW3 . ..............

CaO ................

MgO.. ...........

so8 . ................

Cl ..................

COz. ...... ..........

tfaaO. ...... ........

K,0 ................

B203 . ...............

Bl.

18. 68 

.43 

.17

. 27

.05

.02

1.49

3.70

34.72 

40.87

.05

101. 05

.83

100. 22

B2.

7.35 

.41

.04

.12.44 

22. 03

15.31 

40.30 

.03

104. 02 

4.96

99.06

B3.

2.37 

.38

.04

13. 55

0.10 

49.61 

.73

108.28 

8.00

100. 28

Specific gravity of mother liquor. 

Bl.. ...................................... !. ->

B2.... .................................... 1.3

B4..... ................................... 1.3

B4.

9.30 

1.30

.21

3.59 

14. 74 

23.25 

47.02 

2.21 

*1.10

103.32 

3.32

100. 00

85 (S0°) 

25 (81°) 

23 (75°) 

1)0 (57°)

*By difference.

Hypothetical combination.

11 .,n

SiOa ............

A1203 . ..........

(CaMg)C03 .....

KC1 ............

tfaCl ...........

Na.,S04 . ....... 

K"a2C03 .........

NaHOOs. .......

NaaB-Oi ........

Bl.

15.97

.17

.27

Trace.

.07

' 1.02

5. 30

2. 62 

42.33

32. 47

100. 22

B2.

0.89

.04

.02

1.00

35. 51

22.08 

25.00

9.12

99.66

B3.

2.60

.04

1.15

57.60

24.24 

14.02

.54

100.28

B4.

10.51

.21

3.51

21.60

6.31 

54.91

.87

2.08

100. 00

In B4 the boric acid, which was proved to exist in some quantity, was 

estimated by difference, as the process for its determination is tedious, 

and exact figures for this substance in cases like the present are of
CHATAKK.J NATURAL SODA. 65

little consequence. In the hypothetical combination the neutral borate 

Na2B2O4 is given instead of borax or the acid borate Na2B4O7. The 

latter can hardly be supposed to exist in such strongly alkaline solutions as those which produced A5 and B4. In the original water the 

acid borate is set down as probably existing, since a considerable 

excess of CO2 is there present, which decomposes the neutral borate, 

forming

DISCUSSION OF RESULTS.

In comparing these analyses let us first consider " crop 1886," Al and 

Bl. These are the first crops of a solar evaporation, and are the only 

ones of any technical importance, unless suitable processes can be 

devised for utilizing the mother liquors, which by simple evaporation 

yield products of too low grade for the market, where the value is fixed 

by the percentage of Na2CO3 in the ash and the proportion of other 

salts must not exceed certain limits.

Compared in this way, crop 1886 mother liquor 1.280 is the purest, 

Bl, mother liquor 1.285, comes next, and Al, mother liquor 1.312, is the 

worst. It is evident, therefore, that if the first crop is to be used 

directly for making soda ash the concentration should not be allowed 

to run as far as 1.280, but, as, in such a case, the crop would be a comparatively small one, the advantages of a recrystallization are plainly 

indicated by comparison of the crop of 1886 with the "best" and 

" crude" of the crop of 1887. (See page 76.)

The rapid increase of SO3 and 01 is shown by the two series. SO3 

reaches its maximum in A3 and B3 and then rapidly declines, while 01 

is greatest in A4 and B3. NaHCO3 is deposited in great part in the 

early stages of the crystallization ; so that, when afterwards, most of 

the sulphates and chlorides are got rid of, the remaining solution contains a very large proportion of Na2OO3, which separates when the solution is chilled.

The solar evaporation thus divides itself into three stages ; first, the 

deposition of a comparatively pure compound of Na2GO3 and NaHCO3 ; 

second, the formation of a product consisting in great part of sulphates 

and chlorides; and third, the production of a mother liquor requiring 

an artificial heat for its further evaporation, but rich in Na2CO3 , and 

containing the major portion of the potash and boric acid.

Fractional crystallization of water of Mono Lake. In this connection 

it will be interesting to compare the results of a similar series of crystallizations of some water from Mono Lake. This water had been concentrated by heating, and consequently most of the bicarbonate was 

reduced to normal carbonate; besides, the total quantity at disposal was 

so small that the results are not very reliable, but will show the general rule.

Ji, L p. 157,
66 WASHINGTON LABORATORY. [BULL. 60.

The concentrated water was about one-sixth of the original in volume, and had a specific gravity of 1.210. On being exposed to a dry 

atinophere for quite a long period it began to deposit cubes of Nad, 

and then a quantity of indefinite crystals (Cl). These were collected, 

the mother liquor showing a specific gravity of 1.348. In time this 

solution gave a second crop 02, but did not vary in specific gravity. 

When, however, the third crop 03, had been obtained, the mother 

liquor showed a reduced specific gravity of 1.335. Continued evaporation yielded 04 mother liquor 1.361, and 05, mother liquor 1.381. The 

final evaporation to dryness gave 06. 05, when examined, was a mixture of cubes of NaCl resting on a layer of salts which, however, was 

too small in quantity to give accurate determinations, since, though 

carefully ground and mixed, concordant results could not be obtained. 

In such cases, where different salts crystallize together, concordant 

results can be looked for only when the sample, carefully weighed, is 

dissolved in water and portions of the solution weighed out for analysis. The figures obtained show that the composition of 05 lies between 

04 and 06.

Sp. gr. mother liquor . .

0,0...... .............

Si04 ..................

CaO...... .............

MgO. .................

SO............... ....

Cl...... ...............

C02 . ..................

Na-iO...... ............

KsO.. .................

O-C1...... ...........

Cl.

1.348

15.21

.07

. .03

.23

1.54

11.07

20. 91

43. 02

.43

102. 41

99.72

C2.

1.348

12.15

.08

.22

7.99

13. 29

24. 24

44 45

.43

103. 02

100. 02

C3.

1. 33f>

.80

.10

.03

.01

' 27. 68

18.40

8.15

48.39

.30

103. 92

99.78

04.

1. 361

4.59

.04

9.14

37.20

7.97

49. 02

.45

108.41 

8.38

100. 03

C6.

Dry.

11.37

.13

.01

3.75

26.87

14.24

39.93

9.60

105. 90 

6.05

99.85

Hypothetical combination.

HaO ..................

SiOz ..................

CaCO;,.... ............

MgCOs. ..............

XC1........... ........

NaCl .................

Na 2S04 ............... 

NaaCOs ...............

NaHCO...............

Cl.

12.28

.07

.05

.48

.69

19.18

2.73 

36. 87 

27.37

99.72

C2.

10 QQ

.17

.14

.46

f>0

91 ^Id

14.18 

41.07 

10.99

100. 02

03.

69

.16

.05

02

.47

on Of:

49.13 

18.27 

1.03

99.78

04.

A 1 Q

.07

.71

60.75

16.22 

14.22 

3.88

100.03

06.

1 t Ql

13

AO

15. 20

V) 9fi

6.65 

33.69

99.85

The comparison of series 0 with A and B illustrates still further the 

rule of deposition for each of the constituent salts. In addition we
CHATARD.J NATURAL SODA. 67

see that while the percentage of chlorides in 01 is much greater than 

in the others, the amount of sulphates varies very slightly, though this 

variation may give us, important hints, as it may have an especial bearing upon the separation of the carbonates.

The relation of Na2CO3 and NaHCO3 is brought out by comparing 

the percentages of the two salts with their molecular weights, 

:N"a2CO3 =106, NaHCO3=84, which gives us the following results:

Crop 1886 ..... 

Al...... ......

Bl. ...........

Cl ............

For cent. 

Cl.

2.36 

4.84

3.70

11.97

Per cent. 

S03 .

1.07 

1.79

1.49

1.54

Per cent. NaJIC03 ; per cent. 

NajCOs.

30. 65 : 40. 87 : : 81 : 112 

30. 12 : 43. 75 : : 84 : 122

32. 47 : 42. 33 : : 84 : 109. 5

27. 37 : 36. 87 : : 84 : 113. 1

The true molecular proportion would be 84 : 106, so that in each case 

we have an excess of Na2C03, the excess being greatest in Al where the 

percentage of SO3 , 1.79, is the largest. Strictly speaking, only Al and 

Bl are really comparable, having been obtained under like condition, 

while crop 1880 was the product of a large mass of liquid, and tlie 

solution C from another locality had been boiled.

Al, as shown by the specific gravity of the mother liquor, is the product 

of a greater degree of concentration thanBl, and is less pure, which, as 

already stated, seems to fix the limit of production of a first crop, for 

Owen's Lake water, at the point where the mother liquor has reached a 

specific gravity of 1.280, or even something less, since above this point the 

ainouut of sulphates and chlorides rapidly increase without compensation by increase of carbonates.

We are now prepared to study the nature of'this combination of 

Na2CO3 and NaHCO:) on which such stress is laid, for reasons that will 

appear in the folio wing discussion:

TTRAO.

Native urao from Venezuela. The occurrence in Venezuela of this 

form of native alkali has already been described on page 40, and on 

page 35, it was stated that this material is found in many places, is of 

the greatest importance in the technology of natural soda, and would 

be treated in a separate section. Referring to page 41 for Boussiugault's 

description of this salt, and repeating the results there given, we have:

Found.

Na2O .........

002...........

H2O ..........

Impurities....

41.22 

39.00

.98

100. 00

Hypoth

Na2C03 ..... 

NaHC03 ....

HvO ........

Impurities..

comp.

46.98 

37.24

14. 80

.98

100. 00
68 WASHINGTON LABORATORY. | BULL. CO.

The impurities are insoluble matter with chlorides and sulphates, all 

of which can be deducted when we desire to calculate the formula of 

the compound as these salts are under the circumstances anhydrous 

(see page 29), hence merely diminish the percentage of urao in the 

original material.

The formula already given for urao is

Na2CO3, NaHCO3 -f 2H2O, 1

and if we deduct the impurities from Boussingault's analysis and recalculate the residue to 100 per cent, and likewise calculate the theoretical percentages for the above formula, we shall have

Na2 0 .............

COs.. .............

EbO ..............

Impurities 

deducted.

41.63

39.38

18.99

100. 00

Theoretical. 

NaaCOs NaH 

C03+2 &0.

41.15

38.94

19.91

100. 00

Difference.

+.48

+.44

 .92

Theoretical composition.

Na2CO,. ..........

NaHCO.{ ... .......

2HzO. ............

47 44

37.61

14.95

100. 00

46 90

07 -17

15.93

100. 00

+.54

+.44

-.98

Again, if we take the proportion between the 

NaHCO3 we have

Na2CO3 : NaHCO3 :: 106 : 84 :: 47.44 : 37.50,

and the

while the amount of NaHCO3 found is 37.61, a difference of only 0.11 

per cent. Hence Boussmgault's urao is an almost theoretically pure 

salt, showing only a small loss of water and a trifling increase of

Native urao from Egypt. The analysis of Egyptian soda by Berny, 

given on page 89, if calculated in the same manner, shows a remarkable agreement with the foregoing. In his original paper, Bemy gives 

as found SiO2 , 0.144; CaO, 0.078; C02, 32.1GO; SO3 , 1.210, and 01, 4.95 

per cent., hence by reducing his analysis, as given, to its constituents 

we have

; Aun; c)e Ckjrjiie, series 3, yol, 36, p. 348.
CIIATAUD.] NATDEAL SODA. 69

Insoluble ..... 

SiO, ..........

so3 . ..........

n

CO...........

CaO ......... 

Na.,0 ......... 

H20 ..........

o-ci........

'Recalculated.

4.100 

.144 

1.210 

4.950 

32. ICO 

.078 

39. 080 

19.009

101. 397 

1.110

100. 287'

Insoluble ..... 

SiO., ..........

CaC03 ........

NaCl .........

Na2S04 .......

NaHCJOs...... 

H20 ..........

Hypothetical composition.

4.100 

.144 

.20 

8.100 

2.148 

38. 45 

30.70 

16.38

100.288

-=14.758

If now we deduct from the last column the 14.758 of impurities we 

shall get column a-, if we recalculate to 100.00, column &; while if we

figure the theoretical proportions of NaHCOn and H2O required for the 

44.95 per cent, of NazCOj in &, we obtain column c, and consequently the 

differences.

NojCOs-... .......

NftHC03 ..~ ......

H20 ..............

a

38.45

30.70

16.38

85.53

b

44.95

35.90

19.15

100. 00

c

44.95

35.02

15.27

DifferC11CO.

0.00

+ .28

+3.88

True character of trona, or the native sesquicarbonate. From this it 

appears that Berny's trona, after deducting the impurities, is urao with 

a very slight excess of NaHCO3 , but 3.88 per cent, excess 'of H2O. 

Whether or not the presence of this excess of water is to be ascribed 

to the Na2SO4 will become clearer as we go on.

Klaproth1 in L802 published the following analysis of a natural soda 

from near Fezzan in the Desert of Sahara:

Na.,0 ...........

COg.... .........

H20. ............

NajSOa..........

As piiblished.

37.00

38.00

22. 50

2.50

100. 00

Impurities deducted.

37.95

38.97

23.08

100. 00

NaaC03 ........

NaHC03 ........

H20..... ........

Hypothetical 

composition.

35.88

45.90

18.10

100. 00

To this mineral the name trona has been given and it is considered as 

a native sesquicarbonate of sodium. As previously stated (page 35)

'Klaproth: Beitriige zur Clicni. Kenntniss d. Mineralkorper, III, 1802, p. 83. Also 

see Dana's Mineralogy, article Troua.
70 WASHINGTON LABORATORY. [BULL. 60.

" sesquicarbonate" is the name given to a supposed compound of 

Na2CO3 and NaHCO3 in the proportion of one molecule of Ka2CO3 

to "two of NaHCO3 , with the addition of water. As by the dualistic 

formula formerly in use sodium monocarbonate was written NaO, CO2 , 

and the bicarbonate NaO, HO, 2CO2 , the formula of the compound was 

written 2 NaO, 3 CO2 whence its name, the HO being omitted, not being 

considered an essential constituent. The formula of the theoretical 

sesqnicarbonate is 3Ta2CO3 , 2 NaHCO3 +3 H2O, which gives us the following percentages with which Klaproth's results are compared:

NajCO, .........

2NaHC03 .......

3H20 ...........

Theoretical.

32.32

£1 99

16.46

100. 00

Klaproth.

35.88

45.96

18.16

100. 00

Difference.

+3.56

5.26

+1.70

These differences are too great to be considered as slight variations 

from a theoretical formula, such as are shown by Boussingault's mineral. 

If Klaproth's trona be compared with a theoretical urao the differences 

are still larger being ^-11.02 Na2CO3, +8.79 NaHCO3 and +2.23 H2O, 

hence we see that we have here a mixture to which neither formula can 

be assigned.

Joffre1 analyzed a trona stated to have come from the same locality 

and supposed to b e the same as Klaproth's. He describes the mineral 

thus:

Incrustations of about 2 to 3 centimeters in thickness. It is in masses which are 

crystalline and perfectly white, except the lower part which, is colored by a trace of 

oxide of iron.

After giving the figures of the analysis below, he says:

The first three numbers correspond to sesquicarbonate of soda, contaminated with 

a little carbonate of soda * * * should be included in the mineral species named 

urao. The presence of carbonate of lime and of chloride of sodium may give confirmation to the views of M. Berthollet concerning the origin of natural soda, which 

he ascribes to the reaction of these two substances upon each ofcher.

NajO ...........

C02 ....... ...

H20...... .......

Sand............

Fe203 . ..........

CaC03 ..........

NaCl...... ......

Na2S04 .........

Joffre.

30 d.1

39.58

19.52

.53

.01

05

.46

.44

Impurities deducted.

40.01

40.18

10 81

Na2C03 . ........

NaHC03 ........

H20 ............

Hypothetical 

composition.

40.08

14 99

100. 00

Theoretical 

sesquicarbonate.

32.32

51.22

16. 46

100. 00

Difference.

+7.76

 6.29

1.47

1 Joffre: Bull. Societe" Chimique, vol 12, p. 102.
CKATABD.] NATURAL SODA. 71

The differences are, therefore, still greater than in Klaproth's trona, 

and in fact, as far as is known, the onlyanalyses of natural soda which 

give a composition at all near to true sesquicarbonate are those of 

Popp. 1

Popp's specimens came from Egypt, and are described as " distinctly 

crystalline salt crusts almost an inch thick," No. 1 was "an aggregate 

of small, transparent prismatic crystals, the prisms being clearly distinguishable."

CaO ..............

so3 . ..............

Cl ................

CO................

Na2O .............

HaO. .............

Deduct 0=C1.....

No. 1.

1.C5

.55

1.65

5.11

33. 15

30.34

22.50

100. 00 

1. 15

99.80

No. 2.

1.35

13. 53

20.25

1C. 55

43. 08

8.87

104. 23 

4. 50

99. 07

No. 8.

.40

37. 50

1.58

13. 50

 43. 10

4.05

.100. 19 

.35

99.84

Hypothetical composition.

Na2S04 ...........

NaCl.. ............

CaCO........ ......

Na-iCOs. ..........

NaIlC03 ... .......

H20 ..............

No. 1.

1.65

2.93

8.42

.99

25. 81

42. 00

18.00

99.80

No. 2.

1. 35

24.01

33. 38

13.40

20.93

6. CO

99.67

No. 3.

.40

66.67

2.61

10.60

17.37

2.19

99.84

Deducting impurities as before and recalculating, \ye have,

NajCOs-.-- ....... 

NaELCOj-. ........

H^O. ..............

No. 1.

30.08 

48.94

20.98

100.00

No. 2.

32.74 

51. 13

16.18

100. 00

No. 3.

35. 15 

57 59

7.26

100.00

From the composition of No. 1, Popp deduced the formula Na2CO3 , 2 

NaHOO3+4 H2O; No. 2 is close to Na2CO3 , 2NaHCO3+3 H2O, while No. 

3 approximates Na2CO3 , 2 NaHCO;! 4-H2O. The theoretical percentages

'Popp : Ann der Cliemie u. Pkarrn., vol. 155, ]>. 348.
WASHINGTON LABORATORY. [HULL. 60.

of these degrees of liydratiou and the differences from the respective 

analyses are as follows:

Na2C03 .. .......

NaHCO,......-.

H,0 ............

4H20.

30.64

48.55

20.81

100.00

Difference 

No. 1.

.56

-I- V\

+.17

........

3 H20.

32. 32

51.22

1C. 46

100. 00

Difference 

No. 2.

+.42

 .09

m

........

1H20.

36.30

57.54

6.16

100. 00

Difference 

No. 3.

1.15

+ . 05

+1.10

........

These results are very remarkable and would appear to settle affirmatively the existence of true sesqnicarbonate in nature, but we shall 

have occasion to refer to them later and give reasons for further doubt. 

The analysis of the incrustation from Brown's Station, Nev., given on 

page 56, may be disregarded in this connection, as the existence of the 

sesquicarbonate appears to have been assumed and one of the determinations obtained " by difference."

Artificial production of sesquicarbonate. The artificial production of 

sesquicarbonate has been claimed by both Winkler and Hermann.

Winkler,1 by dissolving 100 parts Na2CO3 and 152 parts NaHCO3 in 

1,920 parts of water and carefully adding 1,920 parts of 80 per cent, 

alcohol, so that the two liquids did not mix, obtained, after the lapse of 

several days, fine, transparent, non-efflorescent, acicular crystals. These 

adhered to the sides of the vessel and with them were crystals of hydrated monocarbonate and bicarbonate, the latter principally on the 

bottom. His analysis of the acicular crystals is given below.

Hermann2 mixed thoroughly ]S"a2CO3 , 10 H2O and NaHCO3 in the proportion of 1:2, melted the mixture in the water of crystallization, and

allowed the cold mass to remain in damp air for some weeks. At the 

end of that time the mass had become crystalline and its cavities were 

lined with crystals of sesquicarbo nate, which he analyzed.

Both Winkler and Hermann give as the formula of the salt, 2 ISTa2O, 

3 CO2+3H2O or Na2CO3 ,2 NaHCO3 + 2 H2O, as is shown by the analyses.

2NauO...... 

3C02 - ......

3H02 . ......

Molecular 

weight.

124 

132

54

310

Theoretical 

per cent.

40.00 

42.58

17.42

100. 00

Winkler.

41.13 

43.30

15.57

100. 00

Hermann.

40.00 

43.06

16.94

loo. oo

1 Buclmer's Repert. f. Pharm., vol. 48, p. 215. 

12 Journ. f. prakt. Chem., vol. 26, p. 312.
NATURAL SODA.

Hypothetical composition.

73

N.T,/:O, .........

2NaIlC03 ......

2H8 0. .........

Molecular 

 weight.

10G

108

36

310

Theoretical.

« 34. 20

54.19

11.01

100.00

Wiukler.

30. 33

53. 87

9.80

100. 00

Diderouco.

 

+2.13

 .32

 1.81

Hermann.

33.02

56.04

10.94

100. 00

Diflereucc.

-1.18

+1.85

 .67

.......

By following the directions given by Winkler small needles, such as 

he describes, were obtained; from these the material for analyses was 

selected with greatcare and appeared to be free from the other salts which 

had crystallized simultaneously. As the latter are sodium bicarbonate, and hydrated monocarbonate, the separation must be carefully 

made, else results may be obtained showing great variety in the proportions of the two. The amount of salt thus secured was small, but 

sufficient for the following duplicate analyses :

H20 . . .

C0a ...

Na20 . . .

a

19.19

40.01

40.69

99.89

b

19. 31

40.01

40.67

99.99

HaO ......

Na,C03 ...

NaHC03 ..

a

14.64

42.72

42. 53

99.89

b

14. 75

42.67

42. 57

99.99

Average.

14.69

42.70

42. 55

99.94

These results do not agree with those of Winkler nor with any of the 

salts described by Popp. Morever, no simple theoretical formula can 

be assigned to the combination, aud we have either ,a sesquicarbonate 

plus an excess of JSTa2OO3, or what is more probable, urao plus an excess 

of NaHCO3 .

The following table is a comparison of the foregoing analyses. As 

the proportion of water present varies for each sample, the percentage 

of £Ia2CO3, 2 NaHCO3, or as it maybe called "anhydrous sesquicarbonate," is calculated for each, and the excess, whether of monocarbonate or bicarbonate, thus shown.

Pongpo. I..---.

Wiukler ...... ....

Na,C03, 2 NaHCOaPer cent. 

62.42

73.28

74.96

77. 75

83.39

87. KG 

69. 40

Excess.

Per cent. 

18. 43 NajjCO,

11.73 Na2C03

6. 88 NazC03

1.27 NaII>:03

1.88 NaHCO,

3. 72 NaHCOa

?. 3-1 Nn^UOs
74 WASHINGTON LABORATORY. [BULL. 60.

The other analyses of natural soda which are known show still larger 

excesses of Na2CO3 than these. So far, therefore, the evidence in favor 

of the existence of sesquicarbonate is very unsatisfactory and must 

remain so until some one has succeeded in producing it by crystallization from aqueous solution by simple evaporation. My own experiments on the artificial formation of urao 1 appear to demonstrate the 

non-existence of the salt.

In addition to the analyses already given, we have Laugier's 2 examination of a Barbary soda, Pfeiffer's 3 analysis of an East Indian soda, 

and Wallace's 4 of several samples of soda from the Loonar Lake.

Wallace calls especial attention to the proportion of CO2 to Na2O as 

shown by his work, and remarks that although the text-books generally 

state that the tronafrom Egypt and other localities consisted of sodium 

sesquicarbonate, yet the analyses show that the sesquicarbonate and 

the neutral carbonate are associated in nearly equal proportions, and 

it appears likewise that under the circumstances in which the deposits 

were made, a compound of soda was formed that contains nearly four 

equivalents of soda to five of carbonic acid. In no case had he found 

the Na2O and the CO2 to be present in the proportions necessary to form 

either the neutral carbonate or the sesquicarbonate, and it is his opinion 

that lack of uniformity in stating the results of analysis was the cause 

of the error.

Tabulating the results of these analyses we have,

Woodward, Ruby Valley (p. 56) ................

Woodward, Humboldt Vallev (p. 56) ............

Pfeiffer ..........................................

Wallace, DullaKhar....... .....................

TJrao.

78.39

78.98

56.66

18.30

33.38

32.46

81.45

6.33

52.48

75.52

5.54

38.49

23.11

Excess 

NasCOj.

1.32

.17

20.59

48.48

6.50

7.84

4.55

OA OK

25.48

12.13

2.34

8.53

8.38

Urao.

100

100

100

100

100

100

100

100

100

100

100

100

100

Excess.

1.68

91

30.34

264 92

19.47

94 19

5.58

478. 00

48.55

16.06

42.24

22. 16

36.26

It is evident from the above that while, in each case, there is an 

excess of the neutral carbonate, the amount of this excess bears no 

general relation to the amount of urao or of sesquicarbonate present, 

and we must consider natural soda either as an indefinite mixture of

1 Pp. 78 et seq.

a Langier: Dingler's Polyt. Jour., vol. 18, p. 482. 

3 Pfeiffer: Journ. f. prakfc. Chemie, vol. 61, p. 439. 

4 Wallace: Chern. News, vol. xxvn, p. 203.
CHATABD.] ' - NATURAL SODA. 75

the neutral carbonate and the bicarbonate or as a certain definite 

compound of these two salts, having the composition either of urao 

(lsa2Co3,NaHCO3 ) or of sesquicarbonate (Na2CO32NaHCO3 ) generally 

intermixed with'an excess of one or the other of the two constituents.

No other combinations of these two substances have, up to the present 

time, been claimed to exist; the evidence for the sesquicarbonate has 

been given', and it remains to consider the proof of the existence of 

urao, not only as an occasionally occurring mineral, but also the sole 

natural combination of the two carbonates.

Urao from Owen's Lake. We have already discussed Boussingault's 

analysis of the original urao, and showed that this gave perpentages 

remarkably close to the theoretical for the formula

Na2C03,NaHC03+2H20, 

a>nd on page 59 reference was made to certain salts from Owen's Lake

which are now to be considered.

The "best specimen," as there stated, is the result of the spontaneous 

evaporation of the water of the lake, for although the crystallization 

occurred in an artificial ground vat and the first crop was redissolved in 

lake water, yet nothing was added to the water, and solar heat only was 

the evaporating agent. Hence such a product is purely natural in its 

character, and must be considered as a "mineral," and not as an artificial substance.

The piece examined was one of several broken from a large fragment 

of the crystal sheet covering the bottom of the vat. It was a mass 

about two inches thick, the upper portion of which was well crystallized 

and translucent; che intermediate part, an interlamination of thin 

translucent crystallized sheets and of fine granular crystalline white 

material; the bottom of the specimen is a layer similar to the upper 

part, but thinner, the crystals being much smaller.

The analysis marked "best specimen" was made from the upper 

portion, which presented a columnar radiated structure, the crystals 

being so grown together that the terminations alone were visible and 

these so combined together that each combination had a curved ridgelike termination or cockscomb form. The specific gravity of the material was 2.1473 taken in benzol at 21.7° C. The " crude" is the fine 

granular material from the central part of the specimen, and is the 

uudissolved residue of the first crop.

The "twig" urao was formed on a branching grass root which 

happened to be suspended in the water of a small natural lagune on 

the east side of the lake. It has the form of a stout twig or of a 

branching coral, each of the branches forming a cylinder, a section of 

which, shows the radiated structure, while the surface of the cylinder 

is rough, the curved edges of the crystal aggregates giving a lenticular appearance. The color is brownish, and one side of the specimen 

shows crystals of Nad and much sand, as the evaporation of the water 

finally left it lying on the mud of the bottom.
76 WASHINGTON LABORATORY. [BULL. 60.

The "lagune" specimen is from another small lagune near by, and 

consists of a thin sheet, the surfaces of which are rough like the preceding specimen. Color pink, due to organic matter. (See p. 95).

"Beach vat." This was formed in a vat dug in the beach and allowed 

to fill by seepage from the surrounding soil. Analyses of this seepage 

water will be found on page 94.

Cl ......................

so3 .....................

C02 .... .................

NajO ........... .......

B^O...... ...............

Deduct 0-C1...........

Best specimen.

.195 

.707 

38.18 

40.98 

20.12

.191 

.697 

38.11 

41.01 

20.09

38.10

20. 00

Average.

.02 

.193 

.702 

38.13 

40. 995 

20.07

100. 110 

.04

100. 07

Insoluble (inorganic) ...

SiO2 ....................

Cl............ ...........

SOS .................... .

CO2 ,... .................

Na20 ...................

CaO ....................

K2O...... ...............

MgO...... ..............

H20...... ...............

O-C1.... ...............

Crude.

.22

.10

1.57

.79

37.00

41.20

19. 62

100. 56 

.35

100. 21

Twig.

2.92 

.14

.05

2.73

.76

35.24

40.22

18.31

100. 37 

.61

99.76

Lagune.

.40 

.12

.09

.21

.63

37.50

40.08

.06

.02

19.94

99.05 

.05

99.00

Beach vat.

4.10 

.27

.04

1.83

.84

35. 10

39.36

18.58

100.12 

.41

99.71

Hypothetical composition.

Insoluble..... 

SiO, ..........

CaC03 ........

MgC03 .......

MaCl. ........

Na-jSO., .......

Na2C03 .......

NaHC03 ...... 

H20 ..........

Best 

specimen.

.02

.32,

1.25

45. 86.

36.46 

16.16

100. 07

Crude.

.22 

.10

2.58

1.39

45.28

34.74 

15.90

100. 21

Twig.

3 06

.05

-4.50

1.35

42.46

33.63 

14.71

99.76

° Lagune.

.52 

.09

.10

.04

.34

1.12

48.73

31.49 

16.57

99.00

Beach 

vat.

4.37 

.04

3.01

1.49

42.36

33.44 

15.00

99.71
CIIATAUO.J 77

Deducting NaCl and other impurities, as before, and recalculating to 

100 per cent., we have 

NiijCO,. ......

NaHCOai....- 

H20 ..........

Best

46.57

37.03 

16.40

300.00

Crude.

47.20

36. 22 

16.58

100. 00

Twig.

46.76

37.04 

 16. 20

100.00

Lagune.

32.53 

17.12

100. 00

Beach 

vat.

46.65

36.83 

16.62

100. 00

Finally, if we compare these new percentages with the theoretical 

figures for urao, already given, we shall find the following dill'ercuces:

Na2C03 ......... 

NalTCOs -..--..

H20 ............

Tlioonitiual.

40.00 

37.17

15.93

Best.

 .33

+.47

Crurlo.

+.30

OK

Twig.

-.14 

. 13

+ 97

Lagune.

+3.45 

 4 61

+1.19

Bflach 

vat.

 .25 

.34

+.59

These small differences show that each of the samples is urao. In 

each case there is a varying amount of NaCl, Na2SO4 and other impurities to be deducted, but when this is done, the residue in four out of 

the five samples has a very close agreement with the .formula of the 

mineral. In the case of the "lagune" the differences are quite large, 

but as the local circumstances attending the production of each specimen are well known, the explanation is simple.

The " best specimen," although obtained like the others by the 

spontaneous evaporation of the natural water, is, in effect, a recrystallization occuriug in a shallow basin of no great extent. The process was 

slow, the insoluble impurities had time to settle, and the product was 

gathered as soon as a tendency to deposit NaCl was observed. That 

this was successfully done is shown by the analysis, but the percentage 

of Na2SO4 is not materially different from that of the other specimens 

made under less favorable circumstances. That this is to be expected 

follows from what we know of the relative solubility of the different 

salts. The solubility of NaCl is but little affected by changes of 

temperature, which have great influence on that of the sulphate and 

carbonates. The sulphate is not only more soluble than urao, but is 

also present in much smaller proportion in this water, hence it is not 

deposited to any extent until most of the urao has separated. Afterward the relative amount rapidly increases, as has been shown by the 

series of crystallizations of the water of Owen's and Mono Lakes.

The " crude," as already stated, is that portion of the first crystallization which was not redissolved. As the first crystallization was 

alfowed. to go QQ ftil £Ta01 had been deposited iq §ome quantity, the
78 WASHINGTON LABORATORY. [BULL. CO.

increased amount of this salt is accounted for; but as the process was 

then interupted, little more sulphate is found in this than in the purest 

specimens.

The " twig'7 urao shows smaller differences from the theoretical proportions, than any of the others. The grass root on which it formed was 

suspended in the water of the shallow natural basin so that the crystallization proceeded evenly at all points. It was only when the decrease 

of the water left the specimen -lying on a mud bank that the salt 

crystals and sand adhered to it. If these impurities are deducted, the 

remainder is a practical^7 pure urao.

The "beach vat" made by spontaneous evaporation of a lye differing 

from the lake water in having a larger percentage of NaHCO3 and a 

smaller proportion of Na2SO4, is also very close in the relations of the 

urao constituents.

Finally we have the "lagune" urao. This was found on the border 

of the small lagune which was then dry. It is apparently the result of 

an interchanging concentration and dilution of the mother-liquor in 

which it was formed. As the water in such a shallow basin evaporates, 

the tendency is to leave a crust of very pure urao at the edge of the 

basin, the deposit towards the center becoming more and more impure 

as the concentrating liquid deposits its salt and sulphate, and becomes, 

as the experiments show, a comparatively pure solution of monocarbonate. If then othe basin be refilled by seepage, as would be the case 

when the lake rises, as it does in the spring, the solution would contain 

a larger proportion of the neutral carbonate, and in consequence, on reconcentration, leave on its edges a urao containing an excess of hydrated 

monocarbonate. If we calculate the amount of urao present in this 

sample we shall find that the excess of Na2CO3 and H2O is almost exactly the amount required for Na2C03+2H20,

"Lagune." TJrao.

NasC03 ......................... .48.73 = 39.73 -t-9.00

NaHCO3 ..'... ................. ...31. 49 = 31. 49

H,O ............................ .16.57 = 13.49 + 3.06 + .02

Impurities ....................... 2.21 =..... .... 2.21

99.00 = 84,71 + 12. 06 -f- 2 22

The deficiency of one per cent, in the analysis is in this respect unfortunate, but can not be easily explained. The analytical figures 

given are averages, derived from two or more closely agreeing determinations of each constituent, the list of which comprises everything that 

can be supposably present.

Artificial urao. In order to determine the conditions under which 

urao is formed, and also to find out if, by spontaneous evaporation, the 

sesquicarbonate or any other combination of the mono and bicarbonate 

might be formed, the following series of experiments was undertaken.
CHATARD.] NATURAL SODA. 79

Some of the analytical results already obtained appeared to give some 

indications of the existence of a mixed carbonate having a formula 

2Xa2OO3+NaHCO3+ xH20. If this could be separated in a pure 

state and the sesquicarbonate also obtained, we should have the following series:

............ .... .... ...... .... ...... ...... .Mouo-carbonate.

+ 1 NaHCOs . ........................... ...Supposed salt.

Na2C03 + NaHC03.-.....-.......--..-- ..-...Urao.

|NaoC03 +' NaHCOs---. ...................... .... Sesquicarbonate.

NaHCOs-- .......................... ..Bicarbonate

For this investigation a number of solutions were prepared, each of 

which contained Na2CO3, NaHCO3 , and Nad, the amount of each salt 

employed having a certain definite relation to its molecular weight. 

NaCl was used because its presence appears to exert a favorable influence on the crystallization of the mixed carbonates.

Solution No. 1 was intended to produce the "supposed salt," and was 

therefore made up as follows: 10.5 grains NaECO3 (=£ molecule) 

26.5 grams Na2CO (=£ molecule) were dissolved in water. To this solution were added 26.5 grams Na2CO3 and 29.25 grams NaCl. These 

latter amounts are purely empirical, an excess of Na2CO3 seemed to be 

needed, so that a quantity equal to that already present was added, and 

us we then have half a molecule, 29.5 grams = £ mol. NaCl was used. 

The solutions as evaporated contained:

No. 1. 10. 05 grains NaH003 = | molecule.

53. 00 grama Na^COs = \ molecule.

29.25 grams NaCl = \ molecule. 

No, 2. 21. 00 grams NatlCQj =i molecule.

53. 00 grams NaaCOs = $ molecule.

29. 25 grams NaCl = | molecule.

This proportion was expected to yield urao :

No. 3. 42. 00 grams NaHC03 = i molecule. 

53. 00 grams Na^COn = -J molecule. 

29. 25 grams NaCl = 4 molecule.

The amount of NaHC03 being twice as great as in No. 2, there was 

a possibility of the formation of sesquicarbonate.

In the course of six weeks No. 1 had deposited a crop of acicular 

crystals. The mother liquor was poured off, leaving a large group of 

small but good crystals, and a number of smaller groups. These were 

collected and carefully dried between filter paper, remaining perfectly 

transparent and unaltered in the air. In the course of another week the 

mother liquor yielded a second crop of acicular crystals.

No. 2 deposited at first' some crystalline scales, afterwards acicular 

crystals were formed ; this material was collected, and the scales were 

carefully separated from the other crystals.

No. 3 behaved like No. 2, except that the crop of scales was larger.

The salts thus obtained were analyzed, giving the following results.
80 WASHINGTON LABORATORY. [BULL. 60.

The figures for No. 1 are averages of two closely agreeing determinations of each constituent:

H20...... ...........

C02 ...... ..........

Na20. ...............

NaCl...... ..........

No.], 

first crop 

acieular.

19.58

38.73

40.07

1.46

99.84

No. 2, 

first crop 

scales.

11.78

51.69

36.54

.51

1UO. 52

Hypothetical combination.

H20...... ...... -...'.

NajC03 .............

NaHCOg...... .....

NaCl...... ..........

15.37

43.69

39.32

1.46

99.84

1.25

.42

98.34

.51

100. 52

By calculating the percentage of urao in each of these salts we find,

H20 ..........

NajCO, .......

NajHCOj .....

NaCl .........

TTrao.

14.84 '

43.69

34. G2

93. 10

No. 1.

Bicarbonate.

4.70

4.70

Residue.

.53

1.46

1.99

Urao.

.14

.42

.33

.89

No. 2.

Bicarbonate.

98.01

98.01

Residue.

1.11

.51

1.02

We see therefore that No. 1,1st crop, is urao, plus 4.70 NaHC03 , 

while in No. 2, ]st crop, the scales are nearly pure bicarbonate.

The, scales of No. 3 being in all respects similar to those of No. 2 and 

of No. 7 (to be described later), were considered as being NaHCO3 , and 

were not analyzed.

In the mean time other solutions had been prepared, in which not 

only the relative proportions of Na2C03 and NaH(JO3 were varied, but 

also that of NaCl, in order that the proper proportions of a typical 

solution for the production of urao might be determined.

For this purpose a solution of Na2CO3 was prepared, 200 cm3 of 

which contained 53 grams of the salt, the amount taken for each experiment, the other salts being added, together with sufficient water to 

effect complete solution.

Solution.

Na^COs. .....

NaHCOa......

NaCl.........

No. 4.

53.00

21.00

58.5

No. 5.

53.0

10.5

H.62

No. 6.

53.0

10.5

58.5

No. 7.

53.0

42.0

58.5

No. 8.

53. 00

5.25

58.5

No. 9.

53.00

5.25

29.25
C11ATAUO.] NATURAL SODA. 81

In preparing No. 4, the NaHCO3 was added in portions to the 200 

cm3 of Na 2OO3 solution, which was vigorously shaken after each addition, but to effect complete solution it was necessary to add water until 

the volume measured 250cm3. To this, the Nad was added, and the 

whole again shaken; an emulsion was formed which speedily became 

solid, so that the vessel could be inverted without loss. Portions of 

water were gradually added until a clear solution was obtained, the 

resulting liquid measuring 590cin3. With No. 5 the NaHCO3 dissolved 

completely without addition of water, but on putting in the NaCl and 

shaking a solid mass resulted, measuring 220cm3. Water was then 

added, and the final solution measured 300cm3 . The same phenomenon 

was observed with each of the other preparations, and all were allowed 

to spontaneously evaporate.

No. 4 deposited at first a quantity of scales, but soon begaii to form 

urao. The mother was then poured off and subsequently produced a 

large crop of urao, the mother liquor of which deposited NaCJ. in small 

but very brilliant cubes.

No. 5 formed radiating wisps or sheaves of very good and quite stout 

acicular crystals (No. 5,1st crop.) The mother liquor continued to 

form these crystals and after some time was poured off. This second 

mother liquor produced in time several large masses of apparently tabular crystals, together with a small quantity of fine needles. These 

masses were collected, and as they showed a strong tendency to effloresce and a portion placed in a small bottle became partially liquefied at 

the atmospheric temperature of 32° 0. (90° F.), there is no reason to 

doubt that they were the ordinary decahydrated salt Na2CO3 +10H2O.

No. 6 yielded a large crop of beautiful groups of radiating acicular 

crystals (No. 6, 1st crop). The mother liquor continued to form small 

acicular crystals, finally NaCl in cubes.

No. 7 deposited crystalline scales, and when acicular crystals began 

to form the mother liquor was poured off and the needles carefully 

separated from the plates (No. 7,1st crop). The mother liquor yielded 

acicular crystals and NaCl.

Nos. 8 arid 9 each deposited acicular crystals, and the mother liquor 

was poured off. The mother liquor of No. 9 formed a quantity of fine 

needles so matted together as to present a woolly appearance. (No. 9, 

2d crop).

H20...... .........

CO2 ........ .......

NajO .............

NaCl..............

No. 5, 

first crop 

acicular.

19.54

37.88

41.02

1.72

100. 1C

No. 6, 

first crop 

acicular.

19.42

37.76

39.85

2.88

99.91

No. 7, 

first crop 

scales.

11.63

51.52

36.49

Umlet.

99.64

No. 9, second 

cropuciciilar, 

matted.

18.91

36.46

39.32

5.58

100. 27

Bull. 60 G
82 WASHINGTON LABORATORY.

Hypothetical composition.

| BULL. 60.

HaO ..............

Na,C03 ...........

HaHC03 . .........

NaCl...... ........

15.96

49.00

33.48

1.72

100. 10

15.55

45.29

30.19

2.88

99.91

.92

.64

98.08

99.64

15.41

46.60

32.68

5.58

100. 27

Calculating the amount of urao as before, we get

H20 .............

Na-iCO-i-... ......

NaHC03 . ........

NaCl. ............

HSO .....

NajCOs-.

NaHC03 .

NaCl ....

No. 5, first crop.

Urao.

14.35 

42.25 

33.48

90.08

NasCOg-H-iO.

1.14 

6.75

.7.89

Residue.

.47

1.72

2.19

No. 7, first crop.

Urao.

.22

.64

.51

1.37

+NaHC03.

97.57

97.57

+Residuo.

.70

Uiidet.

' .70

No. 6, first crow.

Urao.

15.38 

45.29

35.89

96.56

NaHC03 .

.30

.30

Residue.

.17

2.88

3.05

No. 9, second crop.

Urao.

14.00 

41.24 

32.68

87. 92

+Na2C03-H20.

.91 

5.36

6.27

+Rosidue.

.50

5.58

6.08

The early products of the other solutions did not differ in physical 

properties from those examined, and were therefore not analyzed. The 

mother liquors, however, if allowed to evaporate till all the urao and

most of the NaCl had been deposited, yielded crops of the monohydrated carbonate Ka2 CO3 , H2O, as was shown by analysis; but any considerable fall in the temperature of the solution caused a crystallization of the decahydrated salt.1

From the results before us it is evident that no such compound as 

the sesquicarbonate is obtained from a solution of the two carbonates by 

spontaneous evaporati on and crystallization, and no other compound 

carbonate but urao was produced i n any of these experiments. If there 

is an excess of NaHCO3 present this will separate first, but the next

1 An abstract of these results was published in a paper on " Urao," in Am. Jour. Sci., 

vol. 38, July, 1889, p. 59 seq. The crystals obtained as above were cryatallographically examined by Mr. Edward F. Ayres, who published his results in the same 

number of the Journal. He shows that urao is monoclinic, but that the angles differ 

but slightly from those'of orthorhombic forms, and quotes Zepharovich (Zeitschrift 

f. Kryst., vol. 13, p. 135, 1887), who obtained similar results on a nrao formed accidentally by Reinitzer, Avhose analytical determinations agree with my own. Reinitzer 

gives as sp. g. 2.14, my own determination being 2.1473.
CMATAKu.] NATURAL SODA. 83

product will be urao. As the urao crystallizes upon and intermixed 

with the previously separated bicarbonate, it is clear that unless the 

two are carefully separated an analysis of the product may give results 

ranging all the way from pure bicarbonate to pure urao, or ultimately 

the neutral carbonate. The variations in the analyses of natural soda 

are thus explainable, since the bottom part of a cake of such soda 

should generally be richer in bicarbouates than the rest. This will be 

still more likely if mucliNaGl is present in the solution, since, as shown 

by No. 6, NaHCO3 was separated, although the proportion of Na2CO3 

present was four times that required for urao. In No. 5 the proportion of NaHCO3 or of NaCl is too low, as shown by the presence of 

Na2CO3 in the first crystallization. No. 9, which was considered as a 

crucial test of the possibility of the formation of the "supposed salt," 

gave even as its second crop only urao, the amount of Na2CO3, H2O 

being too small to be considered otherwise than as an impurity. The 

first products of No. 2 and No. 7 are NaHOO3 almost pure, as was also 

No. 3,1st crop, and No. 4,1st. No. 2 differs from No. 4, as does No. 3 

from No. 7, only in having one-half the quantity of NaCl; all of them 

deposited NaHCO3 , but No. 2 less than the others.

No. 1, which in amount of NaCl is midway between Nos. 5 and G, 

shows more NaHC03 than No; 6, but less NaCl. In this case the 

amount of NaCl in the solution was not sufficient to separate NaHCO3 

until the solution had become sufficiently concentrated to deposit urao, 

when both salts crystallized together. This is indicated by No. 2, 

where the increase in the amount of NaHCO3 had the effect of depositing a portion of it before the urao had formed.

That the presence of NaCl is not necessary for the formation of 

urao was proved by the following experiment. A saturated solution 

of chemically pure sodium carbonate was prepared, and into this pure 

carbonic acid was forced under pressure until a considerable amount 

of bicarbonate had been deposited. The solution was then filtered 

and put aside to evaporate spontaneously. No further separation of 

NaHCO3 was observed, and in time a crop of acicular crystals was 

obtained which on analysis yielded the following results :

Urao. Na2Co3 H20. Kosiduo. 

H2O..... 20.14 HS 0....... 1(5.33= 15.21 -f .59 + .53

NaaO.... 41.40 NaaCO.,-... 48. 35 = 44. 85 +3.50

CO....... 38.Gt) N:iHC03 ... 35.55= 35.55

100.23 100.23 95.61 4.09 .53

The salt is therefore urao with a small proportion of Na2CO3 , H2O. 

The residue of water is very nearly sufficient for the dihydrated salt, 

but in view of what has been already shown it is more reasonable to 

consider it as an excess. It will be observed that no tendency to form 

sesquicarbonate is evinced, although it would seem that the circumstances were most favorable for its production.
84 WASHINGTON LABORATORY. [BULL. 60.

Experiment has also shown that if a moderately concentrated solution of pure Na2CO3 be exposed to the air until crystallization begins, 

the first crystals obtained are urao, owing to the absorption of CO2 

from the air during the slow evaporation. It is therefore very remarkable that the voluminous literature of soda takes such slight notice 

of this salt, which must have been so frequently seen by those working 

with soda salts.1 Even Lunge's great work mentions urao but once, and 

then only as a synonym for trona, although its nature and properties 

would appear to give valuable hints for technical work.

As has been already seen, Wallace had a suspicion that such a compound existed, but Mondesir 2 has the credit of being the first to publish 

a method for its production in a pure state. After alluding to the 

doubts concerning the nature of " sesquicarbonate," he gives an account 

of his work on the mineral waters of Eoyat, in the course of which he 

established the presence of urao. In describing it he says:

This salt is very stable in saturated solutions of NaCl probably because it is only 

slightly soluble even with the aid of heat, and even on boiliug loses its acid carbonic 

acid with excessive slowness. Nevertheless a certain excess of the neutral carbonate 

is necessary for its preservation.

His method of preparation is to dissolve 28 parts of NaCl and 28 

parts of Na2CO3 .10H2O in 100 parts of water. The solution is then 

heated nearly to boiling and a thoroughly incorporated mixture of 8 parts 

NaHC03 and 28 of Na2CO3 .10H2O is gradually added in small portions, 

the liquid being continually stirred, and the loss by evaporation being 

made good by addition of distilled water. As soon as the solution is 

complete the liquid is allowed to cool slowly, when the urao crystallizes 

in fine needles. He advises that the temperature of the liquid should 

not be permitted to go below 20°0. (68°F). The salt crystallizes in 

fine needles matted together, and when treated with water, is decomposed, Na^CCs going into solution, cwhile NaHC03 is undissolved.

To this salt, which he recognizes as being the same as Boussingault's 

urao, lie gives the name "carbonate quatre-tiers," or "four-thirds carbonate," on account of the relation of OO2 to NazO. In the sesquicarbonate we haye the relation of one and one-half equivalent of CO2 to 

one equivalent of Na2O, whence its name, while in urao the relation is 

four-thirds of an equivalent of acid to one of base. It might, therefore, 

be called the " tetra-trita " or "tetrita carbonate."

Mondesir's view that the presence of NaCl and excess of Na2CO3 is 

of value in the formation of the salt is in harmony with my own results, though my work shows that the NaCl is not absolutely necessary, 

and that the aid of artificial heat can be dispensed with unless the atmospheric temperature is below 20°C. If the solution is cooled down 

below that point, the excess of Na^CO3 is liable to crystallize out as the 

decahydrated salt.

1 See note on p. 82 concerning Reinitzer's work. 

?|kjondesir? Paul de ; Comptes Rendus, Mai 31, 1887, civ. 22, p. 1505,
CHATARD.] NATUKAL SODA. 85 

ANALYTICAL METHODS.

The analytical methods employed in these analyses are iu general 

well known. The salts and solutions necessarily contain only traces 

of other bases beside alkalies, and those were determined in the usual 

manner. Silica may exist in some quantity, but the amount is usually 

small.

SO3 and 01 were determined gravimetrically and in duplicate, the 

results agreeing in most cases very closely. When SO3 is precipitated 

by BaCl2 in such solutions containing alkaline salts only, and these in 

small quantities, and care is taken that the precipitant is iu slight 

excess only, the precipitation is both rapid and complete and the 

precipitate is pure, the after treatment with HOI rarely showing a loss 

of any consequence.

The C02 was determined by distillation, the gas being collected and 

weighed in a Liebig potash bulb, and the apparatus and method are 

fully described in "Analyses of waters-of the Yellowstone National 

Park." Gooch and Whitfield, Bulletin No. 47, TJ. S. Geol. Survey, p. 15. 

With care and experience the results agree very closely. For the boric 

acid, in the water of Owen's Lake, the excellent method of Gooch 1 was 

followed; for the Mono and Eagtown waters the process ot Stromeyer, 

with modifications of my own, was used; but, though giving very fair 

results, the process can not be compared for ease, simplicity, and accuracy 

with the former method.

The determination of the alkalies in such very dense, waters was, at 

first, found to be difficult, owing to the large quantities necessarily 

taken. To get determinations which shall be fairly accurate when referred to a liter, portions of not less than 50cm3 should be taken, the 

water in all cases being carefully weighed. The amount of alkaline 

chlorides corresponding to 50cm3 of such waters is very large, and, 

when the final evaporations are being made, there is great liability to 

loss, owing to the formation of a salt crust on the surface of the liquid 

and subsequent spirting, caused by steam and ammonia vapor produced 

under the crust. This takes place no matter how carefully the evaporation be carried on, and many determinations were thus lost.

The use of hydrochloric acid enables us, however, to completely 

obviate this difficulty. The purified alkaline chlorides are to be evaporated till crystallization begins; the platinum vessel is then removed 

from the water bath, and an equal bulk of very pure, highly concentrated hydrochloric acid added to the solution. A copious precipitation of finely granular salts at once ensues, and, on replacing the vessel 

on the water bath, evaporation goes on quietly and rapidly, no salt 

crust is formed, and when the final heating is given, little decrepitation occurs. In this manner it is as easy to handle several grams of

'Gooch: Proc. Am. Acad. Sci., 1886, p. 167.
86 WASHINGTON LABORATORY. [BULL. 60.

chlorides and to obtain accurate determinations as it is when we have 

to deal with the far smaller quantities usual in mineral analysis.

The water in the salts was determined by means of the apparatus 

figured. A is a combustion tube drawn out and bent at a right angle. 

The platinum boat B, containing the salt, rests upon the thin sheet of 

asbestos paper 0, used to prevent adhesion between the platinum and 

the heated glass. D is a roll of asbestos paper wrapped with thin 

platinum wire, which fits loosely in the tube and prevents back currents of air during the heating. The bent end of the combustion tube 

enters one limb of the (J tube E, which is my own form, and differs, as 

the drawing shows, materially from the forms now on the market, in 

having an especially large bulb at the bottom. The two limbs of this 

tube are filled with glass beads wet with strong sulphuric acid. Sufficient acid should be put in so that the narrow tubes are filled up to the 

bends and the air forced to bubble through.

FIG. 4. Apparatus for determination of water.

In using the apparatus the tube is thoroughly heated and then 

allowed to cool, a current of perfectly dried air being continually passed 

through it. The part of the tube where the boat is placed is protected 

by a semi-cylinder of sheet-iron lined with asbestos paper.

The (J tube, having been weighed, is then attached to the combustion tube as shown and the air current regulated. The platinum boat 

which has been heated and then cooled in a desiccator, is now weighed 

and about one grain of the salt put into it and spread evenly along 

the bottom. The salt should be very finely pulverized to prevent decrepitation on heating. The boat with its contents having been weighed, 

it should at once be inserted into the tube and the asbestos plug 13- 

which has been highly heated and should still be hot, shoved in close 

behind the boat.

The tube is now heated gradually, beginning at the plug. As the 

water in such salts is driven out in great part at a low temperature 

the heating must be done cautiously and the air current watched, since, 

if it is too slow, water may condense in the cold part of the tube behind 

the plug. This regulation of the air current is the more difficult, since 

the acid CO2 of the bicarbonate is set free simultaneously with the
CHATAUD.] NATURAL SODA. 87

water, but upon it and the gradual heating depends the success of the 

operation.

The water bath F, of which F1 is a top view, is now pub into position, 

so that one limb of the U tube fits into the curved recess in the sido of 

the bath. A small alcohol lamp keeps the bath hot, so that the water 

driven out of the salt may not condense in the upper part of the limb. 

By the use of this bath the time of the operation is much shortened.

As soon as that part of the tube containing the boat appears free 

from condensed water it should be highly heated until all the moisture 

has disappeared from the drawn-out portion. This will generally take 

from twenty minutes to half an hour, and when completed the water bath 

is removed and the apparatus allowed to cool, the air current being 

still kept up. As soon as the tube is cool the (J tube is disconnected 

and the boat removed and placed in a small, well-stoppered glass tube,

which has been weighed. The increase of weight of the JJ tube gives 

he aniouut of water in the sample, while the weight of the small tube 

containing the boat and calcined salt, if subtracted from the sum of 

the weights of the boat, the salt taken and the weighing tube shows a 

loss which is the water plus the acid 002 of the bicarbonate. The 

calcined salt which should be sintered together, but not fused, can then 

be used either for a determination of the residual C02 or, as is usually 

done, dissolved and the alkali determined by standard sulphuric acid, 

methyl orange being used as the indicator, the same portion being then 

used for the Cl determination.

Many attempts were made to collect and weigh the C02 driven off by 

heat, but it was found impracticable to do so without at the same time 

sacrificing the water determination. No matter how carefully the heat 

and air current are regulated, the CO2 comes off too rapidly for proper 

absorption in the potash bulb, and if the air current is too slow, water 

condenses back of the plug and this determination is too low.

When no attempt is made to absorb the OO2 the results are very 

satisfactory. In the analysis of urao " best specimen " given on page 

7G, we have as the mean of three closely agreeing CO2 determinations 

38.13 per cent., while two determinations of the alkali gave 40.28 per 

cent., equivalent to 28.58 per cent, of CO2 required to make mouocarbonate. Deducting, this amount from that of the total C02 we have 

9.55 per cent, as the acid OO2 of the bicarbonate present. The determinations with the above described apparatus gave the following 

results:

Salt taken.

1. 0040

1. O'lOO

1. 158.3

I. 0638

Loss of 

boat.

29. fit

29.58

29. 49

29. 53

H20.

20. 12

20.09

20. 00

20.07

Differonco=C02.

9.39

9.49

9.49

9. 40
WASHINGTON LABORATORY.

We have therefore as average 9.46 per cent. CO2 found, which being 

deducted from the calculated amount 9.55, leaves an excess of 0.09 per 

cent, not driven off.

In another sample of urao:

Salt takeii.

1. 1801

1. 2297

1. 20G6

1. 0880

1. 1761

Loss of 

boat.

29. 27

29. 35

29.39

29.20

29.32

H2 0.

19.80

19.83

19.85

19.80

19.82

Difference CO;;.

8.47

9.52

9.54

9.46

9.50

C0a in 

residue.

28.69

28.64

28.49

28.67

28.62

Sum of 

C0a .

38.16

38.16

38.03

38.13

38.12

Two determinations of total CO2 gave 38.17 and 38.22 per cent. 

average 38.19. Two determinations of alkali gave 40.19 and 40.22 per 

cent. Na2O, average 40.20 equivalent to 28.53 per cent. CO2 . Hence, as 

28.62 per cent. CO2 was found in the residue and only 28.53 was necessary for the combination Na2CO3 , we have 28.62 28.53=0.09 per cent. 

(3O2 not driven off.

In a sample of Trommsdorff's 0. P. sodium bicarbonate there was 

found:

Salt 

taken.

1.4265

1. 5995

1. 3200 

1. 3723

1. 4296

Loss of 

boat.

36. 68

36. 81

36.71 

36.73

36.73

H20.

10.91

10.90

10.91 

10.98

10.92

Difference^ 02 .

25.77

25.91

25.80 

25. 75

25.81

C02 in

residue.

26.25 

26.37

26.31

Sum of 

COS .

52.05 

52.12

52.09

Two determinations of total C02 gave 52.06 and 51.90, average 51.98 

per cent. Two determinations of alkali gave 36.86 and 36.90, average 

30.88 per cent. Na2O, equivalent to 26.17 per cent. CO2. Subtracting 

26.17 from 26.31, the average amount in the residue, we have 0.14 per 

cent. CO2 not expelled by heating to the sintering point.

Comparing these amounts of excess of CU2 retained by the residues 

of the ignition, we find the following relation :

Sample.

TJrao, No. 2 .........

Number of 

determinations.

3

4

4

Average 

weight 

taken.

I. 0638

1. 1761

1. 4296

Average 

excess, 

per cent.

0.09

0.09

0.14

Relation of 

excess to 

weight.

0.084

0.077

0.091

0.084

Hence we may say that if sodium bicarbonate, or a salt containing a 

large proportion of it, is heated till it sinters without fusing, and is 

kept at that temperature for one hour, it still retains CO2 in excess of 

the amount required to form monocarbonate with the alkali present,
CIIATABD.] NATUKAL SODA. 89

and that for quantities of from 1 to L.5 grams this excess may be 

considered as one-tenth of one per cent, of the weight of the salt taken. 

For an analysis of sodium bicarbonate by means of this method it 

is therefore sufficient to determine the loss by ignition, the H2O, and 

the alkali in the ignited residue to obtain the total amount of CO2 in 

the sample, adding in an amount of CO2 equal to 0.10 per cent, of the 

weight of the salt taken. This method for the analysis of bicarbonate, 

or " baking soda " is much more rapid, far easier and quite as accurate 

as the distillation process, and may prove of value for technical purposes.

ORIGIN OF NATURAL SODA.

We have seen that this material occurs in many widely separated 

localities, which have, perhaps, but one characteristic in common,

namely, a very dry climate. The presence of volcanic rocks belonging

to late geologic periods, though proved in many instances, has not as 

yet been shown for a few of them, such as Hungary and Egypt.

Dryness of climate has no other effect, probably, than to retain within 

a given region its product of natural soda, which would otherwise be 

continually carried off to the sea through natural drainage, though the 

consequent inclusion of the drainage in closed basins may be necessary 

to permit of certain chemical after-reactions.

lu an arid region like our Great Basin, but a small portion of the 

total rainfall reaches the ocean. Eivers of considerable magnitude terminate in "sinks" or lakes without outlet. Such lakes are naturally 

impregnated with salts, since each drop of inflow brings its quota, and 

the only loss that such a basin suffers is by evaporation, which carries 

off no solid matter.

Unless chemical changes occur in the lake itself, such a body of water 

represents a simple concentration of its inflowing streams, and if we 

find it to contain any given salt, it is evident that this salt has either 

been brought as such into the basin, or is a product of chemical afterreactions among the constituents of the lake water. If the salt has 

been brought as such it is a product of rock or soil decomposition, and 

is in solution as a result of a leaching process, whether the water came 

from a deep seated spring or is a mere surface drainage.

The existence of springs carrying sodium carbonate is well-known, 

since many of them have a world-wide reputation for their medicinal 

qualities. Although most of them are weak solutions, a comparison 

of their compositions with those of the waters described in this paper 

will show that they would by sufficient evaporation yield a very pure 

natural soda. The sodium carbonate in such springs is produced by 

decomposition of the alkali-bearing rocks through which the water flows, 

and this decomposition is brought about by the combined action of air 

and moisture, aided in many instances by heat and pressure.

The air absorbed by water contains a much larger proportion of oxy-
90 WASHINGTON LABORATORY. [BULL. GO.

geu and carbonic acid than the normal atmosphere, the composition of 

which may betaken as

Oxygen..................;...... .......................... 20.9512

Nitrogen................. ................................ 79.0073

Carbonic acid............................................ 0.0415

while the air absorbed by water at 15° C. (60° F.) contains, according 

to Buusen,

Oxygen.................................................... 34.12

Nitrogen................................................... 63.62

Carbonic acid.............................................. 2.26

The alkali-bearing minerals are generally silicates, having for bases 

ferrous or ferric oxide, alumina, lime, magnesia, soda and potash in 

varying proportions according to the character of the mineral. Thus 

ortboclase feldspar is composed, essentially, of silica, alumina and 

potash; albite, of silica, alumina and soda; anorthite, of silica, alumina 

and lime, but they are rarely found pure and there exist many intermediate steps, so that orthoclase usually contains soda and lirne in varying proportions, while magnesia and ferric oxide replace in part lime 

and alumina respectively.

By the action of water, containing carbonic acid, upon such minerals, 

the alkalies and alkaline earths are converted into carbonates and dissolve in the carbonated water. Hence they are leached out of the residue, which is rendered the more porous through the decomposition, and 

if the water so charged does not 011 its way to the surface meet with 

sulphates or chlorides of other metals which, by double decomposition, 

would produce alkaline sulphates or chlorides and non-alkaline carbonates, the alkaline carbonates make their appearance as constituents of 

a mineral spring. In such springs the salts of sodium are usually in 

much greater proportion than those of potassium, not only because the 

soda minerals are, in general, more easily decomposable, but also because 

soils have a strong tendency to take up and retain the potash salts from 

water percolating through them while readily giving up their contents 

of soda salts.

If the waters of such springs flow into basins without outlet and the 

rate of evaporation equals the inflow, a concentrated solution gradually 

results, and if the inflow be interrupted, we shall in time have a dry 

basin in which the salts have deposited as a crystallized mass. It is 

evident that if the geological character of a country is favorable to the 

production of such alkaline springs, the dryness of the climate or the 

excess of evaporation over rainfall determines the degree of concentration of the contents of their basins, the number of which is dependent 

on the topography, and the consequent productiveness of the region in 

natural soda.

We have so far considered original formation and simple evaporation 

only. There are, however, a number of instances in which the alkali 

appears to be the result of more complicated chemical reactions. We 

have already seen the views of Szabo and Moser as to the mode of
CHATAHD.] NATURAL SODA. 91

origin of the Hungarian soda, in which the carbonate of lime is supposed to play a part, Luuge' refers to the fact that from a damp mixture of common salt and lime soda effloresces in the air after several 

weeks' time, and also states that " from a solution of common salt a solution of bicarbonate of lime precipitates sodium bicarbonate; apparently 

this reaction explains the formal ion of soda efflorescence in soils containing common salt." If the more soluble magnesium bicarbonate be 

substituted for the calcium salt we have Weldon's process for soda 

making.

It may therefore be said that if common salt and limestone or dolomite are present together in a soil, subject to the action of air, moisture 

and climate, all the conditions for the production of natural soda are 

at hand, and it is thus that the origin of the soda of Egypt may be 

explained. Kussegger's description of this locality has already been

cited. After ascribing the formation of the sodium carbonate to reactions occurring between the CaCO3 Na2SO4 and Nad, by which Na^COs 

Ca012 and CaS04 are formed, he says:

The first two (Na^COs and CaCl2 ) dissolve in the water of the lakes together with 

the undecoraposed NaaSQj and'NaCl, and thus we have a lye containing Nad, 

NaaS04, NasCos and CaCl2 .

A very slight knowledge of chemistry tells us that Na^COs and CaCl2 

cannot exist together in solution, since CaCO3 must be precipitated at 

once, NaOl remaining in solution; so Karsten (loc. cit.) adds the following note:

This transformation of the salts is undoubtedly a consequence of the oxydation of 

the pyrites in the clay to sulphates, followed by a double decomposition of these sulphates by the NaCl and CaCOs in the clay. The sodium and calcium sulphates so 

formed are then reduced to sodium and calcium sulphides and these are decomposed 

by means of NaCl and CaCO;) . The process must, therefore, be considered as very 

complicated and as demanding nob only length of time but also a co-operation of 

special conditions, precisely as they occur in the Egyptian lakes. The organic matter hero present may well be considered as the sole and only cause whereby the sulphates are reduced to sulphides, these being changed then to carbonates.

Abich, in his description of the Armenian localities, already given in 

part, ascribes the formation of the sodium carbonate there found more 

particularly to the action of plant life. The salt grasses and other 

plants which grow in that region yield an ash rich in soda salts, those 

from Armenia being richer in Na2CO3, while those from the Steppes 

contain a larger proportion of Na2SO4. The soil of the Steppes contains much Nai2SO4, but is poor in NaCl, precisely the re verse of the soil 

of Armenia; hence the conclusion that the Na2CO3 is formed by the 

action of the plant on NaCl, comparable with the formation of potassium carbonate, which usually predominates in the ash of land plants. 

The growth, death and decomposition of successive crops of such plants 

would, under this view, continually increase the amount of sodium carbonate in the soil without taking into consideration the amount pro1 Lunge: Sulph. Acid and Alkali, Vol. 2, p. 310.
92 WASHINGTON LABORATORY. [BULL. 60.

duced by direct weathering of the eruptive rocks so abundant in that 

region.

We have already seen that the deposits of Wyoming consist in great 

part of sulphates and chlorides, though occasionally the percentage of 

carbonate becomes sufficiently large to be of importance. This is also 

true of the Lake Bonneville region as described by King in the 40th 

Parallel report, already frequently quoted. In vol. 1, page 500, he 

shows that the salts are mainly chlorides and sulphates, the former 

largely predominating, while carbonates are generally absent. The 

water of the Great Salt Lake may therefore be taken as typical for the 

region. As one proceeds westwardly the occurrences of alkaline carbonates are more frequent and the percentage of this salt greater until 

we reach the Lahontan region of western Nevada, where the proportion of alkaline carbonate is usually greater than that of sulphate.

The cause of this chemical change in the nature of the salts, though 

much discussed, is not yet ascertained. So far as we know, there is no 

such difference between the rocks of the eastern and the western portion of the Great Basin as would account for this increase of the carbonate. In both sections the eruptive rocks are of similar character, 

and, by their decomposition, should yield the same products. It is possible that the fact that volcanic action has persisted to a much later 

date on the western border than on the eastern side may have some 

influence. Hot springs are much more common along the foot of the 

Sierra Nevada, and some of the volcanoes have been active at a comparatively recent date. The enormous volume and high temperatures 

of the heated waters of the Com stock Lode may also be considered as 

showing a probably greater activity in rock decomposition but not, 

necessarily, a difference in character of product.

Once formed through rock decomposition, a solution containing 

sodium chloride, sulphate and carbonate would afterwards lose none

of its carbonate unless soluble earthy salts were added to it; on the 

contrary, when such a water reaches an enclosed basin, the proportion 

of sodium carbonate tends, following the views of Karsten, to increase 

through the reduction of the sulphate by organic matter and the subsequent action of the atmospheric carbonic acid on the sulphide; a reaction which requires a period of comparative rest, which such a basin 

affords. It has been already stated that the waters of springs carrying alkaline carbonate may lose the whole of it on the way to the surface 

by passing through formations containing non-alkaline soluble salts, 

snch as gypsum, calcium chloride or magnesium salts, resulting in the 

formation of calcium or magnesium carbonate and alkaline sulphate or 

chloride. The same reaction would occur if the surface water percolates through soils containing these salts, or if water containing them 

be added to the streams or basins.

It is probable that an alkaline lake or the dry deposit resulting from 

its desiccation is in all cases the result of both primary rock decomposition 

and .subsequent chemical change. The latter usually appears to be the
NATURAL SODA. 93

subordinate agent, but still occupies a definite position, and in this connection the results of the examination of certain seepage waters from the 

shore of Owen's Lake are interesting. The analysis of the water of 

this lake shows that sulphides are absent, the most careful tests showing merely a doubtful trace. On page 76, a urao was described as 

having been produced from seepage water collected in a vat dug on the 

beach and for practical reasons it was desirable to study the nature of 

the seepage. To this end, small pits were dug in a line extending 

from the vat to a point much above the highest recent water mark of 

the lake. From each of these pits,. beginning with the one most 

distant from the lake, a sample of the seepage water was taken and the 

specific gravity tested, as follows:

Sample.

TSo.1.... ............

INo.2...... ..........

No.3................

No.4...... ..........

No.5...... ..........

!No.6...... .........

iNo.7...... ..........

No. 8.. ..............

Temperature.

°C. 

32

31

31

32

v>

V)

31

Ql

25

Specific 

gravity.

1.005

1.035

1.050

1.050

1.062

1.090

1.108

1.085

1.063

1.062

Kern ark a.

Do.

The soil of these pits showed no variety; in each case it was found 

that the surface sand was underlaid by a dark grey material similar to 

a very sandy clay and closely resembling the " volcanic ash" common 

in this section, and which it is considered to be. A sample was taken 

from pit No. 9 and analysed as follows, having been partially dried, 

when it became pulverulent and of a pale yellowish grey color.

H20 at 110°. ...........

C02 iri Holnblo part ....

C02 in insoluble part . .

so3 ...... ..............

Cl. ....................

Si02 . ..................

Tin

PA- ..................

Al,0f--. ..............

FoA . ..............

FoO. ....... ...........

MnO ..................

CaO. ..................

MgO ..................

K20. ..................

Na20 ..................

0-C1. ................

.65 

2.50

.87

6.35

.45

CO

.... 55.81

.80

97

.... 10.07

3.43-

.67

91

9.14

2 99

2 OQ

3.09

100.41

.20 

100.21

H2O ....

NaCl

Na,S04 .

Na2C03 .

CaC03 .-

Si02 -..-

Ti02 ...-

P20S ..~

A1203 -.-

JFo203 ...

FoO ....

MiiO....

CaO ....

MgO....

K2O ...

Na-fO ...

...................

Sohible part. 

........... 1.45

........... .80

........... 55.81

........... .80

........... .27

........... 10.07

........... 3.43

........... .67

........... .23

........... 1.05

........... 2.22

........... 2.98

........... .75

3.15

4 34

14.44

78.28 

100.21
WASHINGTON LABORATORY.

Analyses of the samples of seepage water.

[HULL. 60.

Specific gravity 

and temperature.

In 1 liter.

C1-... .............

<»n

0 .................

C02 .~. ...........

0... .............

K. ................

Na....... .........

Si02 . ..............

A1203 .............

Ca. ...............

Mg ...............

B203 .... ..........

H...... ...........

Pit No. 5.

1.06872 (22.5° 0.)

Weight.

24.31C 

G.092 

1.210

15. 172

5. 510 

2.352 

32. 064 

0.290

present 

.072

87. 096

Per cent.

27.92 

0.99 

1.40

17.42 

6.33 

2.70 

36.82 

.34

.08

100. 00

Pit No. 8.

1.0881 (24.1° c.)

Weight.

29. 412 

8.604 

1.732 

.120 

21. 100 

7.672 

2.612 

41. 896 

.316 

.008 

.020 

.009 

undot .. 

.120

113. 681

Per cent.

25.87 

7.62 

. 1.52 

.11 

18.56 

6.75 

2.30 

36.85 

.28 

.007 

.02 

.008

.105

100. 00

Pit No. 9.

1.07308 (21° C.)

Weight.

23. 808 

4.936 

.988 

.161 

19. 320 

7.024 

2.020 

33. 420 

.200 

.008 

.014

undet .. 

.170

92. 142

Per cent.

25.84 

5.36 

1.08 

.17 

20.97 

7.63 

2.20 

30.24 

.29 

.01 

.015

.20

100. 00

Hypothetical combination.

Si02 . ....... .... r .

A1203 . ............

CaC03 .... ........

MgCO, .........

KOI ..............

NaCl .............

ffjbS04 . . .........

Na2S..............

Na2C03 ..........

NaHC03 ..........

Weight.

.290

4.487

36. 549

10.812

28. 876

6.076

87. 096

Per cent.

.34

5.15

41.96

' 12. 41

33.17

6.97

100. 00

Weight.

.310

.008

.044

4.091

44.545

15. 370

37.884

10. 192

113. 681

Per cent.

.28

I no )

4.39

39.18

13.52

.26

33.33

8.96

100. 00

Weight.

f .008

 1 . 032

3.864

36. 199

8.757

27. 817

14.813

92. 142

Per cent.

Oft 1-

4.19

39.28

9.49

30.19

16.08

100. 00

In comparing these analyses we must remember that the water here 

examined is not the lake water, but the drainage from fresh springs 

along the base of the Inyo Range. As the water passes through the 

volcanic ash it gradually becomes laden with the salts produced by 

the decomposition of the soil as shown by No. 5. At this point the 

amount of sulphur or sulphuretted hydrogen present, though small, was 

unmistakable, showing that a reduction of sulphates had begun. In 

No. 8 the percentage of chlorides had diminished, and that of bicarbonate had increased, while the percentage of sulphates was somewhat 

larger, although sulphides were present in weighable quantities. No. 9 

is very regular in its results if compared with No. 5. The chloride and 

sulphates have suffered a considerable decrease, while sulphides are in
oiiATAiiD.] NATURAL SODA. 95

as large a proportion as we should expect, considering that they would 

be destroyed at once ifiii solution with bicarbonates. The sodium 

monocarbonate is apparently less in amount than in the first analysis, 

but we observe a great increase in bicarbonate, so the percentage of 

alkali in the last analysis shows a large gain over the first one. As the 

distance from one pit to the next was uot more than a hundred yards, 

this process of alkali production is really quite a rapid one, and the 

solutions obtained are stronger and of better quality for practical purposes than the mass of the lake water.

CAUSE OF THE BED COLOR OF CONCENTRATED ALKALINE BRINES 

AND OF THE SALTS OBTAINED FROM THEM.

The red color which brines, particularly those of an alkaline character, are apt to assume when concentrated, and which is frequently

taken up by the deposited salts, has often been noticed. The cause of 

this color has been studied by Payeri,1 who finds that it is due to the 

presence of the small crustacean, Arteiuia salina, Leach (Cancer saliuus, 

Linn.), known in the West as the "alkali shrimp." In his experiments 

carried on at the Salines of Marignano, he found that the brine in concentrating to 15° B. becomes entirely clear and colorless, continuing 

until it reaches 20° B., at which point large numbers of small animals, 

grey or greenish grey in color, are observed swimming in the liquid. 

As the brine concentrates to nearly 25° B. all of these little crustaceans 

die, turn red, come to the surface and form a red foam, which is composed 

of the fragments of their bodies and gives a peculiar odor. Experiments showed that if the concentration of the brine did not exceed 

20° B. the animals were healthy, provided that they had air and that the 

solution did not become acid. If the solution became acid, the animals 

became sluggish and moribund, but were i evived as soon as the solution 

was rendered alkaline.

The same may be said of the brine at 15° B. For a short time the 

animals were very lively, but on the fourth day became sluggish. 

Rendering the solution alkaline revived them to some degree, and on 

reducing a portion of the solution to 3° B. the Crustacea in it remained 

alive and vigorous up to the time when the paper was written.

Those in the solution at 20° B. were lively during two days, then 

began to die, and all were dead on the third day. In fresh water all 

died within four days. In solutions at 23° B. all died within twentyfour hours, having become much redder than in the weaker solutions, 

sind settled on the bottom as a brown sediment. These experiments 

show that a certain degree of concentration and a certain degree of 

alkalinity are necessary for the life of these animals, and that greater 

concentration cruses death and the consequent red coloration.

The letter of Audouin accompanying the paper gives the observa-

'Payen: Ann. de Chimie, pt. 2} vol. 65, pp. 156-169,
96 WASHINGTON LABORATORY. [HULL. GO.

tions of Schlosser made at Lymington, England, in October, 1755. The 

latter describes these animals as follows:

The body is merely a tube, cylindrical or vermicular in form, very slender, and 

about one-third of an inch in length. At one end of this tube are two antennae, very 

delicate and short, and two black eyes, round and elevated ; between these eyes is a 

black spot, which may be a third eye. A curved month is placed under the eyes. The 

body is provided with 21 pairs of natatory legs, the longest being in the center of 

the body, the others becoming shorter as they approach the head and tail. The posterior part is bare, the anus being at the extremity. The females have posterior to 

the last pair of legs a sac, usually three or four times the diameter of the tube, containing eggs; the males have, anterior to the first pair of legs, two long flattened 

arms, with these they seize the females, and while attached to them appear to squeeze 

out several eggs. The animals thus attached swim together for some time.

D'Arcet observed the red color of the Egyptian lakes, but finding 

only a few arteinia, did not consider that the color was due to them,, 

In the West the arteinia are very plentiful and the red color is very 

usual, though generally ascribed to some property of the salt grasses. 

It is probable that the opinion of Payen is the correct explanation.

LEACHING OF ALKALINE SOILS AND CLAYS.

A chemical examination of a soil always includes a leaching with 

water and the analysis of the soluble portion. This is especially necessary in the case of samples from alkaline terranes, where the percentage of soluble salts is often large, and unless these can be extracted 

without alteration, no correct conclusion can be drawn as to the character and agricultural possibilities of the soil. In such regions crops 

can seldom be grown without irrigation, which not only supplies the 

plants with the necessary moisture, but also improves the laud by leaching out the surplus salts, which may, under exceptional circumstances, 

be profitably recovered from the teachings.

The extraction of the soluble constituents from such soils and clays 

is often difficult, because when the sample is mixed with water subsidence is exceedingly slow, and filtration, if at all practicable, yields a 

very turbid solution. Having to examine a number of such samples, 

experiments were made to find out the simplest method of securing a 

clear aqueous solution containing only the naturally soluble salts. The 

presisteut turbidity seems to be in some way connected with the 

alkalinity of the solution, since if this is rendered slightly acid, subsidence is rapid and a clear liquid is easily obtained. By acidifying, 

however, all the carbonates are decomposed and the resulting solution 

tells us nothing concerning the character of the original material.

It is well known that sea water precipitates the finely divided 

suspended material from inflowing river waters, and experiments based 

on this observation have 3hown that the addition of a small proportion 

of pure sodium chloride is all that is needed to obtain a clear and unaltered solution. Three samples of so-called ' clays" from Owen's 

Lake have been especially examined for this purpose.
CHATAKD.] NATURAL SODA. 97

In making vats at the soda works at this place it was found that some 

of them could not be rendered water tight without great expense, and 

the reason of this was sought. Sample No. 1 represents this class of 

ground, while the combination of Nos. 2 and 3 is "good ground," holding water without difficulty. If the samples are dried the difference is 

strongly marked, No. 1 becoming very friable, while the others are as 

tenacious as a brick clay of inferior quality. If the dried samples are 

mixed with a little water all become pasty, but if much water is added 

the emulsion of No. 1 subsides rapidly, a few hours being amply sufficient to give a clear supernatant liquid, which can be poured off without 

disturbing the compact underlying sediment. Under like conditions 

Nos. 2 aud 3 remain turbid, and after the lapse of thirty days not more 

than one-tenth of the supernatant liquid was even approximately clear. 

By the addition of a sufficient amount of common salt the subsidence

was rendered as rapid and as complete as in No. 1, and the sediments 

can be washed by decantation. For the determination of chlorine, 

dilute nitric acid is added till the solution becomes acid, producing the 

same effect as the addition of common salt.

No. 1 is from the " upper works " at Keeler, Owen's Lake. It is covered 

by the surface sand, is yellowish grey in color aud, as stated, friable. 

No. 2 is "sandy clay " from the "central works." This is immediately 

under the surface sand, is about 12 to 18 inches thick, and is said to be 

the best for vat-making; underlying this is the " blue clay," No. 3, of 

undetermined depth and also very good. Analysis gave the following 

results:

H2Oatl'JO°.......

H'.jO at rod lieat. . . 

SiO, ..............

Ti02 ...... ........

Al,0.t .. ........... 

Fe2 0s --.. - ---- 

FeO ..............

MnO. .............

CaO ..............

MjiO...... ........ 

KnO ..............

Na 20 .............

S03 . ..............

(Jl ..............

CO...............

No. 1.

4.02 

1.18 

45. 83 

.30 

8.05 

2.77 

.43 

.12 

4.88 

1.23 

2.86 

14.21 

1. 85 

7.33 

0.44

101. 50 

1.65

99.85

No. 2.

1.41 

2.73 

53. 24 

.25 

10.81 

2.09 

.77 

.10 

9.18 

5. 82 

2.64 

2.06 

.08 

.05 

8.75

100.51 

.01

100. 50

No. 3.

2.05 

2. 40- 

54. U2 

.30 

11.25 

2.77 

.94 

.08 

8.70 

4. Ul 

2'.77 

2.10 

trace, 

trace. 

7.21

100. 49 

.49

100. 00

Wnter...... ......

Solulilo part ...... 

<Ja<J03 . ...........

No. 1.

5.08 

24.80 

0.18 

63. 79

99. 85

No. 2.

4.14 

1.20

19. 07

70. 03

100. 5U

No. 3.

4.45 

1.41 

15. 34 

79.29

100. 4'J

Composition of soluble part.

Soluble.

KC1 ..............

NaUl .............

Na2SOj ...........

Na2COg . .......... 

NaHCOs--- .......

Si02 .:............

A1203 . ............

No. 1.

4 13

11. 15

3.30 

7.50 

1.17

.39 

.11

24.80

No. 2.

09

.14 

.87

.10

No. 3.

1.18

.23

1.20 ( 1.41

Bull. 60-
98 WASHINGTON LABORATORY. [BULL.GO.

No. 1 is evidently in great part sand, made up of quartz and small 

grains of eruptive rocks, and contains but little real clay. Hence it 

absorbs large quantities of soluble salts, but parts with them readily 

on leaching, leaving a porous residue, which, on account of its granular 

condition, subsides rapidly when mixed with water. Nos. 2 and 3 contain only small quantities of soluble salts, but chlorides are practically 

absent, and the residues containing considerable quantities of carbonate 

of lime may be viewed as marls.

The clarification by the use of Nad must be considered as a physical 

phenomenon since, so far as our present knowledge extends, no chemical change is supposable under the conditions. In each of the following experiments, begun September 11, 1888, the air dried material was 

weighed out and put into a cylinder containing the given amount of 

salt dissolved in 50cm3 of water. The cylinder was then corked, shaken 

vigorously and allowed to stand without further disturbance.

Exp. A: 10 grams clay No. 2 (sandy clay), no NaCl. Subsidence 

very slow. Nov. 28. Height of column 85mm, height of sediment 47mm, 

supernatant liquid slightly turbid.

A£: 10 grams No. 2, 0.025 gramme NaCl. Subsidence much more 

rapid, having been, apparently, completed about Oct. 1st. On Nov. 28, 

height of column 85mm, sediment 33mm.

A£: 10 grams No. 2, 0.05 NaCl. Subsidence complete within fortyeight hours. Column 92mm, sediment 33mm, liquid clear and line of deinarkation between, sediment and liquid sharply defined. Al and A2, 

containing 0.1 and 0.2 grams NaCl respectively, showed complete subsidence within 24 hours.

Series B: 10 grams No. 3 (blue clay) taken.

B: No NaCl. Nov. 28. Column 86mm, of which about 5mm could be 

called clear, the next 10mm, though translucent, was turbid, the rest

opaque.

B£: 0.025 grams NaCl. Nov. 28, column 88mm, sediment 50mm, demarcation fair.

B^: 0.05 grams NaCl. Nov. 28, column 81mm. Sediment 44mm, 

demarcation definite, solution clear.

Bl: 0.1 gram NaCl. Nov. 28, column 84inrn. Sediment 28mm. Sedimentation complete within a week.

B2: 0.2 grams NaCl. Nov. 28, column 87mm, sediment 28mm. Subsidence complete within 48 hours.

Two portions of each clay of 5 grams each with 0.025 and 0.05 gram 

NaCl, respectively, showed a rate of subsidence much more rapid than 

that of the corresponding 10 grain portions, and this rate seems to depend upon the salinity of the solution. The further investigation of 

this subject involves complicated problems in physics, and for practical 

purposes it is sufficient to know that by the use of small quantities of 

the soluble portion of sue!} clays can be easily and completely
CHATARD.] NATURAL SODA. 99

CONCLUSTONS.

The conclusions arrived at in the course of this work may be briefly 

summarized as follows:

First. Natural soda is formed partly by direct decomposition of rocks 

through the action of air and water, aided at times by heat and pressure, and partly by subsequent decompositions occurring either in soils 

or in closed basins. These reactions, especially those of the latter class, 

are much influenced by the action of organic matter, which not only 

reduces sulphates, but also, in the form of certain organic acids, has 

been found to be a powerful reagent in rock decomposition.

Second. Natural soda is, essentially, a definite compound of sodium 

monocarbonate and bicarbonate, and the other accompanying salts 

are to be considered only as impurities. The proportion of the two carbouates forming this compound is one molecule of each. Any excess of 

either carbonate above this ratio is considered to be merely' accidental, 

and the existence of the so-called sesquicarbonate or combination of 

one molecule of mouocarbouate with two molecules of bicarbonate is 

believed to be very doubtful; at present, the strongest proof of its 

existence is derived from certain crystallographic determinations.

Third. The mineral urao is the pure form of natural soda, and this 

compound^ having a relation of four-thirds of a molecule of CO2 to 

one molecule of Na2O, may be called the " tetra trita " or "tetrita" 

carbonate. The sodium carbonates are therefore considered to be but 

three in number, namely: monocarbonate, tetrita carbonate and bicarbonate.

Fourth. The nature and properties of urao render it the most suitable form in which the natural sodium carbonates can be separated from 

accompanying salts. Hence any technical method devised for the manufacture of commercial soda from the natural material should be based on 

the formation and separation of this compound. The method described 

as being employed at Owen's Lake is, as far as it goes, simple and good, 

but the yield is not large, when the extent of the plant is considered. 

Owing to the small proportion of bicarbonate present in th,e original 

water, the crop is smaller than could be obtained if the amount of bicarbonate could be increased. Whether this can be economically done 

can be answered by practical experience only, but the following suggestions may be of value.

As the first step in the purification of a natural soda, it must be dis 

solved, and the solution should be clear. If such a solution be analyzed it will be found, in most cases, that the proportion of bicarbonate 

present is insufficient to give the largest practicable yield of urao. The 

amount of carbonate in the first crop depends upon the amount of 

bicarbonate in the solution, as this separates first and in separating 

takes with it a proportionate amount of monocarbonate. We have 

already seen that a scuja ash of very good quality can be made at Qwen'g
100 WASHINGTON LABORATORY. [BULL.60.

Lake, but the yield under present conditions must be small in proportion to the amount of solution used. If the percentage of bicarbonate 

could be economically increased, the first crop should be much larger 

without detriment to its purity, and the increase may be effected either 

by the direct addition of bicarbonate or by its formation in the solution by causing the latter to absorb carbonic acid under pressure.

If the direct addition of bicarbonate is preferred, advantage may be 

taken of the fact noticed by Mondesir and others, that if urao is treated 

with an amount of water insufficient for its complete solution, it is decomposed, NaaCOa going into solution, while NaHCO3 is left behind. Heat 

increases the rapidity of the decomposition, but the temperature of the 

solution should not exceed 37.5C 0. (100° F.). The NaHCO3 thus obtained can then be dissolved in the raw solution of the natural soda, 

which for this purpose must not be too concentrated and, as the bicarbonate dissolves slowly, agitation of the salt with the liquid will hasten 

this stage of the process.

The solution of Na2GO3 obtained by this treatment of a portion of 

the urao may be utilized by converting it into bicarbonate, using, for 

this purpose, the carbonic acid given off during the calcining of the 

soda ash. The proper form of furnace for calcining such material is a 

continuously working muffle, in which the soda is mechanically fed, 

stirred and delivered, while the CO2 is obtained in a pure condition and, 

when cooled, can be introduced at once into the solution of Na2CO3 . 

For rapid absorption a pressure of about 25 to 30 pounds to the square 

inch is advisable, hence a pump must be used and the absorbing vessels should be made of light boiler iron. The absorption should not 

exceed the point at which bicarbonate begins to precipitate, and if the 

absorbing vessels are properly arranged in a series the carbonating 

will be a continuous operation and the plant required for quite extensive works will be found to be much smaller thau would be supposed, 

The carbonated solution can be added directly to the raw solution.

If the formation of bicarbonate in the raw solution is preferred, a 

portion of this may be thoroughly carbonated and then added to the 

rest. This method has some advantages over the first one, but would 

probably require a somewhat larger carbonating plant for works of an 

equal capacity.

While the summer temperature is usually sufficiently high for the 

proper production of urao, the season is short, under the most favorable 

circumstances, and the output of works depending entirely upon natural 

heat correspondingly small. On the other hand, the temperature of the 

solutions should not be allowed to exceed 100° F. If it be possible to 

maintain the solution at this temperature during the crystallizing stage, 

in an economical manner, a great gain would be made, as the works 

could be run throughout the year, there being, usually, but little difficulty in obtaining and storing up an ample supply of concentrated raw 

solution. In this direction there is an extensive field for the exercise
NATURAL SODA. 101

of educated ingenuity in the utilization of the waste heat of the calcining furnaces, as also in the economical application of heat derived from 

fuel burned for this purpose only. The description of the salt works 

at Pomeroy, Ohio, given in my paper on salt-making processes, in the 

Seventh Annual Report of the U. S. Geological Survey, shows a most 

ingenious and exceedingly close utilization of heat derived from fuel of 

very poor quality, and may give many hints to those desiring to work 

in this direction.

The utilization of the mother liquor of the first crop is a problem 

which can only be solved by the growth of this industry. Doubtless in 

time something can be done with the vast quantities of chlorides and 

sulphates which are waste products, but their value is too small to give 

much hope for their utilization under present conditions. The industry 

is in a preparatory stage only, but will surely become of great importance in the future; the present consumption of sodium carbonate in 

this country is probably not less than 250,000 tons and is increasing, 

and a large part of this amount could be supplied by the Great Basin 

if its resources were utilized. If those who may hereafter take up and 

prosecute this branch of chemical industry shall find the information 

given in these pages of value to them, the purpose of this paper will 

have been realized.

ANALYSES OF SIX NEW METEORITES.

BY J. EDWARD WHITFIELD.

The Bockwood Meteorite. This meteorite was found about the middle 

of March, 1887, by Mr. Elihu Humbree on the range of the Crab Orchard Mountains, in Tennessee. The field in which it was picked np 

is now owned by Mr. W. B. Lenoir, and is situated 8£ miles west from 

Uockwood, in Cumberland county. The material for analysis was 

received from Messrs. Ward and Howell, of Rochester, N. Y., the present owners of the meteorite, to whom I am indebted for the privilege 

of description.

FIG. 5. The Eockwood Meteorite.

There were three pieces found, the smallest measuring 10cm x 8cm 

X 6cm, and weighing 1.65 kilos; the next larger, measuring 20cm x 

16.4cni x 6.5cm, and weighing 2.64 kilos; and the largest, an irregular 

egg-shaped mass, a little flattened on one side, measuring 38cm x 

25.3cm x 21.5cm, with a weight of about 38.5 kilos and specific gravity 

of 4.240. An idea of the appearance of this piece can be had from the 

foregoing cut, which is from a photograph reduced to -g natural size. 

The mass is quite brittle, very hard to saw, but easily broken by hammering. Cut slices show many irregularly shaped stony fragments with 

some nodules, the largest seen being about 1cm on the surface diameter. In the larger slices the stony part is so broken as to give the polished surface a brecciated appearance.

In analysis, the metallic portion was freed from the mineral part by 

crushing to rather fine particles and separating by the aid of a magnet..-

103
104 WASHINGTON LABORATORY. [HULL. CO.

This was again treated in the same manner, and the resulting metal 

washed with alcohol and quickly dried ; by this method it was found 

possible to free the metal from all but the merest trace of stony substance.

The metallic portion proved to be an alloy, rich in nickel, as is shown 

by the following figures:

Per cent. 

Fo........................................................ 87.59

Ni.... ..................................................... 12.09

Co......................................................... tTilCO.

Cn ........................................................ trace.

P ......................................................... none.

S.......................................................... none.

99. (58

The metallic grains seem to be quite evenly distributed through the 

mass. In but one instance does a nodule appear to have attained a 

size larger than that of a pea, and on the section of this nodule we were 

able to obtain the Widmannstiitten figure by etching. Cut No. 2 shows 

the polished slice containing the nodule of natural size:

I'm. 6.- Section of Rockwnod Meteorite.

The rocky part, after being freed as well as possible from metal, was 

finely ground and digested with dilute hydrochloric acid, and the resulting soluble and insoluble portions investigated separately, but from the 

fact of there being a number of minerals mixed together no satisfactory conclusions could bo, drawn from the examination. The mass was 

therefore analyzed as a whole with the following results:

Per cent.

SiOj........................................... 41.93

A12O3 .......................................... 9.27

FcO ........................................... 22.94

CaO ........................................... 9.09

MgO....... .................................... 8.76

Fo............................................. 3.75

Ni ............................................. 1.74

Cl ............................................. 0.18 = 0.32 Fed*

P.............................................. O.C5

S .............................................. 1.58

99.88
ANALYSES OF METEORltES. 105

By the analysis of the portions soluble and insoluble in dilute acid 

it was found that the greater part of the lime and but a trace of 

the magnesia had gone into solution, proving the absence of oliviue, 

and giving good grounds for the supposition that the rocky portion is 

mainly a mixture of anorthite and a silicate related to ai!£ite, but very 

rich in iron. It will be noticed that the ratio between the iron and 

nickel in the metallic portion is greater than that in the rock. This is 

accounted for by the fact that in the rocky part of the meteorite the 

iron, as metal, has been greatly oxidized, as is shown by the large 

amount of rust covering the specimen, caused no doubt by the chloride 

of iron present, aud is reckoned as FeO, accounting for the large proportion of iron in the supposed augite.

Owing to the bad condition of the fragments subjected to analysis 

we have no grounds on which to compute the phosphorus and sulphur

as schreibersite and troilite, but from the fact of these minerals being

among the more common constituents of this class of meteorite, and 

also that in the main analysis of the rock portion phosphorus and 

sulphur were found,'it is probable that the phosphide and sulphide of 

iron are two of the minerals present.

One of the polished slices contained a small nodule, which was sacrificed in order that its nature might be determined, and the following 

figures give the results of analysis. The mineral was finely ground, 

the metallic portion, if any, separated by aid of the magnet, and the 

residue was digested in dilute hydrochloric acid.

The insoluble portion was found to be 94 per cent., the composition of 

which is

Per cent. 

SiO8 ............ ............................................ 51.85

AlaOa .......... :........................................... 4.52

FoO-.'......................................... .............. 13.26

CaO ......................................................... 1.09

MgO........................................................ 29.28

100.00

This gives the ratio of R/'O to SiO2 =.93 : .86, which corresponds well 

with the mineral enstatite, although in this case much of the magnesia 

is replaced by. iron. The soluble portion consisted of iron with a slight 

trace of nickel, which tends to show that the nodule contained some 

metallic particles which it was impossible to extract with the magnet. 

During the digestion in acid, as no sulphuretted hydrogen could be 

detected, we infer the non-existence of sulphides in the nodule.

The total mineral was also analyzed with the following results:

Per cent. 

Si02 ........................................................ 49.96

A1803 ....................................... ................ 4.75

FeO ...........................4............................ 15.97

CoO + NiO................ .................................. trace.

CaO ........................................................ 1.15

MgO........................................................ 28.15

99.98
106 WASHINGTON LABORATORY. [BULL. 60.

This meteorite, then, is a lithosiderite,. poor in metal, the metallic 

.portion not exceeding 16 per cent, of the mass. The stony part is 

probably anorthite and eustatite.

Chattooga County Meteorite. This mass of meteoric iron was found 

by Mr. W. J. tfox, about the 27th of March, 1887, on his farm near Holland's Store, Chattooga county, Ga. In all 12.5 kilos were found, but 

the mass was rather roughly handled, being broken into pieces and 

some of them worked into horseshoes and nails by the local blacksmiths. Three of the fragments were obtained by Mr. G. F. Kunz, of 

New York city, and described by him in the December, 1887, number 

of the American Journal of Science.

The material received from Mr. Kuuz for analysis gave the following 

results:

Per cent. 

Fe.......................................................... 94.60

Ni.......................................................... 4.97

Co.......................................................... .21

P.....'...............:...................................... .21

>...................................................... ..traces. Ss >

99.99 

Specific gravity............................................. 7.801

Taney County Meteorite. We received from Mr. George F. Kuuz, the 

present owner of this meteorite, the material for analysis. The description has been fully given by him in the December, 1887, number of 

the Am. Journal of Science.

This being one of the class termed stony meteorites, a number of 

analyses were made on the rocky portion, in order, if possible, to ascertain the character of the minerals present.

The analysis of the metallic part is as follows:

Per cent. 

Fe.......................................................... 89.41

Ni.......................................................... 10.41

Co.......................................................... .29

P........................... ................................ .16

100.27

Of the rock material separated from metallic grains the'analysis gave

Per cent.

SiO2 ........................................................ 45.88

Al,0a....................................................... 7.89

FeO ........................................................ 19.73

CaO........................................................ 6.02

MgO........................................................ 17.96

NiS......................................................... 1-67

FeS......................................................... .54

99.69

The fragment as received gave a specific gravity of 4.484. As far as 

I can judge the insoluble mineral of the rocky portion is eustatite, and 

the soluble part a lime-iron silicate with considerable A12O:». Of the
WIIITPIBLD.] ANALYSES OF METEORITES 107

portion insoluble in dilute hydrochloric acid the following figures are 

the results of analysis:

SKV............................................. 52.39 =.87

AlvO*............................................. 7.11

FeO.............................................. 14.68 .20 ^

CaO.............................................. 4.40 .08>.81

MgO............................................. 21.33 .53)

100. 00

Eatioof SiO2 : R"O = .87 : .81 which agrees pretty well \vith enstatite; 

but here the MgO is replaced by much FeO, and the presence of 

A12O3 makes the ratio vary a little from the normal 1 : 1. Deducting 

all the S as NiS and the Fe to correspond to the remaining S from the 

soluble part, we have for the percentage of the soluble part:

Per cent. 

Si02 .................................................... .... 26.95

Al£>3 ....................................................... 17.69

FeO ........................................................ 35.98

CaO........................................................ 15.98

MffO........................................................ 3.40

100.00

The little MgO h°ere probably cotnes from the slight solubility of the 

enstatite in the hydrochloric acid.

This meteorite is similar to the so-called Newton county, Ark., 

stone described by Dr. J. L. Smith, 1 and Mr. KULIZ has found that 

the mass originally fell in Taney comity, Mo., but that a fragment was 

broken off and taken to Newton county, Ark.

Linnville Mountain Meteorite. About the year 1882 a mass of meteoric iron was found on Linnville Mountain, Burke county, N". C. 

Eventually it came into the hands of Mr.'Kunz and was described by 

him in the American Journal of Science.2

Material for analysis was furnished by Mr. Kunz and gave the following results:

Per cent. 

Fe.......................................................... 84.56

Ni...................... ................................... 14.95

Co.......................... ................................ .33

Cu........................................................... none.

S-.......................................................... .12

C............... ...... ....................................... trace.

P........................................................... trace.

99.96

The Fayette County Meteorite. The meteorite described below was 

found some ten years ago at Bluff, a settlement on the Colorado Kiver 

about three miles southwest of the town of La Grange, in Fayette county, 

Tex. Bluff' can not boast of being a village, as it is simply made up 

of a few farms scattered within a radius of two miles. The farmers are

'Am. Jour. Science, vol. 40, 1865. 2 Ibid., vol. 36, Oct., 1888.
108 WASHINOTON LABORATORY. [BULL.GO.

mostly Germans or Bohemians, and as they are generally of the superstitious class, it is riot strange that the finder, a Bohemian, named 

Eauiosek, should have been struck by the appearance of the stoue, and 

especially by its weight. As it is probable that he never heard of such 

a thing as a meteorite, it is safe to say that he did not know the nature 

of his find; still he seems to have come to the conclusion that it was 

something foreign to the soil.

There is a tradition in Fayette county that Santa Ana, at the time 

of his flight after the battle of San Jacinto, buried his war treasures 

somewhere near La Grange, and the belief has so fixed itself in the. 

minds of the inhabitants that many fruitless attempts have been made 

to discover them. The finder of the meteorite, with the tradition fresh 

in his mind, reasoned that so large and heavy a stone must mark the 

place where some treasure was deposited; he therefore rolled the stone 

a few feet aside and dug a deep hole at the exact spot where the stoue 

had been, without finding anything to pay him for his labor.

For several years the stone lay where the Bohemian had left it; then 

he sold the piece of land to Mr. C. Hensel, who still owns it; but before 

the latter had taken possession Raniosek removed the stoue to his own 

farm, about a mile away, where for five years more it lay neglected in 

his yard.. His reason for removing it was that its weight led him to 

suspect it contained some valuable metal.

About three years ago Mr. H. Hensoldt took charge of the school at 

Cedar, two and one-half miles from Bluff settlement. While spending his 

time in hunting for fossils, minerals, etc., the attention of the farmers 

was drawn to him, and in January, 1888, he was informed of the str.nge 

stone in Mr. Raniosek's yard. Immediately on seeing it he recognized 

it as a meteorite, and a very fine specimen of its kind.

After obtaining possession'of the stone Mr. Hensoldt disposed of it 

to Messrs. Ward and Ho well, of Rochester, N. Y., to whom we are indebted for the material for study and the privilege of description. On 

receiving the stone Mr. Howell published a notice in Science (February 

3,1888, p. 55) putting it on record as the " LaGrange Meteorite," but 

on finding that this name had already been applied to the Oldhatn 

County, Ky., Meteorite, agreed that it should be called the Fayette 

County Meteorite.

The stone possesses all the characteristics of a meteorite. The pittings 

are well marked, but the crust shows only in the deeper depressions; 

a freshly fractured surface shows, besides the grains of metal, a greenish-gray appearance not unlike some greenstones. A particularly interesting feature of the stone is the presence of a few dark-colored veins 

varying greatly in dimensions the one in the specimen for examination being some 2mm in the greatest width and 60mm in length.

The three dimensions of the mass are 58cm x46cm x28cm, and the 

total weight about 146 kilos. A good idea of the appearance of the 

meteorite may be had from figure 7.

Before the specimen was pulverized for analysis the vein was care-
WHITlilELD.] ANALYSES OF METEORITES. 109

fully sawed out, so as to keep all the vein material from the mass. The 

rock was then ground as tine as possible, and a portion (1 grain) treated 

with iodine in cold water, to separate the metallic particles. The residue

O 6IN I FT 2FT

FIG. 7. Tho Fayotto County Meteorite.

was filtered on a Gooch soluble filter and washed free from iodine. The 

rocky material, after being weighed, was treated with dilute hydrochloric 

acid and allowed to stand for some time, then filtered, and the residue 

weighed; in both cases the mineral being separated from' the filter by 

using the proper solvent for the anthracene washed with ether and 

alcohol and dried at 100° C. This temperature was not sufficient to 

drive all the water from the mineral part, which accounts for the discrepancy of about 2 per cent.

The following figures will show the composition of the metal and the 

rock, soluble and insoluble, in hydrochloric acid ; also the results of a 

complete analysis of the total mass:

SiOj ................

Fe ..................

FcO ................

Al-fOs. ..............

PA- .-. ....

CaO ................

MnO...... ..........

MKO. ...............

NiO ................

Ni...... ............

CoO. ...............

Co..................

S.. '.................

Less 0 for S ........

No. 1.

Total mass.

37.70

3.47

2.17

91

2.20

.45

25.94

1.50

fif\

.10

.09

1 Ift

99.79 

.65

99.14

No. 2.

5.67 per cent, 

of total (motal).

82.42

15 44

2. 14

100. 00

No. 3. *

33.3 per cent, 

of total (insolubloinHCl).

49 64

35.56

4.12

4 93

.54

25.21

100. 00

No. 4.

C0.62 per cent, 

of total (Holuble 

in HC1).

i)3. 59

1 'M

.42

28.08

2.06

97

2 1 ft

101. 09 

1.09

100. 00

The percentages in all except the first are calculated from the weight 

found.
110 WASHINGTON LABORATORY. [BULL. 60.

From these figures it will be seen that the minerals which go to make 

up the rocky portion of the meteorite are essentially olivine and enstatite, with considerable pyrrhotite, as is also shown by the microscopical description, for which I am indebted to Mr. G. P. Merrill, of 

the U. 8. National Museum, by whom the paper was published in the 

American Journal of Science.1

The stone belongs to the class of meteorites to which G. Rose 2 has 

given the name " chondrites." To the unaided eye the chrouditic structure is not distinctly marked, a broken surface showing a fine-grained 

and evidently crystalline granular rock, very compact, of a greenishgray color, and thickly studded with small metallic points with a brassy 

luster. A polished surface shows the stone to be composed of small 

chondri rarely over 2mrn in diameter, thickly and firmly compacted in a 

fine granular groundmass. Throughout the entire mass are thickly 

distributed innumerable small irregular flecks of a steel-gray, brassy, 

and bronze-yellow color, presumably native iron and pyrrhotite.

The striking feature of the stone is its fine and compact texture, which 

exceeds that of any chondritic meteorite with which we are acquainted, 

but which is perhaps most closely approached by the stones of Dhurinsala, India, and Cabarrus county, N. C.

Thin sections of the stone show, under the microscope, a confused 

aggregate of rounded and irregular, often fragrneutal, olivine and enstatite grains and chondri, embedded in a fine granular groundmass of the 

same mineral composition.

The chondri occur in both rnonosomatic and polysomatic forms composed either of olivine or enstatite alone or the two minerals associated. 

The peculiar grate-like or barred forms so characteristic of olivine choudri are here represented, as are the radiating fan-shaped forms of eustatite.

The large greenish microscopic chondri are, under the nriscroscope, 

seen to be made up of innumerable enstatite granules So arranged as to 

form oval or fan-shaped areas of radiating columns, inclosing large, 

quite perfectly outlined, crystals of the same mineral. These included 

forms are nearly colorless or merely gray through iuclosures of innumerable dust-like particles, and show sharp and well-defined cleavages 

parallel to either prism and a parting parallel to the orthopinacoid. 

Both olivine and enstatite are nearly colorless or gray through iuclosures of dust-like particles, and carry but few cavities.

In addition to the minerals above mentioned there were noticed occasional broad, irregular plates of a rnouocliuic mineral, light gray in 

color, but polarizing brilliantly in red and yellow colors, and which gave 

extinction angles varying from 25° to 31° Such are presumably augite 

or a closely allied pyroxene. Nothing that can be certainly identified 

as a feldspar was observed. Occasional small nearly colorless angular 

forms show faint indications of twin structure, and it is possible may

1 Whitfield & Merrill: Am Jour, of Science, vol. 36, Aug. 1888.

8tj. fjeriiu; 1333) y, 1861,
WIIITFIBLD.] ANALYSES OF METEORITES. Ill

be a plagioclase. In two sections were observed irregular outlined interstitial areas perfectly colorless and full of gas cavities. These in 

some cases remained quite dark durkig a complete revolution of the 

stage, and in others gave decided polarization in light and dark colors, 

and in converging light showed indistinct biaxial interference figures. 

The position of these areas relative to the other constituents is that of 

an interstitial glass or a secondary mineral like a zeolite. As they 

show neither cleavage nor crystallographic outlines, and moreover are 

to be found but rarely in the sections at hand, it is impossible to identify them satisfactorily.

The metallic iron occurs in the usual rounded and irregular masses 

one to two millimeters in diameter, and is apparently in about equal 

proportions with the pyrrhotite: the latter showing a bright brassy 

luster in strong contrast with the

silvery white iron.

The black vein above noted.traverses the stone in the form of an 

irregular fissure (often expanding 

and contracting abruptly, as is 

shown in Fig. 8), for a distance of 

about 60mm, and varies in width from a mere line up to 2mra. Near 

its lower end it bifurcates, and incloses a portion of the mass of the 

meteorite some 15min long by 2mm wide. 1

From a fragment containing a portion of the vein thin sections were 

prepared, and the remaining vein material, separated as clearly as possible from the inclosing rock, was subjected to chemical analysis, the 

process being essentially the same as in the analysis of the meteorite 

proper. Although the vein material is more compact and much darker 

in color, the analysis shows very little difference from that of the mass, 

the main apparent difference being the absence of the lime bearing 

mineral. The following are the figures obtained by analysis on material that weighed a little less than 0.4 grams:

FIG. 8. Vein in Fayetto County Meteorite. 

Natural size.

Fe...... .......... 

MCo .............

Metal.

2.30

3

CDK

Si02 .............. 

FoO. .............

A12 03 - ...........

CaO .............

MgO.... .. ........

(NiCo)O.......--.

Leas 0 for S ......

44 per 

cent, of vein. 

Insoluble in 

HC1.

56.52 

12.35

1.51

25.53

4.09

100. 00

51 per 

cent, of vein. 

Soluble in 

HC1.

27. C3

-> 34. 31

2.41

32.12

3.27

.52

. 100. 26 

.26

100.00

'Since the above was written Messrs. Ward and Howell have sliced the stone 

through the center and published in fccjeijcfi of Ji|J}e 1, ltf&}] ti tigm-« gUy\YJujj; tliQ 

f the yeijjs,
112 WASHINGTON LABORATORY. [HUM,. CO.

The same difficulty, with regard to water in the mineral, exists here 

as in the analysis of the mass.

From the figures it appears that the portion soluble in hydrochloric 

acid is essentially olivine in composition, while the insoluble is evidently a mixture of the same insoluble constituents as the mass of the meteorite. The filling material of the vein is, to the unaided eye, quite 

black and without luster; under the microscope it is seen to penetrate 

very irregularly and by innumerable minute vein-like ramifications into 

the stony mass on either side, arid to carry numerous iuclosures of a 

colorless mineral substance and blebs of metallic iron and pyrrhotite. 

The exact nature of the colorless inclosures can not be ascertained. 

On treating an uncovered slide with hydrochloric acid a part of these 

were dissolved, others were unacted upon. Under the microscope they 

are full of irregular rifts and fracture lines, but show no true cleavages. 

Some of them are in the form of single individuals, others have the 

structure of fragments of polysomatic chondri. Nearly all contain included black amorphous material, and many show distinctly included 

specks, giving the silvery white and brassy yellow reflections of the 

metallic iron and pyrrhotite. In many cases they are not separated 

from the black vein material by sharp lines, but seem to pass into it by 

gradations. Between crossed uicols many of them act like a gum, others 

remain always light, recalling the well-known crypto-crystalline structure of chalcedony, and still show here and there occasional small areas 

giving the characteristic polarization colors of olivine and enstatite. 

On examining the walls of the vein areas were observed where the 

gray and yellowish enstatites and oliviues retained their normal properties at the distance of one or two millimeters, but at contact with the 

black-vein matter were reduced to the colorless non-polarizing condition of the iuclosures.

The black matter of the vein when viewed in strong reflected light 

shows a dull bronze luster, less brilliant than that of the pyrrhotite 

particles which it incloses. The thinnest portions of the slide when 

examined with a power.of 175 diameters show a brownish amorphous 

base through which are scattered abundant irregular dust-like particles 

and flecks of a perfectly black opaque material, the nature of which it 

is impossible to ascertain by the microscope alone.

The structure of the vein is shown in figure 9, in which the finely 

dotted portions represent the black amorphous vein matter with bronzy 

luster, the entirely black areas, the blebs of metal and pyrrhotite, and 

the irregularly rounded clear or partly clouded areas the colorless silicates.

From the study of these veins as above described we are inclined to 

cousider the colorless particles as olivine and enstatite residuals which 

have been deprived of their normal optical properties by the forces 

active in forming the vein. What the exact character of the black and 

amorphous material may be still remains a, matter of conjecture. It
WUITFIEUX] ANALYSES OF METEORITES. 113

is unacted upon by acids, and when tested with a needle point it breaks 

up readily into earthy fragments which are not attracted by the magnet.

Mr. Howell informs me that the 

stone in his possession shows three 

of these veins, the largest exposure 

of any one on a broken surface being 

about four inches. The width and 

general character of all, he states, 

appear to be uniform throughout, 

though this can be ascertained definitely only by breaking the stone.1

Owing to the small amount of vein 

material which was available for chemical analysis and the impossibility 

of separating it completely from the inclosing rock, the results obtained 

can be regarded only as suggestive. The main points brought out can 

be best shown by reproducing here a comparison of the results:

FIG. 9. Portion of vein highly magnified.

Si02 ................

re..................

FoO... ..............

A1203 - ..............

CaO ................

MnO. ...............

MgO. ...............

Ni, Co. ..............

S...... ..............

Specific gravity. ....

Mass of 

meteorite.

37.70

4.41

23.82

2.17

2.20

.45

25.04

1.75

1.30

3.510

Vein 

material.

38.06

2.30

22.98

1 89 ^

27.52

3.26

.26

3.585

1 In structure these veins seem to only remotely resemble those described by Tscherinnk (Sitz. der kais. Akad. der Wiss., vol. 85, Part 1, p. 204) in the Mocs meteorite, 

and which, it will be remembered, he argued indicated an elevation of temperature 

since the consolidation of the stone, such as, aided by reducing vapors and gases, fused 

the iron and pyrrhotite without affecting the silicates. He describes the brown and 

black "Fullmasse" of the vein as an admixture of the same substance as the meteorite itself, and an opaque half glassy black admixture resembling the hlack veinlike material of the Orvinio stone. The silicates occur in the vein in the form of 

small sharp splinters, the iron in granules, and the pyrrhotite in the form of little 

leaves and small kernels, often so arranged as to give rise to a fluidal structure. Dr. 

Hans Reusch has described (N. Jahrb. fiir Min., iv Beil.-Band, 3 Heft, 1886, pp. 491- 

492) veins in the Stalldalen meteorite which present features in part common to those 

of the Fayette stone. To the unaided eye the filling material is black and opaque 

and carries metallic particles. Under the microscope it shows a brownish gray, isotropic and sometimes glassy substance densely crowded with rounded transparent 

fragments. The upper figure in his Plate xiv closely resembles in structure the 

vein matter of the Fayette stone, but as far as can be judged from his description 

the included particles seem to have retained their normal optical properties. Reusch 

regards this black vein material as the result of a partial refusion of the chrondite 

gubstance.

60 8
114 WASHINGTON LABORATORY. [BULL. 60.

These differences are too slight to be considered of great value unless 

found to be constant by further investigation.

San Bernardino County Meteorite. A prospector working in the San 

Etnigdio Mountains, California, found this meteorite, and thinking it 

to be a lump of some valuable ore sent it to Mr. Thomas Price, of San 

Francisco, for assay. Unfortunately before the nature of the sample 

was discovered it was put through a crusher and hence only small 

pieces could be obtained. On finding that it was a meteorite, Mr. Price 

sent a few fragments to Mr. G. P. Merrill, of the TJ. S. National Museum, 

for investigation. Mr. Merrill has published a note on the subject in 

the June, 1888, number of the American Journal of Science, and later 

a full description in Vol. 11 of the Proceedings of the National Museum.

From Mr. Merrill we received material for analysis, but the bad condition of the fragments made a complete analysis almost impossible.

The mass consists of

Per cent. 

Metallic portion............................................. 6.21

Soluble in HC1. .......................................... 51.26

Insoluble in HC1............................................ 42.23

Of this the metallic portion gave as its composition 

Per cent. 

Fe........................................................... 88.25

Ni. ......................................................... 11.27

Co.......................................................... .48

The soluble portion is presumably all olivine and pyrrhotite, with 

some secondary iron oxide. The analysis of this portion by separation 

with dilute hydrochloric acid was a failure. The insoluble part was separated by long digestion in dilute acid followed by boiling in sodium carbonate. The remaining powder showed, with the aid of the microscope, the presence of very pure eustatite and very little else, and the

chemical composition upholds this view.

Per cent. 

SiOi........................................................ 54.42

FeO ........................................................ 14.03

CaO ........................................................ 2.46

MgO........................................................ 29.11

100.02

From these figures it will be seen that the mineral is a highly ferriferous eustatite (bronzite) with a small amount of a lime-bearing pyroxene mineral. The relative proportions of the various constituents as 

they exist in the first rock can not be estimated with any degree of 

certainty for the reasons already stated.
TWO SULPHANTIMONITES FROM COLORADO.

By L. G. EAKINS.

The mineral first to be described was sent to the Denver laboratory 

of the U. S. Geological Survey iu the latter part of 1885 by Mr. E. K. 

Warren, of Crested Butte, Colo.

At that time a hasty qualitative examination was made, establishing 

the fact that it was a sulphantimouite of lead, and since then nothing 

more has been done with it until the present analysis was made.

This mineral comes from the "Domingo" mine, on the ridge between 

Dark Canon and Baxter Basin, Gunnison county,Colo., in which locality 

it is known as "mineral wool." It consists of aggregates of small 

acicular crystals, forming matted, wool-like masses in the cavities of 

a highly decomposed gangue rock of siliceous material mixed with 

some calcite. It is dull grayish-black in color, with occasional spots 

of iridescence, due undoubtedly to a slight superficial oxidation.

In procuring material for analysis a lot of loose material sent by Mr. 

Warren was slightly crushed and rubbed with water in a mortar and 

poured off, the fine needle-like crystals floating off readily; this was 

afterward purified by a retreatinent in the same manner, and then subjected for a short time to the action of dilute hydrochloric acid to 

remove the slight amount of attached calcite. The material obtained 

in this manner appeared under the microscope to be perfectly pure and 

homogeneous, with the exception of a slight amount of gangue still 

remaining.

No crystalline form could be made out, and on account of its peculiar 

nature no attempt has been made to determine either specific gravity 

or hardness. Heated before the blow-pipe it fuses readily without decrepitation ; in the closed tube it gives a slight sublimate of sulphur 

only; in the open tube it gives off sulphurous acid and dense white 

fumes of oxide of antimony; heated strongly the antimony all volatilizes, leaving a fused residue of sulphate of lead, slightly colored by 

the iron present; on charcoal it gives the lead and antimony coatiugSj 

and in the reducing flame with soda a lead button. It is soluble iu 

Jjot strong hydrochloric acid with evolution of hydrogen sulphide.

115
116 WASHINGTON LABORATORY. [BULL.GO.

The analysis is as follows:

Atomic ratios. 

Ag ...... ................................ trace.

Cu....................................... trace.

Pb....................................... 39.3)5 -r-207 = . 190

Fe.... ................................... 1.77 -=- 5(5 = .032

Mu ...................................... trace.

Sb.................. .... ................. 36.34 4-120= .303

S........................................ 21.19 -f- 32= .662

Insoluble gangue......................... .52

>.222

99.15

Dividing these atomic ratios by .222, we get:

Pb,Fe............................................. 1.00 =3.00

Sb................................................. 1.36 4.08

S .................................................. 2.98 8.94

Giving the formula: (Pb, Fe)3Sb4S9 ,.or 3(Pb, Fe) S, 2Sb2S3 .

This mineral, it is seen, tills a place in the group, 3ES, 2( As,Bi, Sb)2S3 , 

of which there are but few good examples, and which until now has 

not had an antimony representative.

The somewhat low summation of the analysis is probably due to two 

causes: First, a small amount of soluble gangue wLich was present and 

undetermined; second, the sulphur is about four-tenths of one per cent, 

less than required, due to the slight natural oxidation of the mineral 

together with an additional amount induced by treatment with dilute 

hydrochloric acid for the removal of calcite. In addition to the complete analysis given, there were additional determinations made of lead, 

antimony, and sulphur, the results obtained being in strict agreement 

with those given above.

The second of these sulphantimonites was collected in the summer of 

1887, by Mr. Whitman Cross. It comes from a mine on Augusta Mountain, Gunnisou county, Colo., this locality being about one mile east of the 

"Domingo" mine. Locally this mineral is also known as "mineral 

wool," and although differing considerably in appearance from the one 

just described, they were, on account of the similarity of occurrence, 

considered as probably identical.

It occurs in a siliceous gangue together with pyrite and sphalerite, 

and forms groups of acicular crystals, which are elongated prisms 

deeply striated, but whose form could not be determined.

The individual crystals of this mineral are considerably larger than 

those of the one previously described, and in consequence they do not 

tend so much to form matted aggregates. Its color is a bright, steely, 

grayish-black, with no tendency toward tarnish or iridescence. The separation of this mineral from the accompanying ones and the gangue was 

a matter of considerable difficulty. On account of their size the crystals 

could not be successfully washed out from the other material, but by 

the use of a rapid current of water and the Thoulet method a small 

quantity was finally procured perfectly free from, everything except
EAKINS.] SULPHANTIMONITES FfcOM COLORADO. 117

some pyrite, and that had no effect upon the analysis, as the mineral 

was dissolved in a mixture of hydrochloric and tartaric acids, leaving 

the pyrite unattacked. It was then filtered through a Gooch. crucible, 

and the amount of pyrite determined and deducted from the material 

taken. The fact that but a trace of iron was found in the analysis is 

conclusive proof that the pyrite was practically unattacked.

Blow-pipe characteristics are the same as in the one before described.

The analysis is as follows :

Atomic ratios. 

Ag............................................. trace.

Pb.... ......................................... 55.52 207 = .268

Fe............................................. trace.

Sb............................................. 25.99 -120 = .217

S, (calculated)................................. 18.98 -f- 32 = .593

100.49 

Dividing these atomic ratios by .217 we get:

Pb ............................................... 1.24 =4.96

Sb................................................. 1.00 4.00

S.................................................. 2.74 10.96 '

Giving the formula :-Pb5Sb4Sn or 5PbS, 2Sb2S3 .

We have here, in formula, a freieslebeuite in which instead of lead 

and silver the silver has been completely replaced by lead, and although 

the crystallographic agreement of this mineral with freieslebenite has 

not been established, there seems to be no good reason for not referring 

it to that species. The first described of the above minerals, 3 (Pb, 

Fe) S, 2 Sb2 S3 , has been given the name " Warrenite," after the gentleman who brought it to our notice. The same mineral has been designated "domingite" by Groth.

COEFFICIENTS OF VOLATILITY FOR AQUEOUS CHLORHYDRIC

ACID.

By EGBERT B. WARDER.

The various questions of physical chemistry are claiming more and 

more attention, and problems relating to states of aggregation seem to 

have a special interest. The art of fractional distillation on a manufacturing scale has developed a great variety of appliances, but much 

remains to place the theory on a satisfactory mathematical basis, especially in the case of bodies which exert a mutual affinity.

The term "coefficient of volatility" was introduced by Wanklyn 1 to 

indicate tlie relative readiness of different constituents to volatilize. 

Thus he found that when a very dilute solution of ammonia was distilled until j^ °f the water passed over, nearly £ of the 'ammonia had 

distilled with it. He estimated that a given quantity of water in. any 

small fraction of the distillate was accompanied by 13 to 14 times as 

much ammonia as the same quantity of water in the boiling liquid. 

Expressed more formally, if a boiling liquid has the composition 

H2O+wNH3, and yields a mixed vapor represented by H2O+wiN"H3 , 

the factor v is the coeflicicient of volatility, and in the case cited v 

equals about 13 or 14. Since this gas may be absorbed in indefinite 

proportions, of course the coefficients n and vn may be fractional, indicating the number of molecules of ISTHg divided by the number of 

molecules of H2O.

In the case of chlorhydric acid, as is well known, when the liquid boils 

under the ordinary atmospheric pressure, it tends to acquire the 

constant composition HC1+8H2O, or H2O+^ HC1. After a stronger or 

weaker acid has reached this composition, on further boiling n=vn and 

the factor 0=unity.

The well known researches of Eoscoe and Dittmar 2 showed that an 

acid of higher composition will boil unchanged under diminished 

pressure; a similar result was observed upon evaporation in a current 

of air of given temperature to supplement the partial pressure exerted 

by acid and aqueous vapor. Hence it is clear that v depends not only 

upon the composition of the mixture, but also upon the pressure (or 

temperature) at which the distillation is conducted. The published

1 Philos. Magazine, [4] 45,129 (1873). Pharm, J. Trails., [3] 3, 543 (1873).

".Jour, Chew, Sop,, 12,128.

119
120 WASHINGTON LABORATORY. [BULL. 60.

data relate to the conditions under which v=l, but no attempt has yet 

been made to show the relation between v and n.

The more recent researches of Eoozeboom show certain conditions of 

equilibrium among solid, liquid, and gaseous phases of aqueous chlorhydric acid 1 and other compounds which are illustrated by thermodynamical theory; 2 but the papers do not discuss the ordinary conditions 

of distillation.

Many operations of manufacturing, geological, and analytical chemistry depend upon the partial or complete separation of volatile constituents. Chlorhydric acid is typical of a large number of substances 

which have strong attraction for the solvent; and a more exact knowledge of its volatility as a function of the composition is the object of 

this research.

EXPERIMENTAL METHOD.

One hundred cubic centimeters of chlorhydric acid of known strength 

was subjected to fractional distillation in a boiling flask of 250cm3 capacity. Successive portions of the distillate were conducted through a 

Liebig condenser and discharged near the bottom of receivers; a loosely 

fitting cork was used to hinder evaporation. The several fractions, 

after weighing in well stoppered vessels, were titrated with sodium hydrate, containing a little barium hydrate and carefully protected from 

the air by soda lime. Phenol phthalein was used as indicator. In 

some cases very weak distillates were evaporated with excess of ammonia, and titrated with ceutinormal silver solution and potassium chromate. The water was determined by deducting the acid from the total 

weight of the fraction. As a rule no reliance was placed upon specific 

gravity, the ordinary summer temperature of the room being far above 

that recognized in the tables; hence the acid used for each distillation

was weighed. The residues in the boiling flask were also weighed and 

titrated for control.

When fractional distillation is conducted for the purpose of separating the constituents, this is promoted by some kind of dephlegmation; 

this may be accomplished by exceedingly simple means, as the walls of 

an ordinary boiling flask, by the complicated appliances of the manufacturers, or by the many devices for laboratory use. The object of the 

present work required the exclusion of dephlegmation, since this would 

introduce an element of great uncertainty. The flask was placed in a 

cylindrical air bath and covered with a conical hood of sheet copper. 

By means of a ring burner (as devised by Gibbs), with very gentle air 

blast, a circle of gas jets was thrown upon the copper cone, so as to 

keep the upper part of the flask heated far above the boiling point

1 Rec. Trav. Claim. Pays-Bas, 3, 84 (1884). Abstract in Zeitsch. pliysik. Chem., 1, 

365 (1887) and 2, 459, (1888).

2 Roc. Trav. Chim. Pays-Bas, 5, 335(1886). Abstract in Zeitsch. physik. Chem., 2, 

462 (1888).
VOLATILITY FOR AQUEOUS CHLORHYDRIC ACID. 121

of tbe fluid, while distillation was effected by a large Bunsen burner 

under the air bath. A-thermometer in the vapor was usually kept at 

a temperature of 145° to 153°. The boiling point of the liquid was from 

1000 to 1090. (varying with the concentration); and from the rate of 

distillation and the space above the liquid, it was estimated that the 

vapor would pass from the surface to the condenser in about six seconds 5 

hence it is not to be supposed that the thermometer indicated the actual 

temperature of the vapor, but something between this and the temperature of.the radiating surface of glass or copper. By this means the 

condensation of moisture upon the sides of the flask was prevented. 

In a preliminary experiment withH2O+.037HCl, the first fifty percent, 

distilled without the hood and ring burner contained no more acid than 

the 10 per cent, distilled with the precaution described; and this was 

only one-twentieth as much acid as distilled in the first 50 per cent,

under the heated cover.

As the distillation proceeded, and the volume of vapor increased, the 

temperature had to be moderated by turning down the flame.

In the distillation of strong acid each receiver was weighed with 10cm3 

water, to absorb the acid fumes.

CALCULATION OF RESULTS.

The weight of HC1 found in each fraction of the distillate subtracted 

from the total weight, leaves the weight of water; and the weights of 

water and acid thus found in each fraction were subtracted successively from the water and acid taken to find the composition after the removal of this fraction. The mean composition of the boiling liquid 

during the removal of each fraction was expressed in the form H2O-fwHCl, the composition of the distillate being HzO+?i/ HC1 or B2O+ 

vriELG\. The coefficient v was then found by dividing n' by n. Four 

distillations gave 25 pairs of values as follows:

I.

n

.0952

. 1031

.1107

.1180

.1231

V

.284

.423

.537

. 043

.868

II.

n

.0081

.0759

. 08G2

. 0984

.1107

.

V

.140

.194

.282

.429

.597

III.

n

.Ofi6C

. OG93

. 0730

.0709

.0800

.0844

.0879

.0911

.0944

.0970

V

.084

.111

.158

.172

.198

.243

.247

.253

.300

.311

IV.

n

.1939

.1853

.1713

.1507

.1474

V

5.44

3.71

2.40

1. 60

1.31
122 WASHINGTON LABORATORY. [BULL. 60. 

DISCUSSION OF RESULTS.

Two points remain to be considered :

First. What formula will best express the values found for v as function of n el

Second. Do the relations here determined point to actual equilibrium 

between liquid and vapor?

No one equation was found to express all the values given above. 

When dilute acid (%=.07 to .11) was boiled rapidly (about one grain per 

minute) the results agreed with the equation

 as in series II. When strong acid '(n=.l5 to .20) was boiled rapidly, the 

values of v were somewhat greater than would be indicated by the 

equation above; approximately,

as in series IV. These two empirical curves, which occupy different 

parts of the field, are entirely consistent with each other, but must be 

regarded as a first approximation only to the function sought. When 

the dilute acid of Series I and III was boiled from 20 to 60 per cent. 

more slowly than that of Series II, the values of v were about 10 to 30 

per cent, less than those indicated by the equation. There can be little 

doubt that v is a function of the rate of boiling as well as of the composition of the liquid. The problem appears to be dynamical, not a question of equilibrium merely, and I hope to investigate this point further.
ANALYSES OF JADE.

By F. W. CLARKE.

In the ethnological collections of the U. S. National Museum there 

are many objects of jadeite, nephrite, and various jade-like stones. 

They represent a wide range of localities, especially as regards 

the North American specimens, and in their external characteristics

they exhibit great variety of color, texture, and quality. Some came 

from regions which have already been well studied, but others, as in 

the series of articles from Alaska and Costa Rica, seemed to merit 

further investigation. At the earnest desire of the late Professor 

Baird, their mineralogical description was undertaken by Mr. G. P. 

Merrill and myself, and our joint paper, giving my analyses and his 

microscopic examinations, has already been published by the National 

Museum. 1 The present communication contains merely my own portion 

of the work, as part of the year's record of the chemical laboratory.

In Alaskan specimens of jade the museum is particularly rich. Since 

the acquisition of that territory by the United States it has been visited 

by many official expeditions, nnd their assembled collections represent 

the entire coast-line from Point Barrow to the southernmost extremity. 

If we except the remarkable hammers of jade-like pectolite described 

by me some years ago,3 all of the Alaskan jades are true nephrites, 

undistiuguishable in most particulars from the nephrites of Siberia, 

New Zealand, or the Swiss Lake Dwellings. In general this nephrite 

is coarse in quality; but occasionally objects are seen having high 

finish, some trausluceucy, and great beauty. The following worked 

specimens were examined, the material for analysis being in each case 

carefully sawed off to avoid unnecessary damage to the object.

A. Part of a small adze, Cape Prince of Wales. Yellowishgreen, mottled. Specific gravity 2.989.

B. Material for a drill, St. Michael's. Siskin green, translucent, 

uniform in texture. Specific gravity 3.000.

C. Small knife, Diornede Island. Blackish-green, mottled and 

laminated. Specific gravity 3.010.

D. Adze, Point Barrow. Nearly black superficially, opaque. 

Specific gravity 2.922.

i Proc. U. S. National Museum, 1888. 2 Bnll. U. S. Geological Survey, No. 9, p. 9.

133
124 WASHINGTON LABORATORY. [BOLL. 60.

The specific gravity determinations were made by Dr. William 

Hallock. The analyses, by myself, were as follows:

Si02 .. .............

A1203 .............

FeO ..............

MnO...... ........

CaO. .............. 

MgO... ...........

A.

1 91

56.01

1 98

6.34

12. 54 

21.57

100. 35

B.

1.42

56.12

.63

7.45

12. 72 

20.92

99.26

C.

2

AO

50.08

1.01

7.67

13.35 

19.96

100. 10

D.

2.06

V7 11

2

C7

^1^1

11.54 

21. 38

99.81

In each case the ferrous oxide represents the total iron. Ferric oxide 

was not discriminated, nor were alkalies looked for. So far the analyses 

are incomplete.

In addition to the above-named implements, another object^ of supposed jade was examined. It was a flaker from Point Barrow, of a 

dull bluish-green color, conchoidal fracture, considerable trauslucency, 

and specific gravity 2.654. These data, together with a partial analysis, 

identify the object as quartz. It contained 97.79 per cent, of silica.

Concerning the origin of the Alaskan jades there has been much 

discussion. Some early writers ascribed it to Siberian sources, but of 

latf years evidence has been gathered pointing to a home locality. 

Native reports indicated a source known as the " Jade Mountain," 

which lies north of the Kowak Eiver about 150 miles above its mouth, 

and after several efforts the spot has been actually visited by Lieut. G. 

M. Stoney. He collected specimens of jade in situ, and a number of 

specimens were submitted to me for analysis. They may be described 

as follows:

A. Greenish-gray, splintery-lamellar in structure.

B. Like A, but more granular.

C. Paler, nearly white, closer grained.

D. Brownish, highly foliated. 

All four were analyzed with the subjoined results:

SiO». ..............

A180S ........... -

FezOs ........... --

FeO...............

MnO..............

CaO...............

MgO..............

A.

1.78

58.11

.24

5.44

.38

12.01

21.97

99.93

B.

1.38

55.87

2.07

5.79

.38

12.43

21.62

99.54

C.

1.76

56.85

.88

4.33

1.45

13.09

21.56

99.92

D.

1.73

57.38

.19

4.43

1.25

12.14

22.71

99.83
CLAKK.E.] ANALYSES OF JADE. 125

If we cotmect this evidence with the microscopic evidence obtained 

by Mr. Merrill, it becomes clear that all the Alaskan jades are essentially identical, varying among themselves no more than specimens commonly vary from a single locality. This disposes of the theory that 

their presence in Alaska is to be accounted for upon the basis of trade 

with Siberia; which theory is also negatived by the discovery announced 

by Mr. G. M. Dawson ("Science," April 20, 1888, p. 186) of small 

nephrite bowlders on the upper part of the Lewes Kiver, in British 

Columbia, not far from the eastern boundary of Alaska. But these 

nephrites are also strikingly like those from many other localities, and 

two of the latter have been included in my comparison. First, a dark 

green water worn bowlder from New Zealand, sent to the Museum by 

Sir Julius Haast; and, second, a small implement from Eobenhausen, 

Lake Pfaffikon, Switzerland, out of the collection of Mr. Thomas

Wilson. The latter specimen, also green, had a specific gravity of

3.015, as determined by Dr. Hallock. The analyses are as follows:

Si02 ..............

AlaOa--- ----------

FeO ..............

CaO. .............

MgO.-.. ..........

Now 

Zealand.

.83

56.73

3.22

 5.90

13.24

19.42

99.40

Switzerland.

.63

56.87

6.33

13.45

21.06

99.84

All the iron is here represented as ferrous. Traces of manganese were 

present, but alkalies were not sought for.

Of jade objects from Mexico the Museum has a large and fine series; 

but nearly all of the specimens are from the one State of Oaxaca. The 

greater number of them are true jadeite; but as jadeite from the same 

region has been described by Damour,1 a very exhaustive review of the 

material did not seem to be necessary. No nephrite was found in the 

Mexican series. Two specimens were analyzed, which may be described as follows. The specific gravity determinations are by Dr. Hallock.

A. Light-colored bead, mottled with emerald green. Specific

gravity, 3.007.

B. Carved head, light green, from Zaachita. Specific gravity, 

3.190. .

1 Bulletin d<? la. Socidtd Miojeralogiqu6? vol. 4, p. 157,
126 WASHINGTON LABORATOEY. [BULL. 60.

Si02 ..............

A12 03 .--- .........

Cr203 .-...- .......

FeO ..............

CaO ..............

Mtrf)

Na,0 .............

K20 ..............

A.

1.81

58.88

25.93

.12

.24

.40

.36

11.04

.63

100.01

B.

.53

58. 18

23. 53

1.67

2.35

1.72

 11.81

.77

100. 56

If the water (ignition) in A. be regarded as replacing alkalies, the 

mineral approximates closely to normal jadeite, AlNaSi2O6. Both 

analyses fit in well with Dainour's work.

With Central American jade objects the Museum is well supplied. A 

few ouiy are from Nicaragua and Guatemala. The finest are all Costa 

Eican. Here too jadeite is the dominant mineral species, although with 

the true jades are many articles of softer green stones, and occasionally 

an object of quartz or chalcedony. For analysis, four specimens were 

chosen, viz: two jadeites, one quartz-like mineral, and one of the softer 

minerals, as follows:

A. Polished fragment, green. Rio de Buena Vista, Costa Eica.

Specific gravity, 2.71, Clarke.

B. Jadeite fragment. Sardinal, Costa Eica. Pale green, translucent. Specific gravity, 3.32, Clarke. 

C. Jadeite fragment. Culebra, Costa Eica. Light green, very

granular, opaque. Specific gravity, 3.27, Clarke. 

D. Small ornament. Las Huacas, Costa Eica. Dark green, very 

soft. Specific gravity, 2.282, Hallock.

Si02 .-.-. ........

A12 03 . ............

Fe203 .--.-. .......

FeO ..............

MnO...... ........

CaO ..............

MgO.. .............

Na,,0. .............

KjO ..............

A.

97. 10

) 1.85

*

98.95

B.

.90

59.38

22. 96

> 1.87

1.52

.67

12.71

trace -

99.81

C.

.!)3

58. 33

21. 63

1.71

.73

4.92

3.09

8.13

. 22

99. 69

D.

10.39

'0.49

11.39

) 2.39

3.83

.57

iindot.

nudet.

99.06

Of these analyses, A speaks for itself. In B and C we observe a 

difference in composition, which is in the line indicated by the appearance of the specimens; that from Sardinal being translucent and nearly
CLAU'KE.] ANALYSES OF JADE. 127

homogeneous; that from Culebra being coarser, distinctly mottled, and 

evidently impure. Specimen 0 is plainly not jade in any sense. It 

was examined microscopically by Mr. Merrill, who pronounced it to be 

a highly altered volcanic tuff, containing a considerable amount of 

bright green chlorite.

Through the kindness of Mr. Thomas Wilson, whose collection furnished the Eobeuhausen nephrite already described, I have been enabled to examine several other worked specimens of minerals which are 

sometimes classed, though loosely, with jade. A massive "saussurite" 

from the Saas Valley in Switzerland, out of the Museum collection, 

may be conveniently included in this series.

A. Fibrolite implement from Brittany. Specific gravity, 3.147.

B. Black stone implement from Estavayer, Lake Neuchatel. 

Specific gravity, 3.132.

C. Dark green " saussurite" implement from Robenhausen, Specific gravity, 3.403.

D. Massive " saussurite," Saas Valley. 

The specific gravity determinations are due to Dr. Hallock.

SiOa ...... ........

A1A .............

Fo,03 ...... .......

FuO .............

MnO. .............

CaO.............. 

MgO ............ ..

NaaO. .............

K.,0...... .........

A.

34.66

03. 24

110110.

.37

99. 58

B.

.65

*45.13

10.55

13. 09

4.20

11.02 

5.48

3.89

1UO. 01

C.

.30

46.90

29.76

) 2.52

11.77 

5.80

3.21

100.26

D.

KA

48. 29

27.65

f 1.45

12. 95 

fi. 30

3.57

99.81

Microscopically studied the second of the specimens was found by 

Mr. Merrill to be a mixture of various minerals. It is evidently a highly 

altered "basic rock," possibly a diorite. The saussurites need no 

special discussion.

MINERALOGICAL NOTES.

1, PETALITE FEOM PERU, MAINE. BY F. W. CLARKE.

In the well-known spodumene locality at Peru, Maine, petalite has 

been found in abundance. The discoverer, Mr. N. H. Perry, of South 

Paris, Maine, kindly furnished me with a fine suite of specimens, upon 

which the following examination was made. The petalite is intimately 

and irregularly iutergrown with the spodumene, and occurs in white, 

pearly, cleavable masses much resembling some varieties of albite. To 

some extent it is stained by dendritic manganese ; but in general the 

mineral is exceedingly pure. An analysis gave the following results, 

the lithia foeing determined by Gooch's process:

^ Ignition ....................................... ............ 1.03

SiO«............................................ .......... .77.29

AliOs...................................................... 10.95-

FftiOs.--.-................................................. trace.

MnO....................................................... trace.

LisO.. ..................................................... 2.62

NagO ...................................................... 2.39

K30 ...... ............................ ..................... trace.

100.28

2. SPESSARTITE FROM AMELIA COUNTY, YA. BY F. W. CLARKE.

This garnet, which is remarkable for its very high percentage of manganese, was analyzed at the request of Mr. G. F. Kunz. It occurs in the 

mica mines of Amelia county, in brilliant, brownish-red masses of considerable size. The specimen analyzed was very light in color, although 

some of the material was quite dark. The analysis was as follows:

Ignition .................................................... .27

SiOg........................................................ 35.35

A.\iOa..................... .................................. 20.41

Fe2 03 -...................................................... 2.75

FeO ........................................................ 1.75

MuO ....................................................... 38. 70/

MgO ....................................................... none.

CaO ........................................................ .94

100.17

3. OLIGOCLASE FROM BAKERSVILLE, K 0. BY F. W. CLARKE.

This mineral, which was also received from Mr. Kunz, has been described by him 1 and also by Penfield and Sperry.2 It occurs in color1 Amer. Jouru. Sci. (3), vol. 36, p. 222. 2 Amer. Journ.' Sci. (3), vol. 36, p. 324. 

Bull. 60 9 129
130 WASHINGTON LABORATORY. [BULL. 60.

less or nearly colorless fragments of extraordinary transparency. Indeed, it resembles glass so nearly that at first sight one can hardly 

realize that it is a feldspar. The composition of the sample analyzed 

was as follows:

Ignition .................................................... .25

Si02 ........................................................ 62.92

A1203 ....................................................... 25.32

Fe203 . 

MnO. 

CaO .. 

K2 0...

Na 20..

. trace. 

.: trace, 

.. 4. 03 

.. .96 

.. 6.18

99.66 

4. WlLLEMITE FROM THE TROTTER MINE,' FRANKLIN, K J.

F. W. CLARKE.

BY

Collected by Mr. W, S. Yeates, and at first thought to be a new mineral. The specimens obtained were nearly pure white, granular, and 

quite unlike ordinary willernite in appearance. The following partial 

analysis, however, served'to determine the species:

Ignition............................. ........................ .25

Si08 ...... .................................................. 27,41

ZnO........................................................ 68.86

96.52

A little manganese and iron are present, but were not determined.

5. DESCLOIZITE FROM BEAVERHEAD COUNTY, MONT. W. F.

HlLLEBRAND.

Through Messrs. W. H. Beck and George E. Lemon, of Washington, D. C., was received for examination a large lump of friable, uncrystallized material, having a dull yellow to pale orange color, and made 

up mainly of a vauadate, but carrying a large percentage of gangue. 

Two samples as pure as could be selected from different parts of the 

lump were analyzed with the following results:

PbO .............

CaO .............

FeO ..............

ZnO .............

VA - -.---..--.

As206 ... ..........

T> f\

HZ0 . ...... -I..

Si02 ...... ........

CaO...............

MgO...... ........

I.

56.02

1.16

0.70

15.96

0.32 

0.27

4.37

0.20

0.10

0.06

II.

55.84

1.13

0.70

15.91

20.80

4.36

0.16

Mean.

55.93

1.15

0.70

15.94

20.80

0.32 

0.27

4.37

0.18

0.10

0.06

99.82
)

> .1173

^

HILLEBUAND.] MINEEALOGICAL NOTES. ' 131

From I 27.62 per cent, of gaugue insoluble in cold dilute nitric has 

been deducted, and from II 22.20 per cent. Manganese was present in 

the gaugue in small quantity, apparently as pyrolusite, but it was not 

dissolved by the acid. The insoluble portion was found also to retain 

very small quantities of lead and zinc, which were estimated and in-' 

eluded in the analysis as probably belonging to the vanadate. The 

water had to be estimated indirectly by deducting from tbe total amount 

of water afforded by the dried mixture of vauadate and gangue that 

belonging to the latter alone, which was found as follows: The mixture 

dried at 100° 0., was dissolved in cold dilute nitric acid, and the insoluble matter, collected in a Gooch crucible, was dried at the same temperature, and then ignited. The loss on ignition gave the water in 

the gangue, there being no ferrous iron in the latter to influence the 

result.

Neglecting the traces of Si02 , CaO, and MgO, as probably derived 

from the gaugue, the following molecular ratio is obtained:

PbO ........................................ .25081

CuO ........................................ .0145!

FeO ........................................ .0097 f

ZnO ........................................ .1963J

V8 08 ........................................ .1140)

As2 05 -...................................... .0014 > .1173 or 1.00

P406 ........................................ .0019

HaO ........................................ .2428' 01-2.07

The water it will be noticed is double that required by descloizite, 

K4 (OH)2 (VO4 )2, but in view of the liability to error inherent in the 

method of water estimation employed, this is not deemed sufficient 

cause to separate the mineral from descloizite, although the close 

agreement of the two water determinations, made as they were on 

samples containing different proportions of gaugue, would indicate the 

correctness of the formula R4 (OH2 )(VO4 ) 2+H2O, which is ^hat of descloizite with a molecule of water of crystallization added.

This, so far as known, is the first observed occurrence of a lead 

vanadate in Montana. The precise locality of the mineral is the Mayflower Mine, in the Bald Mountain mining district.

6. PRELIMINARY RE MARKS ON NORTH AMERICAN URANINITES

BY W. F. HlLLEBRAND.

A large crystal nearly an inch in diameter from Andrews's formerly 

Hales's quarry, in South Grlastonbury, a few miles northeast of Middletown, Conn., showing octahedral, cubical, and dedecahedral faces, 

having been identified as uraninite with about 10 per cent, of thoria, 

the question arose: Was this thoria an essential constituent of the 

mineral or was its presence due to admixture of some thorium mineral, 

as thorite or orangite? With a view to settling this point a careful 

analysis was made accompanied by a microscopical examination of a 

thin section of the crystal. The results were not conclusive, therefore
132 WASHINGTON LABORATOEY. [BULL. 6&.

other material from the same locality was sought for and obtained from 

Prof. W. N. Rice and Mr. E. F. Sheldon of Middletown, Conn. Analysis 

showed its chemical identity with the first specimen, and established 

beyond question that the thoria could not be derived from any thorium 

silicate. The observation was made that unless certain precautions 

were taken the estimation of UO2 in the mineral was very unsatisfactory, and might be many per cent, too low. If a rather concentrated 

sulphuric acid is used for decomposing the mineral in sealed tubes, an 

insoluble uranous sulphate is formed which often crystalizes out in 

beautiful green crystals of considerable size, which dissolve very 

slowly when the contents of the tubes are emptied into cold water preliminary to titration with potassium permanganate. This defect was 

remedied by using a very dilute acid 1 vol. H2SO4 to 6 vols. H2O 

and the'final reaction was then as sharp as could be desired. A more 

important precaution to be observed is the manner of filling the tubes 

with carbonic acid gas. This must invariably be done by introducing 

the gas from a generator and sealing during its introduction, and never 

by using sodium carbonate in the tubes themselves. In the latter case, 

before the seal can be made, outside air in greater or less amount is 

certain to enter and its oxygen is sufficient to lower the percentage of 

UO2 found by several per cent., as repeatedly ascertained by actual experience.

The results thus obtained after employing every possible precaution 

to guard against oxidation of UO2 or reduction of UQ3 during the process of decomposing the mineral and'subsequent titration were perplexing to the last degree in view of the results arrived at by Comstock 1 

and Blomstrand 2 independently of each other, which appeared to prove 

definitely that all varieties of uraninite could be considered as orthouranates of uranium and lead, in which thorium and other metals of the 

earths might replace basic uranium. The Glastonbury uraninite could 

by no possibility be referred to an orthourauate, but was a decidedly 

basic salt.

In extension of the investigation uraninite from Black Hawk, Colo.r 

from North Carolina and from Branchville, Conn., was analyzed. The 

North Carolina material was so evidently in process of alteration, being seamed in every direction by very minute cracks filled with yellow 

decomposition products, that its analysis could give no clue to the relative proportions of the two oxides of uranium in the original fresh substance, but the presence of nearly 4 per cent, of rare earths mainly 

thoria was ascertained. The Branchville material was kindly given 

by Professors Brush and Dana, of New Haven, being the remainder of 

the stock from which the material for Cornstock's analysis was taken. 

Its re-examination was undertaken with the view of ascertaining whether 

thoria had not been overlooked, as would almost certainly be the case 

had ammonium oxalate instead of oxalic acid been employed as a test

'Am. Journ. Sci. (3), vol. 19, 1880, p. 220.

*Geol. For. Fork., VII, 59, 1884, and Journ. prak. Chem., XXIX, 191, 1884.
WHITFIELU. DUMORTIER1TE. 133

for the rare earths. This proved to be the fact, there being nearly 7 

percent, of thoria present in the mineral, which had undoubtedly been 

included in the UO3 of Comstock's analysis. This alone would utterly 

invalidate the formula assigned by him, but in addition the UOg was 

found uniformly higher by many per cent, than his analysis showed. In 

different samples selected from the material at my disposal, however, 

the percentage was not the same, but differed by several units, and the 

density rose always with the percentage of UO2 . The Colorado mineral, 

which unlike that from Connecticut and North Carolina does not occur 

 crystallized, is likewise not referable to an orthouranate, being as basic 

as that from Glastonbury, Conn. It is remarkable for the low percentage of lead less than 1 per cent, of oxide and for the absence of any 

other qualitatively similar element, as well as for the presence of about 

7 per cent, of zirconia j thoria being entirely wanting.

The question of the composition of this interesting mineral, which 

seemed so satisfactorily settled by the researches of Coinstock and 

Blornstrand above referred to, must hence be considered as again 

opened for discussion. My own analyses and experiments are as yet 

too indecisive to admit of forming any conclusions entitled to weight 

as to the probable constitution of the mineral,-but as opportunity offers 

they will be prosecuted, and extended to material from any other localities in this country or abroad that may become available, and will be 

published in detail at some future time.

Trifling amounts of rare earths other than thoria were found in the 

Glastonbury and Colorado specimens as well as in those from North 

Carolina.

7. DUMORTIERITE FROM NEW YORK AND ARIZONA. BY J. EDWARD WHITFIELD.

In the November (1887) number of the American Journal of Science 

Dr. E. B. Riggs published some observations, including a chemical 

analysis, on a mineral found at Harlem, N. Y., and generally supposed 

to be indicolite. The notice led to correspondence between Mr. J. S. 

Diller and Prof. E. S. Dana, the latter identifying it as dumortierite.

The composition, as determined by Dr. Riggs, conformed to no known 

mineral, and he was justified in provisionally calling it a new boro-silicate, but on further examination by Mr. Diller of a somewhat larger 

amount of material it was found that the mineral was associated with 

tourmaline, which no doubt accounts for the results of the analysis.

It was decided to analyze another portion which was known to be 

purer than that examined by Dr. Riggs. This was done, and the following figures are the results obtained: SiO2 31.44 per cent.; Al2Oa 68.91 

per cent., with the smallest trace of boric acid. Their quantities compare fairly well with the theoretical amounts necessary to satisfy M. 

Damour's formula Al8Si3Oi8 for dumortierite.

At about the time this work was being done on the New York
134 WASHINGTON LABORATORY. [BULL. 60.

^ s>

mineral, a small piece of rock from Clip, Arizona, was sent to the National Museum for identification. Prof. F. W. Clarke recognized it as a 

specimen of dumortierite accompanying quartz, and it was subjected 

to analysis to confirm his opinion. Following are the results of the 

examination :

^ Per cent.

SiOj........................................................ 31.52

AlaOs......................... ....-.... ......-........... 63.66 -

CaO........................................................ none.

MgO ....................................................... .52

TS&iO....................................... ................ .37

K20. ....................................................... .11

B203 ........................................................ 2.62

Ignition..................... ........................... 1.34

100.14

These figures show that the mineral was rather impure, and it was 

thought advisable to obtain, if possible, more of the mineral, and endeavor to separate it as far as possible from the accompanying rock. 

Mrs. C. A. Bidwell, the sender of the first specimen, kindly furnished 

quite an amount of much better material, in which the only mineral 

associated with the dumortierite was quartz.

As dumortierite is not acted upon by hydrofluoric acid, the rock was 

crushed to small particles and digested in this acid for a length of time 

sufficient to remove most of the quartz. The mass was then washed 

with water, dried, and any quartz that might remain was separated 

by Thoulet's solution. After thorough washing, the material was examined with the aid of the microscope and found to be free from gangue.

After being ground exceedingly fine and dried at 104° C. for about 

three hours, the material was analyzed with the following results :

Per cent.

Si03 ............ ............................................ 27.99

AUOa-.............................................. - .... 64.49

PaOs....-.......... .......'...-....... ................ -20

CaO .....-..-....-.......-.--...--...........--..-....-.-.. none.

MgO........................................................ trace.

B2 03 ........................................................ 4.95

H2 0........................................................ 1.72

99. 35

These figures show less impurity than the' first specimen analyzed j 

but if dumortierite is a simple silicate of alumina as stated, by M. 

Damour 1 these results either do not uphold his conclusions or they show 

the material to be a mixture of dumortiefite and some other compound.

If we assume the formula of M. Damour to be correct and estimate 

all the SiO2 in the analysis as belonging to the formula Al8Si 3Oi8 , then 

there will be left unaccounted for a small amount of A12O3 , H2O and

1 Ball, tie la Soc. Min. de France, vol. 4, p. G.
EAKINS.] XANTHITANE. 135

B2O3 , and these are present in the proportions represented by the formula A1B3O6 ,2H2O. If this mode of interpretation be correct, then the 

mineral from Arizona corresponds approximately to the formula,

3Al8Si3O18, 

A1B3O6.2H2O,

which requires A12O3 65.2 per cent., SiO2 27.6 per cent.; B2O3 5.4 per 

cent.; H2O1.8 per cent.; agreeing quite closely with the actual analysis. 

A borate of alumina corresponding to the above formula is, we believe, 

not actually known, and concerning its properties nothing can be predicated. If it exists, it is certainly remarkable that it should withstand 

the treatment with hydrofluoric acid which the Dumortierite received 

during the process of purification.

We are deeply indebted to Mrs. C. A. Bidwell for the supply of material for investigation, which at the cost of much personal labor she so 

liberally furnished.

8. XANTHITANE FROM NORTH CAROLINA. BY L. G. EAKINS.

Through the kindness of Mr. William Earl Hidden some fine speci-* 

mens of xanthitane were obtained, the material coming from Green 

Eiver, Henderson county, N. C. It was first described by C. U. Shepard 

in the American Journal of Science, 1856, vol.( 22, p. 96.

The material I examined is evidently an alteration product of sphene, 

following the form very closely. It is light yellow, friable, and mixed 

with impurities which can not be removed, preventing the determination of whether or not it is a definite mineral; but it is interesting from 

the fact that it apparently represents a clay with the silica replaced by 

titanic oxide.

Specific gravity 2.941 at 24°. The air-dried material loses 6.02 per 

cent, of water at 100°. The following analysis is on material dried at 

100°: .

Si02 ........................................................ 1.76

TiO2 ................................................ ........ 61.54

A1203 ....................................................... 17.59

Fe2O3 ............................... ......................... 4.46

CaO ........................................................ 0.90

MgO........................................................ trace.

VtO6 ........................................................ 4.17

H2O ........................................................ 9.92

100. 34

9. TRIPLITE FROM THE BLACK HILLS, DAKOTA. BY L. G. EAKINS.

The material for this analysis was taken from a large specimen of 

several pounds weight, in the collection of the National Museum. It 

comes from a tin mine near Eapid City, S. Dak. In reality it probably
136 - WASHINGTON LABOEATORY. [BULL. 60.

represents a mixture, but in general appearance it seems to be fairly 

homogeneous, and in composition it approaches closely to triplite.

It is brown in color, varying from light to dark, and translucent in 

thin pieces. In getting material for analysis any visible impurity was 

carefully picked out.

The composition is as follows:

Si02 ........................................................ .43

A1203 ....................................................... 8.74

Fe203 -..~...-i-............................................ 2.36

FeO ........................................................ 1.97

MnO........................................................ 29.13

CaO ........................................................ 6,72

MgO........................................................ trace.

K2 0 ........................................................ trace.

Na<jO ............................. .......................... 5.25

Li2 0............. .......................... ........: ........ .13

Pg06 .................. ...................................... 39.68

HsO .............................................. ........ 3.67

F........................................................... 2.35

Cl .......................................................... .25

C0a ......................................................... .26

100. 94 

Less O ..................................................... 1.05

99.89

10. KAOLIN FROM THE WATERFALL MINE, GUNNISON COUNTY, COLO.

BY L. G. EAKINS.

This mineral occurs in a large mass, filling a cavern which has been 

opened for mining purposes in Bedwell Basin, Gunnison county, Colo. 

It is especially interesting on account of being the containing mass of 

aggregates Of galena and pyrite crystals which are scattered irregularly 

through it.

It is very fine and white, and on slightly rubbing up with water the 

material as it comes from the mine it can easily be floated off jn a pure 

condition.

The analysis is as follows:

Si02 ........................................................ 47.28

A12O3 .................... v ................................. 36.19

Fe2O3 ................. r.............. ,1..................... trace.

CaO ........................................................ .42

MgO........................................................ trace.

K20 ........................................................ 5.74

Na,O ....................................................... .51

H2 0 ........................................................ 8.72

PS05 ........................................................ .57

99. 43
PYROXENE AND SERPENTINE. 137

11. NATIVE GOLD FROM PERSIA. BY CHARLES CATLETT.

The sample of gold, inclosing quartz, was submitted for assay through 

the State Department by the American minister to Persia, and was 

the property of the Persian Government. The specimen was of unusual interest as coming from a region so little known mineralogically. 

The native gold, which was of very light color, was analyzed with the 

following results:

Au..............-...I-.................-................../. 93.24

Ag...- ...................................................... 6.65

Fe... ....................................................... .11

Cu ......................................................... none.

100.00

12. PYROXENE AND SERPENTINE FROM MONTVILLE, N. J. BY

CHARLES CATLETT.

The series in question was collected by Mr. G. P. Merrill, of the National 

Museum, and submitted to this laboratory for analysis. It consisted of 

a dark gray, and a white pyroxene (A and B), and a dark and a light 

serpentine (C and D), resulting from their respective alteration. An 

alteration product (E) closely related to the others was analyzed at the 

same time.

SiOs . .............

CaO ..............

CaC03 ...... ......

MgO...... ........

MgCOg...... ......

A1203 . ............

Fe203 ...... .......

FeO ..............

MnO...... ........

80s ............ ...

KS0...... .........

Na.,0...... ........

A.

51.45

i na

24.02

18.43

2 Qd

LOG

.96

99.94

B.

48.17

* 19

21.96

10.44

17.61

.71

.52

.18

.24

99.95

C.

40.23

14.24

39.46

2.18

4.02

100. 13

D.

49 Qfl

14.12

19 11

.07

Q7

.17

99.85

E.

4 39

* 1. 26

87.75

4.07

1.67

i ...

.13

.12

.28

99.70

THE SUBSIDENCE OF FINE SOLID PARTICLES IN LIQUIDS.

[Second Paper.]

 By CARL BABTTS.

(1) In my earlier work I endeavored to analyze the phenomenon of 

sedimentation into parts such that the conditions under which subsidence is to be explained from a chemical, or from a physical point of 

view, may be better discernible.1 To do this I first considered the question in its purely mechanical aspects.2 If P is the resistance encountered by a solid spherule of radius r, moving through a viscous liquid 

at a rate a?, and if Ic be the frictional coefficient, then P=Q7fTcrx. Again, 

the effective part of the weight of the particle is 'P'=$icr* (p p1 ) g, where 

q is the acceleration of gravity and p and p1 the density of the solid 

particle and the liquid, respectively. In case of steady motion P=P'. 

Hence v

........ (1)

In any given case of thoroughly triturated material, the particles 

vary in size from a very small to a relatively large value; but by far 

the greater number approach a certain mean figure and dimension. An 

example of this condition of -things may be formulated. To avoid 

mathematical entanglement I will select

y ax3 \ 2e~x2 .......... (2)

where y is the probable occurrence of the rate of subsidence x. If 

now the turbidity of the liquid (avoiding optical considerations) be

1 The present article, being a continuation of Bull. U. S. G. S., No. 36, 1886, is largely 

based on the experimental evidence there tabulated. Mr. William Durham (Chem. 

News, vol. 30, 1874, p. 57 ; id., vol. 37, 1878, p. 47),waa the first to give an incentive 

to this class of experiments.- Much of our knowledge of the effect of precipitants is 

due to him. Moreover, the theoretical views at which he ultimately arrives may be 

regarded as a definite point of departure. In this country, Prof. T. S. Hunt (Proc. 

Boston Soc. Nat. Hist., Feb., 1874), Prof. W. H. Brewer (National Acad. Sc. 1883; 

American Journ. Sci., series 3, vol. 29, 1885, p. 1), and Prof. C. R. Stuntz (Cincinnati 

Soc. Nat. Hist., Feb., 1886), have occupied 'themselves with similar work. Professor 

Stuntz's paper contains further references among others to Waldie's results (Jourual 

Asiatic Soc., Bengal, 1873; Chem. News, 1873). Meanwhile Mr. William Hallock has 

made experiments on the subsidence of lamp-black in connection with his work on the 

density of that substance. (Of. Bull. U. S. G. S., No. 42, 1887, p. 132 ) I may add that 

my own experiments were suggested by Professor Brewer's memoir.

2 Cf. Kirchhoff: Matliematische Physik, lecture 26, § 4, 1876.

139
140 WASHINGTON LABORATORY. [HULL. 60.

s,

defined as the mass of solid material per unit of volume of liquid, then 

the degree of turbidity which the given ydx particles add to the liquid 

is, caet. par., proportional to r3ydx, where r is the mean radius. Hence 

the turbidity T, at the outset of the experiment (immediately after 

shaking), is

$r3ijdsc=T0 

u o

where equations (1) and (2) have been incorporated.

If the plane at a depth, d, below the surface be regarded, then at a 

time, t, after shaking, the residual turbidity there is

(3)

This equation describes the observed occurrences fairly well. In proportion as1 the time of subsidence is greater, the tube shows opacity at 

the bottom, shading off gradually upward, through trauslucency, into 

clearness at the top. If, instead of equation (2), there be introduced 

the condition of a more abrupt maximum; if, in other words, the particles 

be very nearly of the same size, then subsidence must take place in 

unbroken column, capped by a plane surface which at the time zero 

coincided with the free surface of the liquid. Again, suppose one-half 

of the particles of this column differ in some way uniformly from the 

other half. Then at the outset there are two continuous columns coinciding, or, as it were, interpenetrating throughout their extent. But the 

rate of subsidence of these two columns is necessarily different, since 

the particles, each for each, differ in density, radius, and frictionai 

qualities by given fixed amounts. Hence the two surfaces of denaarkation, which at the time zero coincided with the free surface. In general, 

if there be n groups of particles uniformly distributed, then at the time 

zero n continuous columns interpenetrate and coincide throughout their 

extent. At the time £, the free surface will be represented by n consecutive surfaces of dernarkation, below it, each of which caps a column, 

the particles of which form a distinct group. This phenomenon is 

Professor Brewer's stratified subsidence. In the case of particles 

which have undergone an earlier fractionated sedimentation, either in 

nature or in the arts, the occurrence of groups possessing the distinctive characteristics here discussed is not improbable. On the other 

hand, when during subsidence the surfaces of demarkation follow each 

other in regular succession, one is tempted to look for something more 

than an adventitious cause for the phenomenon. An orderly arrangement of groups of particles, might for instance, indicate successive 

stages of hydration. (Of. § 6.) In case of stratified subsidence it is convenient to speak of orders of surfaces, numbering them from the top 

downward. It is not uncommon to observe seven or even ten consecutive orders.
BARUS.J SUBSIDENCE OF PARTICLES IN LIQUIDS. ^ 141

(2) With these deductions as a point of departure, I then attempted 

to find relations between rates of subsidence, the viscous and capillary 

properties of the liquid, and its electrical behavior under analogous 

conditions of concentration and of temperature. This general survey 

proved that the phenomenon of sedimentation is unique; that the frictional resistances encountered by the particles are apparently different 

from the viscosities of the liquids in which subsidence takes place; that 

many of the occurrences observed are closely allied to the electrolytic 

and the capillary properties of this liquid. Finally, utilizing Professor 

Brewer's stratified subsidence, which I obtained very clearly with 

certain kinds of tripoli, I commenced a series of more rigorously 

quantitative measurements, showing that, caet. par., rate of subsidence 

is primarily dependent on the turbidity of the mixture.

In my experiments with tripoli, the observed rates of subsidence 

( cm/ (sec x 106 )) in ether, alcohol, water, glycerine, were 7500,1300,3,0.9, 

respectively; but, owing to the difference in character of the divers 

precipitates, these figures have no further signification than to emphasize the said difference in character. (Of. §§ 5,6.) Let water and ether 

be mixed so that there shall be equal bulks of etherized water below and 

aqueous ether above, and then let the dust (bole) be added. If now 

the mixture is violently shaken and then allowed to subside, the ether 

is washed clean of particles in a few minutes, whereas the sediments 

remain suspended in the water for weeks and even months. Here, 

however, the separation and subsidence are promoted by the surface 

energy of water. On the other hand, if dry tripoli be added to ether dried 

over CaCl2, in a test tube, and if the tube be held obliquely after shaking, subsidence is so rapid that the upward current of ether along the 

upper line of the tube is almost tempestuous.

The close relation of the present phenomena to electrolytic phenomena appears at once by observing that so little as a single molecule of 

HC1 (for instance) added to 10,000 or even to 50,000 molecules of H2O, 

produces appreciable increase of the rate of subsidence. Remembering 

that the arrangement is in three dimensions, and supposing the molecule HC1 as large as the molecule 1 H2O, the effect of the molecule 

HC1 must be appreciated at a distance of at least 30 times its own radius, 

and extend much beyond this asymptotically. Quiucke's radius of capillary attraction, ,000005cm, being about 100 times the molecular radius 

H2O, it appears that the striking effect of the molecule HOI in accelerating subsidence is not an abnormal occurrence, at least when considered physically. Other points of view are given in the Bulletin.

(3) To account for these phenomena as a whole, Mr. Durham in his 

second paper (1. c.) proposes a hypothesis in virtue of which the scope 

of the action of affinity is enlarged, and suspension regarded as the 

lower limit of solution. This view is fast gaining ground; nevertheless,

1 The estimated diameter of H2O, distance between centers of adjacent raoleculea 

=40/109cm. Kohlrausch. Wied. Aiin., vol. 6, 1819, p. 209.
142 WASHINGTON LABOKATORY. ! BULL. 60.

without concise experimental reference to the density and size of the 

solid particles, and the viscosity of the liquid, Mr. Durham's explanation contains no sufficient reason for the observed suspension, nor for 

changes of rate of subsidence. Prof. Brewer's ingenious hypothesis of 

colloidal hydrates, so constituted that the particles may ultimately swell 

up and float, something like gelatinous silica, or even like starch grains, 

is more direct; and before further reasons of the cause of suspension 

are sought, the validity of this inference must be tested. This test is 

feasible, I think. If the phenomenal difference of rate with which the 

same particles subside in water and in ether is due to volume changes 

of the particles, then a marked difference in the density of the sediment 

(clay or tripoli) in water and in ether, respectively, must be experimentally demonstrable. Of. Equation (1). I made these experiments with 

both solids, using two nearly identical density flasks, one for water and 

the other for ether, in the usual way. The powders were sampled and 

dried at 200° in an air bath, for half a day, transferred to the pyeuometers, dried and weighed when cold. They were then left in a desiccator for 18 hours and again weighed; and finally dried in vacuo, 

and weighed. The results throughout were satisfactorily constant. By 

aid of an apparatus specially devised for the purpose, the two flasks 

were once more thoroughly exhausted (mercury air-pump), and then 

filled with water and with ether, respectively, in vacuo, over sulphuric 

acid. In both cases (experiments made consecutively) the vacuum 

ebullition was kept up for some time to give full assurance of the expulsion of air, etc. The density of the ether had been previously determined 

by the same flasks, once for each experiment.

I thus obtained for tripoli

In water, density=Jw =2.672, 

In ether, density=^e =2.697.

Again I obtained for white bole

In water, ^=2.639, , '

In ether, Ae -2.663.

The manipulation being somewhat difficult, the observed differences 

of Aw and Jc are no larger than the many sources of error led me to 

anticipate, particularly in view of the fact that the two samples, for 

ether and for water, may not have been absolutely identical. The concentrated ether used was the same commercial reagent with which I 

obtained the subsidence phenomena. In consequence of the high but 

normal values of both Aw and Je , I saw no need of specially purifying 

it. I add finally that after calcination the dry tripoli Tost 1.2 per 

cent, in weight, and the dry bole about 11.4 per cent. In both cases this 

is probably water of constitution, the elimination of which was of course 

not permissible. It is well to note that in spite of differences of chemical composition, bole particles are about equally well suspended before 

and after calcination, and the phenomena with ether dried over Ca012 

are identical with the above.
BARUS.] SUBSIDENCE OF PARTICLES IN LIQUIDS. 143

(4^ These results show that the densities in the two cases (sediment 

in water and in ether respectively) are not essentially different. Moreover, the density of tripoli is so near that of quartz, and the density 

of bole so near that of kaolinite, as to leave the hydration hypothesis 

very seriously in the lurch, so far as favorable evidence is concerned. 

It is improbable that the addition of water to the dry powder is accompanied by sufficiently marked volume changes ; it is certain that the 

enormous variation of rates of subsidence actually observed, when the 

particles descend in water, in solutions, and in ether, must be referred 

to some general cause apart from the.density of the particles and the 

viscosity of the liquids.

(5) This premised, the explanation of sedimentation may, I think, be 

satisfactorily based on the following principle: If particles of a comminuted solid are shaken up in a liquid, the distribution of parts after 

shaking will take place in such a way that the potential energy of the 

system of solid particles and liquid, at every stage of subsidence, is the 

minimum compatible with the given conditions. In the case of solid 

particles and pure water the configuration answering these conditions 

is schematically

Particle,' water.. . particle, water.

In the case of solid particles and ether, or of solid particles and solutions, this configuration is schematically

Particle, particle... .ether, ether.

For the truth of this inference, iny paper contains abundant experimental evidence. The principle asserts that in case of water the sediment is graded and the suspended material granular, whereas in ether 

the sediment is apparently homogeneous, as I found; that the bulk of 

sediment is necessarily less in water than in ether, being compact in the 

first instance and of a microscopically arched or castellated internal 

structure, in the second instance, as I found ; that the effect of a precipitant is particularly marked when the mixture is densely turbid with 

relatively coarse particles, as I found; that, finally, the phenomenon of 

sedimentation must be of a distinct and special kind, and by no means 

the immediate converse of capillary viscous transpiration. The inferences are thus based on equation (1) above, and follow at once when k and 

p are constant. In the Bulletin I computed the relative size (radii) of 

the particles of tripoli subsiding in water, alcohol, ether, to be 1,19, 

and 24, respectively.1 It is exceedingly curious to note in case of water,

irrhis is the first hypothesis developed in detail in Bull. U. S. Geol. Survey, 

No. 36, pp. 34, 35, 37. In a recalculation since made with more accurate value of A; 

(water 0° to 100°, Slotte's data, in Wied. Ann. vol. 20, 1883, p. 262; ethyl and 

methyl alcohol, Graham's data in Phil. Mag. (4), vol. 24, 1861, p. 238; ether datum 

from Landolt and Boerustein's tables, p. 153 ; glycerine ?7=10.0g cm. l sec. 1 , estimated 

roughly), the radii of the particles in water, ethyl alcoho], methyl alcohol, ether 

and glycerine are found to be r=0.000009cm, 0.00019cm, 0.00018cm, 0.00020cm and 

O.C0005cm, respectively. In case of bole suspended in-water at 15° and at 100°, the 

radii were approximately <0.000010cm and> 0.000020cm, respectively. Section 6
144 WASHINGTON LABORATORY. [BULL. 60.

despite the phenomenally large surface energy of the liquid, the subsidence takes place in such a way that for a given mass of suspended sediment the surfaces of separation are a maximum. On the other hand, 

in case of subsidence in ether, or in salt solutions, the solid particles 

behave much like the capillary spherules of a heavy liquid shaken up 

in a lighter liquid with which it does not mix. In other words, the 

tendency is to reduce surfaces of separation to the least possible value, 

large particles growing in mass and bulk mechanically, at the expense 

of the smaller particles. Finally it is clear that the condition of stratified sedimentation is very slow subsidence of a granular precipitate.

(6) The experimental evidence adduced bears directly on the size of 

the particles of any precipitate. A given mass of small solid particles 

presupposed, the observations of the foregoing paragraphs make it 

probable that the potential energy of the system of solid particles and 

liquid increases with the radius of the particle. These observations 

also show that the potential energy of the system of solid particles 

alone decreases as the size of the particles increases, a state of things 

due both to the immediate action between solid particles and probably 

also to the surface energy of the liquid in which suspension takes place. 

Under these conflicting conditions it is probable that there is a critical 

shell within which the energy solid-liquid decreases less rapidly than 

the energy solid-solid; and beyond which shell the energy solid liquid 

increases more rapidly than the energy solid-solid. This critical shell 

being compatible with the conditions0 of minimum potential energy of 

the subsiding system, as a whole, is the size of the precipitated particles; 

for any change of the radius of a particle bounded by the critical shell, 

implies an expenditure of work, which under the usual conditions of 

subsidence is not available.

(7) t have finally to endeavor to assign some value to the radius of 

the critical shell for the case of the above water suspensions. In iny

experiments with tripoli, rates of subsidence, ac in cm/ (sec x 106 ), varied 

from x=\ to #=20, according as higher orders of surfaces or turbidities of lower degree were chosen. Taking the more usual value x=3, 

the radius of the particles subsiding was probably not less than 400 

times the molecular radius of water. The bole particles under analogous 

conditions of suspension in H2O, were smaller, probably only 100 water 

radii. In Professor Brewer's indefinitely suspended clays, the limit of 

comminution can not be estimated at all, except perhaps from purely 

optical consideration.1 Whether in this extreme case colloidal hydrapoints out, that whereas these dimensions may be called in question when considered 

absolutely, the relative values of radius are probably true.

The fact that particles so extremely light descend at all is a most striking result, 

showing the extreme delicacy of these experiments. In case of tripoli-water, for 

instance, the estimated weight of particles is only 1/1011 milligram. Being invisible 

microscopically it must weigh less than 1/1010 milligram.

1 The optical properties of light reflected from particles small in comparison with 

the wave length of light are discussed by Stokes (Phil. Trans., 1852, p. 530). How 

large a particle may be without interfering with optical clearness, I can not say.
BAUDS. J SUBSIDENCE OF PARTICLES IN LIQUIDS. 145

tion with concomitant volume changes is still demonstrably absent, 

remains to be seen. To test it, a sufficient quantity of the extremely 

fine material would have to be collected and dried by low temperature 

evaporation, an excessively tedious task.

Again, in Bulletin No. 35, p. 21, I point out at some length that 

"when the particles decrease (in size) from some estimable mean value 

indefinitely," liquid viscosity, being at least partially, if not largely 

kinetic in character, can no longer be considered constant; that therefore a particle may descend, or in other words the continuous and 

constant action of gravity produce an effect even when the weight of 

the particle is below the mean or physically measurable value of the 

friction encountered; that the limits of time-variation of viscosity willincrease as the radius of the circumscribed space decreases. In such a 

case the particle to be stationary must weigh less than the lower limit 

of the variable Anscosity a quantity which may reasonably be conceived 

to,approach zero very nearly. I carried these inferences one step 

further by supposing, rationally I think, that the limits within which 

this elementary viscosity (say) varies, will increase with the degree of 

molecular agitation of the liquid. On the basis of this postulate I 

then endeavored to explain sedimentation kinetically, both in its relation 

to temperature and the effect of precipitauts.

One point which antagonizes this hypothesis in part must not be lost 

sight of. Two or more particles sufficiently near together tend to screen 

each other, and, receiving impact mainly on their outer surfaces, will be 

held in permanent coherence so long as the conditions of pronounced 

molecular agitation last. This is observed to some extent in solution 

suspensions, ether suspensions, and in water suspensions at high 

temperatures (100°). There is therefore some difficulty in preserving 

the granular state (Bull. 36, p. 38).

To pass judgment on the validity of such an explanation, it is necessary to have in hand better statistics of the size of the particles relatively to the water molecules than are now available. Indeed whether 

the liquid water molecule is simply H2O and not some more complex 

form can not at the present state of science be decided. Inasmuch as 

the particles in pure water are individualized aud granular, it is 

apparently at once permissible to infer the size of the particles from 

the observed rates of subsidence. But my observations show that the 

said rates decrease in marked degree with the turbidity of the mixture. 

Hence the known formulae for a single particle are not rigorously applicable though it can not be asserted whether the cause of discrepancy is 

physical or mathematical in kind. It follows that special deductions 

must be made for stated groups of particles before an estimate of their 

mean size can be fairly obtained. 

Bull. 60 10

A NEW METHOD OF MAKING ALLOYS.'

BY WILLIAM HALLOCK.

While occupied with a careful study of an article by W. Spring 2 on 

the production of Wood's alloy, and seeking the forces possibly brought 

to bear in his experiments, the following explanation occurred to ine, 

and was subsequently verified by critical experiments. The method of 

production used by Mr. Spring was to mix filings of the four metals iu 

the proper proportions, subject the mass to a pressure of 6,000 atmospheres, file up the block thus produced and compress it a second time, 

obtaining as an end result a block of Wood's alloy.

Now, if at any time during the various operations, be it the first 

compression, the subsequent filing, or the second compression, or if anywhere in the whole mass, the original metals came in contact all 

together, then at that point \ve should have a particle, a molecule as it 

were, of Wood's alloy. If thereafter the temperature ever rose to 70° 

0., that particle would melt and dissolve down its immediate neighbors 

until finally the whole mass was liquefied and converted into a homogeneous mass of alloy. Without waiting to consider how improbable 

it was that the three or four metals could be brought simultaneously 

into perfect enough contact to act as a real alloy, I tried the experiment and it proved an easy success.

The metals were filed to fine grains and mixed in the proper proportions, one part cadmium, one part tin, two parts lead, and four parts 

bismuth. A glass tube of 5mm inner diameter and 70mm length, sealed 

at one end, served as containing vessel. About 6 grams of the mixed 

filings were placed in this tube and packed down, an iron wire 3mm 

diameter, held between the thumb and finger, being used as a packer; 

which certainly eliminated the possibility of any considerable pressure. 

The tube was thereupon so placed upon the water-bath that the sealed 

end containing the rnetals projected downward into the boiling water. 

In this way the filings remained dry and were kept at a temperature of 

98° to 100° C. After remaining in this position for eighteen hours 

(over night) the filings showed signs of sinking together, which would

1 Kead before the Philosophical Society of Washiugtou, D. C., at the meeting of 

February 1.8, 1888. 

* W. Spring: Ber. der Cheiu. GeselL, vol. 15,1882, pp. 595-597.

147
148 WASHINGTON LABORATORY. \UULL. W.

indicate a beginning of the reaction. The tube was jarred upon the 

table to assist the condensation and again placed on the bath. Two 

hours later the tube contained a homogeneous liquid globule of Wood's 

alloy. The experiment was repeated, using two larger tubes, into which 

the metals were packed with a lead pencil, and producing some 30 

grams of alloy. Of course when the operation is once started there is 

no limit to the quantity which can be produced. One tube remained 

on the water-bath over a week without signs of a solution and yet 

finally dissolved.

In further application of the same principle lead and tin were meltel 

together at 190° to 200° 0. by simply laying a piece of tin upon a carefully cleaned piece of lead and placing the whole in an air-bath at 190° 0. 

A few hours suffice for this experiment. The melting points of the 

above metals are cadmium 315° 0., tin 230° 0., bismuth 267° 0., lead 

325° 0. Potassium and sodium were also used, melting at 62° 5' C. and 

95° 6' C. respectively.

A very interesting and striking experiment is the production of the 

alloy of equal parts of potassium and sodium, which is liquid at temperatures above 0° 0. Pieces of the two metals are simply placed with 

freshly cut surfaces in contact and slightly pressed together; in a few 

seconds the liquid alloy, which resembles mercury, is visible in drops 

around the contact surface, and an hour or two suffices to produce 

several cubic centimeters of the fluid.

It is my intention in the near future to follow up these observations 

by a series of experiments intended to establish and extend the principle 

here illustrated. The heat phenomena which doubtless accompany 

these reactions will also be investigated. Possibly also some electrical 

manifestations may be discovered, and perhaps some facts bearing upon 

the origin of contact electricity may be developed. In the mean time I

would propose the following law: An alloy can be produced out of its 

original constituents without considerable pressure if the temperature 

be above the melting point of the alloy, even though it be far below 

the melting point of the most easily fusible constituent.

Probably this law will also be found applicable wherever under the 

existing circumstances the product is a liquid, even though the original 

substances be solids.
MISCELLANEOUS ANALYSES.

BOOKS COLLECTED BY B. D. IRVINO.

A. Separations from the gabbro of Ashland County, Wis.: 1, Feldspar; 2, diallagej 3, magnetite, partial.

[Analyses by \V. 3T. Hillobrand.l

H20 ..............

SiOa .............. 

Ti02 ....... .......

PsOs - -.-- . --

A120S .......... ... 

Fo803 . .........

.FoO ..............

MnO. ............. 

SrO.JBaO. ......... 

CaO...... ......... 

MgO.... ........ ..

K.,0. ..............

Na2 0 .............

Li20..............

No. 1.

23

53.30

29.03 

.55

.23

none, 

traces. 

31.40 

.13

.40

4.87

100. 14

No. 2.

.33

40.80 

1.29

2.80 

2.48

10. 82

.37 

none. 

16. 50 

15. 33

.12

.51

100.41.

No. 3.

8.47

50. 29

30. 70

89.46

B. Garnet, separated from the garnetiferons actinolite schist of 

Penokee Gap, Wis.:

[Incomplete analysis on only 0.54 gram, by T. M. Cbatard. |

SiO2 ........................................................ 39.31

AlaOs........................................................ 12.86

Fe3O3 (total iron)........-......--. .......................... 46. (56

MnO............ ............................................ 1.03

CaO ........................................................ 1.88

MgO........................ ... ............................ 1.90

103.64

The excess, 3.64, is oxygen added to ferrous iron. Correcting, \ve have 

approximately Fe2O;) , 10.21 j FeO, 32.81.

C. Limestones and iron carbonates: 1, Limestone, near Sunday 

Lake, Gogebic district, Mich.; 2, Limestone, Penokee region, Wis.; 3,

149
150 WASHINGTON LABORATORY. f BCLL. GO.

cherty iron carbonate, Gogebic district; 4, iron carbonate, outlet of 

Sunday Lake; 5, iron carbonate, Palms mine. Gogebic district.

[Analyses by "W. F. Hillebrand.]

H20 ..............

C02 . ..............

Si02 ..............

Ti02 ...... ........

T> Cl

01 ................

A1203 - ...... .-----

Fe203 . ............

FeO ..............

MnO...... ........

CaO ..............

MgO .............

FeSj... ...........

No. 1.

.30

45.31

3.07

.0!)

.86

.15

29.72

19.95

99.45

No. 2.

.27

40.27

.63

.03

.75

.08

30.94

20.68

99.65

No. 3.

.54

41, 10

3.16

.06

.08

.93

15.18

1.15

26.65

11.01

.34

100. 20

No. 4.

.68

25.21

28.86

.20

1.29

1.01

37.37

07

.74

3.64

99.97

No. 5.

.60

19.24

46.47

.10

(?)

.70

.86

28.57

.40

.49

2.30

99.73

(Same series continued): 6, Iron carbonate, Miner and Wells' option, 

Sec. 13, T. 47 K,E. 46 W., Michigan; 7, " iron carbonate," bed of Slate 

Creek, Huron Bay slate quarries, Michigan; 8, iron carbonate, north, 

west £ Sec. 18, T. 47, R. 45 W., Minnesota; 9, slaty rock, supposed iron 

carbonate, bed of Cross River, near Gnnflint Lake, Michigan.

[Analyses by T. M. Chatard.]

H20 ..............

CO2 . ..............

Si02 ..............

Ti02 ......... ....

T> (~\

S03 - ..............

A1203 ...... ..----.

Fe203 . .........

FeO. .............

MnO..............

CaO ..............

MgO.... ..........

No. 6.

1.71

17.72

46.01

.12

.07

.15

.83

1.35

26.07

2.04

.63

2.86

99.61

No. 7.

.25

39.68

7.05

.27

.21

.48

1.33

.19

50.08

.57

100.11

No. 8.

1.52

22.44

36.73

.19

.01

.16

.38

.98

34.81

.52

.48

2.74

100. 96

No., 9.

1.99

.41

.60

.20

.60

14.45

1.84

4.54

.11

2.33

2.34

K20. 5. 03

Na,20. 1. 37 

100. 58

(Same series continued): 10, Iron carbonate, west end of Gunflint 

Lake, Minnesota; 11, iron carbonate, north side of lake; 12, limestone, 

east end of Ogiskemannissi Lake, Minnesota; 13, limestone, north side 

of Gunflint Lake, Canada.
CUATAKU.] MISCELLANEOUS ANALYSES.

[Analyses by T. M. Gliataril.]

151

H,0 ..............

C02 .... ...........

Si02 ..............

TiO»...... ........

P

/-\

S03 ...............

A1203 -.... ........

Fo208 ~. ..........

FeO ..............

MnO.. ............

CaO ..............

MgO...... ........

'No. 10.

2.08

5.22

58.23

OQ

.19

.06

5. 01

18.48

.25

.38

9.59

99.52

No. 11.

1.22

19.96

46.46

no

.14

.24

26.34

.21

1.87

3.10

100. 31

No. 12.

1.07

24.70

41.99

.05

.32

1.24

.42

4.77

,20

10.85

8.41

100. 08

No. 13.

.99

32.42

23. 90

.17

.07

.44

10. 72

.28

22.25

8.52

99.76

H2O

NOVACUL1TE FORM MARQUETTE, MICH. 

[Collected by G. H. "Williams; analyzed by "W. F. Hillebrnnd.]

2.35

Si02 ........................................................ 76.99

P2O5 .............................. ...... .................... trace.

AlaOs ....................................................... 13.92

................................................... .45

FeO ....................................... ............ .77

MnO........................................................ trace.

CaO ........................................................ .32

MgO......................:................................. 1.12

K.,0 ........................................................ 3.65

Na,0......................................................... .56

LisO ............................ ...... ............ .......... trace.

100.13

BRICK-CLAY FROM NEW ULM, MINN.

Color greenish-gray. Brick made from it is reddish-brown, strongly 

sintered, somewhat fractured. Eeceived from Hon. John Lind.

[Analyzed by T. M. Chatard.) 

Ignition .................................................... 10.73

Si02 ........................................................ 61.32

Ti02

S03

.66 

.27 

.19

Al80s...... .................................................. 12.27

FeaOs..... .................................................. 3.62

FeO .

MuO. 

BaO , CaO .

4.18

.27

.05

.99

1,76

3.59

.42

100,32
WASHINGTON LABORATORY. (BUM,. (JO.

ROCKS FROM MONTANA. 

[Collected by A. C. Peale and G-. P. Merrill.]

A. From hills east of Fort Ellis: 1, Bock, analysis by T. M. Chatard; 

2, ground mass; and 3, portion soluble in hydrochloric acid? analyzed 

by L. G. Eakins.

H20 ..............

Si02 ..............

Ti02 ...... ........

P f\

A1203 .............

0,0* .............

FeO......... ......

MnO...... ........

CaO...... .........

MgO. .............

K2O...... .........

Na,jO...... ........

A.I.

5.42

46.90

.41

.44

10.17

.33

1.22

5.17

.10

C.20

20.98

2.04

1.16

100. 54

A. 2.

1 90

65. 23.

17.48

.98

3.08

2.02

4.63

3.79

99.11

A. 3.

20.88

3.89

2.21

4.28

1.01

16.44

51. 29

100. 00

B. From hills north of Camp 6 (Peale), East Gallatin River.

C. Partial analysis of vein from rock north of East Gallatin Eiver.

[Analyses by L. G-. Eakiiis.]

H2O .............. 

SiO* ..............

TiO....... ........

PgO....... ........

C02 ...... .........

A1203 ...... .......

CraO3 . ............

FoaOa-.. ..........

FeO ..............

MnO..............

BaO...... .......

CaO .............. 

MgO.............. 

K.O ..............

NozO .............

13.

4.14 

49.47

.21

.37

3.31

12.15

1.93

4.07 

.10

.03

9.30

10.80 

2.42

2.08

100. 44

C.

65. 19

16.38

2.31

.56 

8.09

1.71

94, 24
MISCELLANEOUS ANALYSES. 153

D. From Cotton wood Creek: 1, Rock, analysis by T. M. Chatard; 

2, portion soluble in dilute hydrochloric acid, analysis by L. Gr. Bakins.

H20 ..............

Q!rt

Ti02 ...... ........

P

r\

S03 . ..............

A1203 . .......... -

Cr203 . ...... ... r ..

Fe203 - -- ..........

FeO ..............

MnO.... .........

BaO ..............

CaO ..............

MgO...... .......

K20 ..............

Na-jO .............

D.I.

3. 19

51.65

.55

.21

.19

13.89

.08

2.70

4.80

.15

.19

4.07

11.56

4. 15

2.99

100. 37

D.2.

12 94

2.93

> 5.07

OPi

8.28

.33

.39

30.90

E. Porphyrite, Cottonwood Creek: 1, Complete; 2, portion soluble 

in dilute hydrochloric acid.

[Analyses by L. G-. Eakins.l

H20 ..............

Si02 ..............

TiOz ...... ........

PA-..--.---.---.

A1203 . ............

Fe203 ..... ........

FeO ..............

MnO..............

BaO ..............

CaO ..............

MgO.............. 

K20 ..............

Na^O .............

Ji.l.

1 OR

52.33

.14

1.02 

15.09

4.31

4.03

.09

.07

7.00

0.73 

3.70

3.14

100. 45

E.2.

13.62

5.93

.08

.78

20.41
154 WASHINGTON LABORATORY. [BULL. GO.

F. and G. Two rocks from northwest of Cottonwood Creek.

[Partial analyses, as requested, by L. G. Eakins.]

SiOg. .............

A1A - 

Fe203 ------------

CaO ..............

MgO.... ..........

K20 ..............

Na20 .............

E.

62.98

18.44

9 4Q

1.79

4.35

5.58

95. 63

G.

54.29

18.47

5.67

3.69

3.98

5.92

4.13

96.15

H. Eight carboniferous limestones. Analyses by 0. Catlett: 1, north 

of East Gallatiu Elver; 2, west of North Bowlder Eiver; 3, 4, north of 

East Gallatin Eiver; 5, west side of Bridger Eange, base of carboniferous ; 6, north of Gallatin Eiver, middle formation; 7, 8, north of 

Gallatin Eiver, upper formation.

CaCOj...... 

MgCOg...... 

Fe203 .......

A1203 -------

In soluble . . . 

Water, etc..

H.I.

54.54 

43.63

| .22

.34 

undet.

98.73

H.2.

54.54 

42.62

.40

a L 78 

undet.

99.34

H.3.

67.85 

6.18

2.50

23.50 

undet.

100. 03

H.4.

59.11 

1.96

1.92

35.26 

undet.

98.25

H.5.

88.50 

.95

.38

9.98 

undet.

99. 81

H.6.

91.96 

1.35

.58

5.99 

undet.

99.88

H.7.

32.28 

13.91

.30

50.74 

undet.

97.23

H.8.

40.21 

' 25.25

5.30

'>5. 24 

uudet.

96.00

ERUPTIVE ROCK FROM THE HENRY MOUNTAINS, UTAH.

[Received from J. S. Diller; analyzed by B. B. Biggs.]

................................................. .69

................................................... 63.16

.................................................. .21

.................................................. .12

.................................................. trace.

.................................................. 17.21

................................................... 2.43

.................................................. 2.30

MnO ........................................................ trace.

CaO.. ............. ..................................... .... 6.27

MgO........................................................ 1.27

SrO... ..................................... ................. trace?

BaO ........................................................ .09

.................................................. trace

H20 .. 

SiO2 . 

Ti02 . 

P205 . 

S03 ... 

A1203 . 

Fe203 

FeO ..

Li 20 .

K2O

4.70

1.84

100.29
EAK1N8.) MISCELLANEOUS ANALYSES. 155

ROCKS FROM NEW MEXICO. 

[Collected by J. W. Powoll; analyzed by L. G. Eakins.l

A. Obsidian from Obsidian Hill Camp.

Hso ........................................................ .33

Si02 ......................................................... 76.20

TiO-2...............................................'......... trace.

A1203 ....................................................... 13. 17

Fe303

FeO ..

MnO.

CaO.

MgO..

K2O ..

NaaO.

.34

.73

.10

.42

.19

4.46

4.31

100,25

Specific gravity...................................... 2.352, 23° 5'

B, C, D, and E. Four basalts, Rio G-rande Canon.

H20 ........

C02 .........

Si02 ........

TiO*. .......

T> n

Cl ..........

ALA.-. - 

Fe203 ....... 

FeO ........

MnO........

BaO- .......

CaO ........

MgO........

K20 ........

Wn»,O

B.

.82

52.27

1.49

trace. 

17.08

2.51 

5.00

.23

.06

8.39

6.05

1.58

4.19

100. 27

C.

.64

.58

51.57

1.43

17.72

0.24 

1.78

.45

.16

8.82

4.91

1.09

3.59

99.88

D.

1.29

.37

52. 37

1.00

trace. 

17.01

1.44 

5.89

.32

.06

7.59

6.86

1.59

3.51

99.90

E.

.53

52.38

1.22

f;fi

18.79

2.88 

4.90

.18

.11

7.70

4.91

.1.76

3.99

99.91

LAVAS FROM NEAR LASSEN PEAK, CALIFORNIA.

(Series collected b,v J. S. Diller.]

1. West end of Lake Bidwell.

2. Silver Lake.

3. Volcanic sand, half-mile northeast of Cinder Cone, 10 miles northeast of Lasseu Peak.

4. Inclusion in lava of Cinder Cone.

5. Lava of volcanic bomb, from Cinder Cone6. One-third of a mile south of Cinder Cone, on border of lava field.

7. Lapilli from Cinder Cone.
156 WASHINGTON LABORATORY. [HULL. (30.

8. Timber line, west base of Lassen Peak.

9. Lava enveloping No. 8.

10. East end of Chaos, northwest base of Lassen Peak.

11. East end of Chaos, northwest base of Lassen Peak.

12.. Two miles south of Luffan's Mountain, Liana County.

13. Two miles south of Luffan's Mountain, Liana County.

14. Northwest base of Luffan's Mountain, at base of high cliffs near 

Lassen Peak.

15. West side of old crater near Thumb, head of Mill Creek.

16. One mile southwest of Thumb, at head of Bailey Creek.

17. Lava resting on dacite, near west base of Lassen Peak.

18. One and one-half miles northeast of Clipper Mills, on tramway to 

Eock Creek, Shasta County.

19. West summit of Crater Mountain.

20. North slope of Crater Mountain.

21. Nodule from No. 20.

22. Near eastern end of rim, Crater Mountain.

23. South base of Burney Butte.

24. Cone at south base of Burney Butte.

25. Northwest summit in rim about the head of Burney Creek.

[Analysis 1 to 21 by W. F. Hillebrand; 22 to 25 by "R. B. Riggs.]

H20 ........

SiOz ........

Ti02 . .......

T> f\

ALA». ......

CrA -------

Fe203 ...... 

FoO ........

MnO. .......

BaO .. .....

SrO- ........

CaO ........

MgO. .......

K20 ........

NazO .......

Li2O. .......

No. 1.

.42

50.18

16. 59

1.51 

5.51

undet.

(?)

(?)

7.64

7.26

1.47

3.58

(?)

100. 16

No. 2.

.86

57.59

16.49

1.22 

4.89

(?)

(?)

7.40

7.72

.99

3.62

(?)

100. 78

No. 3.

.26

55.93

17.34

1.50 

5.20

undet.

(?)

(?)

8.04

.7.29

1.35

3.32

(?)

100. 23

No. 4.

.68

79.49

11.60

.33 

.49

.none.

(?)

(?)

1.64

.09

1.52

4.04

(?)

99.88

No. 5.

.30

56.70

.65

.20

15.75

1.29 

5.32

.19

.03

7.67

7.16

1.56

3.36

100. 18

No. 6.

.28

j 54.56

.53

.18

16.04

.95 

6.07

.17

.03

8.89

8.71

1.18

3.05

100. 64

No. 7.

.27

56.53

.54

.15

17.50

1.35 

5.03

.12

(?)

8.07

5.94

1.55

3.51

100. 56

No. 8..

.91

55.14

.52

.18

19.10

6.16 

.54

.11

.07

8.36

4.23

1.04

3.71

100. 07
1UGG8.] MISCELLANEOUS ANALYSES. 157

H.,0 ........

Si03 ........

TiO-i. .......

Pa06 - -- ---.

A1A------- 

Ci-iA.- - 

ro»o........

FoO ........

MuO........

BaO ........

SiO>... ......

CaO ........

MgO. .......

K20 ........

Na20....--.

LisO ........

No. !).

1.37

08.32

' .12

If). 26

1. 00

1.26

.07

a. 20

1.32

2.81

4.27

100. 07

No. 10.

.74

08.72

.31

.09

15. 15

1.10

1.70

.11

.07

.03

3.30

1.28

2.78

4.26

09.76

No. 11.

.77

K'j qc

.50

.10

.19. 22

3.28

 4.48

.15

(?)

.03

9.76

4.80

99

2.89 i

100. 44

No. 12.

.55

63.47

 trj

.13

16. 75 

trace?

2. 15

2. 75

.04

.04

5.72

1.02

3.94

100. 60

No. 13.

1.09

57. 04

.47

.08

19.11

4.37

2.48

1 9

.02

7.34

3 04

1.1.6.

3.48

100. 70

No. 14.

1.09

58.08

.16

18.37

2.92

3.38

TO

.03

.02

7.05

<* 'V,

1.33

3.CC

100. 01

No. 15.

1.03

63.81

.38

.10

17. 07

2.11

2. 15

.09

.04

.03

4.97

2.28

i.no

4. 08

100. 10

No. 16.

1.04

59.84

.19

16.81

1.88

3.00

.14

.07

.02

0. 30

2.13

3.03

100. 07

H2 0. .......

SKV........

Ti02 ........

P206 . ...... 

SOS . ........

AiA--...

Cr-A -------

Fo,A-------

FeO .......

MnO. .......

BaO ........

SrO. ........

CaO ........

MgO........

K2O ........

Na,0. ......

Li20. .......

i

No. 17.

.69

56.51

.48

.14

18.10

A. 5>fi

2.68

.11

.04

.04

8.15

4.52

1.15

3.23

trace.

100. 10

No. 18

.85

74.60

.16

.03

13.41

1.28

.30

.06

.11

1.08

.20

4.50

3.38

trace.

100. 02

No. 19.

.40

08.12

.25

.14

10.24

1 9f!

2.08

.10

no

09

" 80

1.35

2.54

3.89

trace.

100. 28

No. 20.

.83

61.17

.45

.14

17.74

1 78

3.51

.12

.06

.04

5.90

2.76

1.71

3.79

trace.

100. 00

No. 21.

.45

53. 85

f;n

.05

18.53

1.96

5.30

.12

<M

.01

9. 60

5.88

.74

2.98

trace.

100. 09

No. 22.

1.47

52.95

.66

trace.

18.25

4. 30

4.19

.12

.01

8.73

4.93

.77

3.57

(?)

100. 01

No. 23.

1.02

62.44

01

.05

16.39

4.60

1.00

.03

6 99

2.65

2.25

3.10

trace.

100. 18

No. 24.

.79

52. 63

.07

.47

17. 62

0.49

3.10

.04

8.62

5.64

1.73

3.38

trace.

100. 58

No. 25.

.00

60.04

.49

.04

17.43

5 on

KO

flft

.04

(?)

6.65

3.51

1.24

4.15

trace.

100. 49
158 WASHINGTON LABORATORY. (HULL. 60.

BASALT, ISLAND OF MYT1LENE. ASIA MINOR.

[Collected by J. S. Diller; analyzed by T. M. Chatard.] 

H30........................................................ 2.12

COs......................................................... 2.32

Si02 ._..................... ................................ 56.58

Ti08 ........................................................ .77

P20fi .. ...................................................... .15

AlaOa ....................................................... 14.88

Cr203 ....................................................... trace?

FesOs....................................................... 2.31

FeO ........................................................ 3.04

MnO.......... .............................................. .16

CaO........................................................ 8.69

BaO........................... ............................ .07

MgO........................................................ 3.76

K20 ........................................................ 2.18

Na20 ....................................................... 3.36

100.39

INCLUSION IN DIORITE FROM CRUGER'S STATION, NEAR PEEKSKILL,

NEW YORK.

[Collected by G. H. Williams; analyzed by T. M. Cbatard.] 

H20 ........................................................ 4.61

Si02 ........................................................ 32.73

AlaO3 ......................... ............................. 46.58

FeO ........................................................ 5.12

CaO........................................................ 11.04

MgO........................................................ 1.00

101.08

Analysis made on only 0.4212 gramme. The mineral is margarite.

WHITE EARTH FROM TALLADEGA, ALA.

[Received from R. A. Moseley, jr.; analyzed by C. Catlett. 

Ignition ................ ...... .............................. 1.94

Si02 ........................................................ 88.92

AJaOa................................ .... ................... 7.47

Fe203....................................................... trace.

CaO........................................................ .18

MgO ....................................................... trace.

Alkaliea.................................................... undet.

98.51

SANDSTONE, BEREA, OHIO.

[Extensively quarried;, analyzed by L. G. Eakins.]

HSO ........................................................ 1.19

Si62 ........................................................ 92.91

AlaOs.................. .................... ........... 3.78

Fe2Os....................................................... trace.

FeO....... ................................................. .91

CaO........................................................ .31

MgO ....................................................... trace.

KaO........................................................ .61

..................................................... .34

100.05
WHITFiELD.J MISCELLANEOUS ANALYESS. 159

KNOX DOLOMITE AND RESIDUAL CLAY.

[From Morrisville, Ala.; collected by I. C. Kussell; analyzed by W. F. Hillebrand. |

Dolomite. Clay.

SiOz .............. 3.24 55.42

. 17 22.17

. 17 8. 30 

FeO .......... ... .06 trace.

CaO .............. 29.58 .15

MgO.............. 20.84 1.45

K20 .............. .......... 2.32

.17 

H20 .............. .30 9.80

45.54

99.90 99.84

Of the water in the clay 2.10 per cent, was expelled at 100°.

DOLOMITE FROM TUCKAHOE, WESTCHESTER COUNTY, N. Y.

The so-called " Tuckahoe marble." Extensively used as a building 

stone. White, highly crystalline.

f Analysis by W. F. Hillebrand.]

Insoluble ................................................... 1.33

H20 ........................................................ .16

Fe203 -.............^........................................ .21

CaO.............................. .......................... 30.68

MgO........................................................ 20.71

C02 ........................................... .............. 46.66

99.75

Of the insoluble portion, 0.71 is silica. The iron is probably in part 

Fe.O.

WHITE DOLOMITE MARBLE, COCKEYSVILLE, MD.

[Analysis by -J. E. "Whitfield.] 

Si08 ........................................................ .44

A* 9Q3 .................. --- .............--..-... --... -... 1.22

FeO ........................................................ trace. .

CaO........................................................ 30.73

MgO....... .................................................. 20.87

C02......................................................... 45.85

Ignition .................................................... 1.22

100.33
160 WASHINGTON LABORATORY. [BULL 00.

MARBLE FROM LOUISIANA.

From sections 19 and 20, T. 11 K, E. 3 W., five miles west of Winnfield. White, abundantly streaked with black. Eeceived from the 

Supervising Architect of the Treasury.

[Analyzed by W. F. Hillebraml.l

Insoluble .............................................. .65

H8O........................................................ .13

CaO................ ........................................ 55.01

MgO........................................................ .60

MnO.... ..................................................... .10

CO* .... .................................................... 43.43

S03 ..~. ................................................... .27

100.19

Traces of A12O3 , FeO, BaO, SrO, 01, and organic matter.

LIMESTONES FROM OHIO AND INDIANA.

Trenton limestoues and Utica shales, collected by Professor Edward 

Orton in the course of an investigation of the oil and gas wells of the 

two States. Partial analyses, as called for.

A. From New Vienna, Ohio. Analyses by F. W. Olarke and E. B. 

Eiggs, jointly. 1, 2, 3, Utica shales. 4, 5, 6, 7, Trenton limestones.

co2 . ........

CaO ........

MgO .......

Insoluble . . .

No. l.

15.24

17. 11

1.25

60. 17

93.77

No. 2.

27.16

33.43

2.16

29.51

92.26

No. 3.

27.40

35. 27

1.32

25.80

89.79

No. 4.

36.20

46.16

1.52

8.47

92.35

No. 5.

37. C4

49.04

.58

9.93

97.19

No. 6.

42. 04

51.18

3.08

2.12

98.42

No. 7.

30.82

23.00

12.90

28.43

95.15

Iron and alumina present in the soluble portions.

B. Trenton limestones from Ohio. Analyses by Clarke and Eiggs. 

8, Arcadia, Hancock County; 9, Air-line Junction, Toledo j 10, gas 

rock, St. Henry's well, Mercer County; 11, oil-rock, Lima. .

C02 . ........

CaO ........

MgO........

Insoluble - . .

No. 8.

38.54

47.17

2.59

8.56

96.86

No. 9.

42.84

30.64

J8.05

3.52

95.03

No. 10.

40.96

50.34

2.86

2.27

96.43

No. 11.

43.92

32.24

17.36

1.64

95. 16

Iron and alumina present in the soluble portions.
CLAKKK.] MISCELLANEOUS ANALYSES. 161

C. Seven Trenton limestones from Ohio. Analyzed by F. W. Clarke. 

12, well No. 3, Bryan, gas rock; 13, McElree well, Kenton; 14, Huntsviile; 15, Prospect; 16, Findlay street well, Dayton; 17, Xeuia; 18, 

New Madison. Air-dried samples.

Insoluble . . .

FoaOa.AL.Ai.

CaC03 ......

MgOO,...-.

No. 12.

9.22

1.51

49.00

38.59

98.32

No. 13.

5.20

1.10

84.32

8.43

99.11

No. 14.

4.41

3.15

57.23

33.16

97.95

No. 15.

26.12

2.57

3.77

98.48

No. 10.

12.34

.58

82.36

1.67

90. 95

No. 17.

9.23

.18

8G.54

2.99

98. 94

No. 18.

11.11

3.60

64 91

17.98

97.00

In 14 and 18 ferrous carbonate was present.

D. Seventeen Trenton limestones from Ohio. Analyses by 0. Catlett. 19, Air-line Junction, Toledo, depth 1,415 feet; 20, Upper Sandusky, city well No. 2; 21, Sandusky, depth 2,260 feet; 22, St. Mary's 

township, Auglaize County, gas-rock, Pauck well; 23, same locality, 

gas-rock, Bennett well; 24, Carey, first city well, depth about 1,350 feet; 

25, Fort Recovery well No. 2, depth 1,065 feet; 26, Loomis and Nyman 

well, Tiffin, depth 1,470 to 1,481 feet; 27, Loomis and Nyman well, 

Tiffin, 1,488 to 1,494 feet; 28, gas-rock, Waggoner well, 6 miles west of 

Fremorit; 29, London, depth 1,594 feet; 30, Celina, depth 1,112 feet; 

31, Port Clinton, 1,660 to 1,700 feet; 32, Wauseon, 2,135 feet; 33, 

Napoleon, 1,830 feet; 34, oil rock, Kossutb, Alien County ; 35, Franklin Township, Mercer County; Doenze's well, 1,107 feet.

Fc203 ,Al203 -

CaCOs-.-..--

MgC03 ......

Insoluble ...

Fe203 ,Al a03 .

CaC03 ......

MgCOs .....

No. 27.

9.88

1.46

79.39

0.20

96.93

No. 19.

2.88

8.68

54. 68

25. 73

91.97

No. 28.

5.22

0.32

52.93

32. 75

!)7. 22

No. 20.

8.18

4.31

64.25

15. 93

92. 07

No. 2&.

15.90

1.84

77.69

1.89

97.32

No. 21.

3.65

4. 58

54.02

33.07

90. 52

No. 30.

2,95

2.95

08.41

24.18

98.49

No. 22.

3.18

3.12

52.18

38.42

90.90

No. 31.

7.46

4.10

71.90

14.34

97.92

No. 23.

1.60

2.48

50.94

35. 55

90.03

No. 32.

18.24

7.28

42. 82

28.11

90.45

No. 24.

5.72

3.08

80.11

8.09

97.00

No. 33.

2.66

2.14

53.85

37.33

95.98

No. 25.

1.89

1.57

87.88

7.43

98.77

No. 34.

1.08

.60

90.72

6.09

99.15

No. 26.

5.60

4.80

52.80

33.40

!I6. 87

No. 35.

3.68

8.38

69.53

10.68

92.27

Bull. 60 11
162 WASHINGTON LABORATORY. [BULL. CO.

B. Six Trenton limestones from Indiana. 1, Union City, 1,160 feet 5 

2, Bluffton, 1,062 to 1,067 feet; 3, Muncie, 920 feet; 4, Greensburg, 

867 feet; 5, Vernon, 905 feet; 6, Wabash, about 900 feet.

I Analyses, 1, by F. W. Clarke; 2, 3, 4, 5, 6, by C. Catlett.]

Insoluble . . .

Fe203 ,Al203 .

CaC03 ......

MgCO, .....

No. 1.

2.14

1.23

83.21

12.48

99.06

No. 2.

2.37

4.48

53.43

37.47

97.75

No. 3.

3.30

3.72

51.96

38. 31

97. 09

No. 4.

.87

.55

94.00

.36

96.38

No. 5.

8.00

.60

85.56

trace.

94.16

No. 6.

3.52

7.58

53.18

30.53

94.81

COQUINA, COEAL, CORAL EOCKS, ETC.

Collected by Professor N. S. Snaler in an investigation of coral reefs. 

Partial analyses, as called for.

A. Five coquina gravels from Florida; 1,2,3,4,Tortugas; 5, Key 

West; samples air-dried.

[Analyses by F. "VV. Clarko.]

C02 ...... .........

Si02 ..............

Al203 ,Fe203 ....... 

CaO ..............

MgO...... ........

No. 1.

3.27

41.46

.19

.19

52.24

1.53

98.88

No. 2.

3.57

41.07

.22

.47 

51.24

2.09

98.66

No. 3.

5.12

40.39

.32

.56 

49.38

1.93

97.70

No. 4.

3.07

41.53

.21

.76 

51.95

1.44

98.96

No. 5.

3.19

41.58

.25

.56

51.52

2.08

99.18

Chlorides and sulphates present; phosphates not looked for.

B. Five coral and shell rocks from Florida; 6, near Fort Worth ; 7, 

east side of St. John's River, near Seville; 8, corroded surface, Miami 

Reef; 9, near Oak Hill; 10, near Melborne.

[Analyses by F. "W. Clarke.]

co2 ...... .........

Si02 ..............

Al2O3 ,Fe203 .......

CaO ..............

MgO..............

No. 6.

2.64

41.59

2.94

.23

51.51

.71

99.02

No. 7.

3.37

39.00

8.50

.73

47.29

1.51

100. 40

No. 8.

2.33

41.22

2.99

.65

51.22

.00

98.37

No. 9.

3.21

39.62

5.87

.95

50.34

.37

100. 36

No. 10.

2.53

34.31

17.83

1.18

43.85

.20

99.96
EAKINS.J MISCELLANEOUS ANALYSES. 163

C. Three coquinas from Florida; 11, coarse shell mass, Senote; 12, 

Salt Key Bank, coral rock; 13, Loggerhead Key.

[Analyses by L. G. Eakins.]

H80 ...............

C02 ............

CaO ..............

MgO...... ........

No. 11.

.11

43.89

.22

.18

54.87

.64

99.91

No. 12.

1.13

43.87

.11

.04

53.54

.71

99.40

'No. 13.

.81

43.71

.20

.22

53.54

.78

99.26

D. Hammock clay, Melborne Creek, Florida.

E. Incrustation formed by evaporating waters, Everglades, Florida. 

F. Ochreous deposit, Paint Eock, Dade County, Fla.

[Analyses by L. G. Eakins-l

H20 ..................

co8 . ..................

Si02 ..................

AlgOj.- ..-..-....

Fe203 -. ...............

FeO ..................

MnO...... ............

Pif»

MgO..................

Alkalies...... ........

D.

1 23. 61

38. 04

I 27. 19

10.73

'.40

undet. 

100. 03

E.

19.50

25.38

19.68

1.59

( ,u

31.32

.30

undot. 

98.94

IT.

.31

J41.30

1.32

^n

7.26

.68

48.96

'.41

100. 54

G. Phosphatic deposit, Island of Sombrero, West Indies.

H. Coralline bottom, Barbados.

I. Itecent coral (Siderostria), Bermuda.

[Analyses by L. G. Eakius.]

H20 ........

COj. ........ 

Cl ..........

P206 . ....... 

Si02 ........

A1203 .......

CaO ........

MgO........

G.

3. Of)

3.47 

.66

39.12 

.14

90

51. 15

97.88

H.

2

7O

4!t. 40

1.17

11

40. 45

99. 21

I.

.51

43.74

OO

55.16

99.87

Alkalies not looked for.
164 WASHINGTON LABORATORY. [HULL. 60.

J. Fourteen coral rocks and one soil from the Hawaiian Islands. 

Analyzed by L. G-. Eakius. 1, Laie; 2, 3, Kohuku Bluff; 4, Kohuku 

coral flat; 5, point near coral flat; 6, modern chalk, Oahu; 7, Diamond 

Head; 8, under lava, Honolulu; 9, near Pearl Kiver lagoon; 10, old 

reef,Waialua; 11, Cam pbell's Ranch quarry, Waianea,Oahu; 12,Wailuku 

Bay; 13, Reef Three, Honolulu; 14, Prison Knoll, Honolulu; 15, Lava 

soil, Diamond Head.

[Analyses Ly L. G-. Eakins.l

H20. ..........

COj. ..........

SiO2 ..........

ALA. .........

re2o3 ..--.....

CaO ..........

MgO. .........

H20 ..........

CO,.. .........

T> n

Cl ............

SiO, ..........

A1203 - ....... -

Fe203 ... .....

MnO. .........

CaO...........

MgO..........

Alkalies......

No. 8.

1.61

38.71

5.34

| 5.11

42.24

5.95

98.90

No. 1.

4.74

41.89

.35

| . 

49.38

1.74

98.29

No. 9.

10. 84

46.22

19.10

12.94

1.72

2.24

99.12

No. 2.

.40

44. 83

.19

I .52

49.34

4.00

99.38

No. 10.

1.33

42.68

1.05

| 1.20

51.07

.11

97.50

No. 3.

.79

43.64

.07

| .»

51.09

2.50

99.42

No. 11.

.40

43.96

.53

] .02

50.69

2.98

99.24

No. 4.

.93

. 43. 89

.25

| .49

53. 34

.67

99.57

No. 12.

1.93

42.80

.45

[ 1.82

50.54

1.83

99.37

No. 5.

.70

43.95

.26

! -«

52.17

1.51

98.80

No. 13.

2.75

40.59

| 2.26

46.52

2.45

98.10

No. 6.

9.84

11.09

qo ot;

19.53

10.71

11.37

3.00

98.85

No. 14.

1.24

42.81

.81

j 1.19

52.67

.42

59.14

No. 7.

1.86

40.81

2.97

£ 2.88

44.82

5.32

98.66

No. 15.

5.30

11. 41

.24

91

32.88

19/19

n

KO

12.20

11.70

undet.

98.18

IEON AND MANGANESE OEES.

Two iron ores and two ochres from the Lucas farm, Jefferson County, 

W. Va. Eeceived from D. B. Lucas.

[Analyzed by C. Catlett.]

Si02 -....-..

Fe..........

Mn, ........

P...........

S. ..........

Ore.

A.

1.18

58.72 

none. 

.075 

.293

B.

4.03 

59.31 

none, 

trace, 

trace.

: r i .

Oclire.

C.

92.07 

2.72 

undet. 

undet. 

undet.

D.

93.57 

2.24 

nnclet. 

undet. 

uudet.
WHITl'IEU). MISCELLANEOUS ANALYSES. 165

Iron ore, Little's ore bank, Jefferson County, W. Va., and Hostler's 

ore bank, same county. From D. B. Lucas.

| Examined by C. Catlett.]

Little's. Hostler's.

Si02 ........ 55.67 67.34

Fe.......... 23.21 22.73

Also from D. B. Lucas, iron ore from Cool Spring ore bank, Clarke 

County, Va., and from Bear Pond, top of Blue Ridge, Va.

[Analyses by C. Catlott.] 

Cool Spring.

29. 63 7. .1.1

Fe.......... 30.50 48.24

Mn......... trace. 1.625

P........... .175 .941

S........... .232' .150

Three manganese ores, from Blkton, Rockiugham County, Va. Received from C. E. Creecy. .

[Analyzed by C. Catlott. 1

A. B. C.

Mn ......... 43.94 49. 66 48. 75

Si02 ........ 15.88 1.80 15.08

Fo.......... 3.43 8.53 2.79

P........... .160 .070 .085

S........... .07 .089 trace.

Four iron and manganese ores, Stuart estate, Lick Mountain, near 

Wytheville, Va. From J. W. Reardin.

[Analyses by J. E. Whitfiold.]

A. 15. C. D.

Fo................ 2.92 2.57 1.98 48.988

Mn ............... 51.05 41.89 57.67 4.54

P................. .161 .035 .009 .394

S ................. trace. .09 .067 .056

Insoluble......... 4.32 4.05 l.«5 10.34
166 WASHINGTON LABORATORY. [HULL. CO.

Also three ores from the same estate, sent in by P. B. Thompson, jr. 

Same analyst.

Fe...... ..........

Mn. ..............

P.................

S...... ...........

A.

34.05

4.93

.118

.083

34.59

B.

38.01

15.23

.05

.088

9.31

C.

3.96

44.60

0.45

15.81

Ores collected by Prof. J. E. Procter. Analyses partly by J. EWhitfield, partly by C. Catlett.

A. From Scott County, Va.: 1, Anderson lands, near top of Clinch 

Mountain, southern slope, 1,150 feet above the railroad water-tank;

2. James Boatwright's land, east side of Stony Creek, Buffalo Eidge;

3. Clinch Eiver Hills, land of J. C. Taylor's heirs, north side of the 

river, 3£ miles above Stock Creek; 4, Slip Hill ore, where North Fork 

of Clinch Eiver cuts through Purchase Eidge.

[Analyses 1, Catlott; 2, 3,4, Whitfield.]

Fe...... ..........

Mn...............

P.................

S.................

Insoluble .........

No. 1.

51. 98

4. CO

1.406

.086

2.07

. No. 2.

47.22

.093

.119

25. 50

No. 3.

49.79

.205

.008

17. 332

No. 4.

11.543

.275

.08

59. 306

B. From Wise County, Va.: 1, 2, 3, Big Stone Gap, top, middle, and 

bottom layers; 4, 1£ miles from Big Stone Gap ; 5, lauds of Virginia 

Coal and Iron Company. All the deposits are on the south slope of 

Wallen's Eidge.

[Analyses by Whitfield.]

Fe... .........

Mn...........

P.............

S .............

Insoluble .....

1, top.

6.65

.30

.096

.136

80.38

2, iiiiilille.

49.44

.015

.132

21. 75

3, bottom.

49.44

.122

.135

^ 24.52

4.

39.70

.47

.200

.085

36.64

5.

52.00

.165

.08

11.17

C. From Lee County, Va.: 1, A. J. Ely's land, north slope of Poor 

Valley Eidge, near Pennington Gap; 2. land of W. M. Pennington, 

near Pennington Gap.

[Whitfield, analyst.]

Fe.... ..........

Mn .............

P ...............

s...... .........

No. 1.

52.82

.124

.115

17.92

No. 2.

20.76

.33

.079

04. 43
CATLETT.] MISCELLANEOUS ANALYSES. 167

D. Iron ore, three miles east of Pineville, on north slope of Pine 

Mountain, Bell county, Ky.

[Analysis by Oatlott.l

Fe..

Mn

P...

S... 

Si02

43.32

1.27

.120

,.342

13.48

E. Supposed iron ore, one-half mile west of top of Flint Hill, two 

and one-half miles from North Carolina line, on the waters of Elk, 

Carter County, Teiin.

[Whitfield, analyst.] 

Insoluble ......-.-..........-.............., <,............. 88.48

Fe..............--..:..-.................................... 5.83

Mn ........................................................ 1.35

P.................................................... ...... .043

S.......................................................... .039

F. Iron ores from Claiborne County, Tenn.: 1, outcrops 100 yards 

east of the Russell shaft, four miles southwest of Cumberland Gap; 2, 

Oty shaft, east end of Double Mountain, one and one half miles west 

of Cumberland Mountain; 3, Van shaft, southern slope of Double 

Mountain, one-half mile west of Gap Creek, two and one-half miles 

southwest of Cumberland Gap; 4, red fossil ore, three miles east of Big 

Creek Gap, southern slope of Cumberland Mountain; 5, red fossil ore, 

200 yards east of Big Creek, 175 feet above creek, on southern slope of 

mountain, Big Creek Gap.

[Analyses by Catlott.]

Si02 ...... 

Fo. .......

Mn....... 

P.........

S. ........

No.l.

4.28 

55. 16

.09 

.910

.162

No. 2.

7.43 

54. 94

.30 

.124

.087

'No. 3.

19. 79 

44.71

trace. 

.108

.269

No. 4.

6.70 

54. 54

.43 

.72

.214

No. 5.

5.66 

53. 83

.53 

.243

.187

G. Ores from Unicoi County, Tenu.: 1, Garland land, on ridge 

between Rock and Martin's Creeks; 2, land of W. and M. Peebles, 

northern slope of Little Iron Mountain, near top of spur; 3, northwest 

spur of Unaka Mountains, one and one-half miles south of Irwin; 4, 

old mine on the Farnum laud, at base of hill opposite mouth of Sciatha 

Creek; 5, divide between the waters of Rock and Dix Creeks, Hann 

tract; 6, Bell lauds, on ridge west of Rock Creek, one and one-half 

miles east of Irwin, 700 feet above Irwin; 7, laud of W. F. Norris,six 

miles from Johnson City, three-fourths of a mile southeast of Buffalo 

Creek; 8, west end of Little Iron Mountain, about one mile west of
168 [DULL. 60.

mill, near top of hill; 9, one-fourth mile southeast from Blue Spring, on 

waters of Indian Creek.

[Analyses by "Whitfleld. 1

Fe....:..

Mn......

P........

S .........

Insoluble.

No. 1.

46.41

3.47

.741

.077

5.06

No. 2.

54.69

trace.

1.102

none.

0.51

'No. 3. No. 4.

2.70

44.94

.282

none.

3.14

23.55

32.98

.551

none.

5.11

No. 5.

41.63

12.13

1.237

.057

3.85

No. 6.

56. 32

trace.

1.432

.059

3.32

[Analyses by Catlett.]

No. 7. No. 8. No. 9.

Fe.......... 2.04 40.37 51.40

Mu ......... 39.37 .38 3.01

P........... .116 .509 .761

S........... trace. .106 .092

SOa......... 18.10 3.77 6.26

Iron ore, Cranberry Bed, Mitchell County, N". C.

[Analysis by Wliitfleld.] 

Fe.......................................................... 51.65

Mn ............................................ ........... .36

P...................--......--..----..---.-....-........... trace.

S.......................................................... .081

Insoluble .................................................. 19.95

Ti02, Ni..................................................... traces.

Ores collected by L. C. Johnson in Louisiana: 1, Miller's Bluff, Bossier Parish; 2, Aubrey, Claibome Parish; 3, Gilmer field, Phelps Lake, 

Bossier Parish.

[Analyses by Catlett.]

No. 1. No. 2. No. 3.

Fe.......... 38.35 43.17 49.97

P........... .18 1.65 .62

S........... .34 .050 .08

Insoluble... 21.40 11.42 12.15

Ores from Arkansas, received from Hon. W. C. Whitthorne, from a 

mountain ridge crossing the line between Polk and Montgomery 

Counties, between the two Salinas Creeks: A, manganese; B, iron ore.

[Analyses by C. Catlett. 1

Si02 

Mn 

Fe.. 

S ... 

P...

A.

4.64

38. 33

18.68

.170

.561

.94

1.32

54.30

.162

1.826
CA'IT.ETT.] MISCELLANEOUS ANALYSES. 169

Iron ore from Wood County, Wisconsin. Section 32, T. 24, B. 4 E. 

Eeceivecl from T. E. Nash.

[Analyzed by J. E. "Wbitfiold.] 

Fe......................................................... 22.15

Mn.......................................................... trace.

S.......................................................... .008

P..........'................................................ .030

Insoluble ........................................ .......... 57.70

Manganese ore (impure rhodochrosite), from Llanbedr, Harlech, 

Merionethshire, Wales. Analyzed by T. M. Chatard, at request of Dr. 

D. T. Day, for purposes of comparison with certain American material.

CO3 ......................................................... 19.04

Mn ......................................................... 31.12

A1A....................................................... 7.63

Fe .......................................................... 4.02

Si02 ....................................................... 21.69

COAL AND COKE.

Two samples of coke from near Piedmont, W. Va. Received from 

G. W. Harrison.

[Analyses by C. Catlett.J

Thomas mine. Davis mine.

Moisture ........... .47 .25

Volatile carbon..... 2.39 2.24

Fixed carbon ....... 87.14 89.23

Ash ................ 10.00 8.28

100.00 100.00 

S ................... .721 .645

Two samples of coal from near Piedmont, W. Ya. Eeceived from 

Hon. H. G. Davis.

[Analyses by C. Catlett.]

^vis unne.

Moisture ........... .70 .70

Volatile carbon..... 19.39 22.03

Fixed carbon....... 72.9D 70.53

Ash ................ 6.8C 6.74

100. 00 100. 00 

S ................... .880 .924

Ash white, coke silver gray and porous.
170 WASHINGTON LABORATORY. [BULL. 60.

Supposed anthracite from near Eomney, W. Va. Received from A. 

W. Kercheval. A shale.

[Analyzed by C. Catlett.l 

Moisture.................................................... .68

Volatile carbon ............................................. 7.32

Fixed carbon................................................ 5. 37

Ash......................................................... 86.63

Three samples coal, Sharp bank, East Fork of Big Creek, Claiborne 

County, Tenn. Eeceived from J. E. Procter.

[Analyzed by C. Catlett.]

Top. Middle. Bottom.

Moisture ........... 2.40 2.10 1.78

'Volatile carbon..... 1 36.81 33.7G 39.14

.Fixed carbon ....... I 57. 88 51. 29 56. 00

Ash ................ 2.91 12.85 3.08

100.00 100.00 100.00 

S ................... 1.087 1.15 2.30

Coke hard to burn;- dark in color; ash brown.

Coal from Pend d'Oreille, Oregon. From Hon. J. K. Jones.

[Analysis by C. Catlett.] 

Moisture .................................................... 7.56

Volatile carbon.............................................. 52.55

Fixed carbon ............................................... 30. 43

Ash......................................................... 9.46

100. 00 

S........................................................... .65

EFFLORESCENCE ON SANDSTONE, FROM CLIFF ORBEK, GUNNISON

COUNTY, COLO.

[Collected by "Whitman Cross; analyzed by L. G. Eakins.]

A12 03 ......... trace. Si02 .......... 55.09

CaO .......... trace. A1203 ......... 9.75

MgO.......... 5.42 Fe203 ......... 1.23

S03 ............ 10.31 CaO .......... .30

MgO.......... .39

Alkalies...... undet.

15.73 66.76

 Water............................................. 16.88

Soluble............................................ 15.73

Insoluble.......................................... 66.76

9f».37

The soluble part is essentially MgSO4 , 7H2O.
CIUTAKL).] MISCELLANEOUS ANALYSES. 1.71

COMMON SALT, FROM HUTCHINSON, KANSAS.

[Received from Hou. P. B.'Plumb, analyzed by T. M. Chatard.l 

H20 ........................................1............... .92

Insoluble ................................................... .09

CaSO, ...................................................... 1.47

MgCl2 ...................................................... .25

NaCl ........................................................ 97.27

100.00

WATER FROM LINCOLN COUNTY, N. C.

Spring on the farm of Willis E. Hall, 3 miles from Lovvesville postoffice, and 20 miles from Charlotte.

[Analysis by F. W. Clarke. Stated in grammes per litre. Total solids, 0.042 gram.]

Si0.2 ..............

Cl. ................

S04 ...............

Cii................

!Na. ...............

K. ................

C03 , difference....

Found.

.0385

.0029

. 3329

. 15 U

.0094

. 0267

. 0022

.0780

.6420

Per cent, of 

total solids.

5.99

.45

51.86

23. 58

1.47

4.16

.34

12. 15

100. 00

Si02 ......................

CaS04 ....................

CaC03 . ...................

MgC03 . ..................

KCl.......................

NaCl .....................

Nu.,C03 . ..................

Hypothetical 

combination.

. 0385

.4716

.0318

.0328

.0042

. 0015

.0601

.0405

99.77 per cent, 

of total.

SURFACE DRAINAGE WATER, ST. AUGUSTINE. FLA.

[Collected by William Kennish; analyzed by T. M. Cliatard. Stated in grammes per liter.]

SiO-i .......... ...

Al203+Fe203 .....

Ca.... ............

Mg ...............

Na...... ...... ...

K... ..............

so4 ...... .........

Cl..... ............

C03 . ..............

Hiii bicarbonates.

Deficit of C03 .....

Found.

.014C

.0015

.0796

.0166

.0639

.0098

.0524

.1076

.OC42

.5952 

.0114

.6066

Per 

cent, of 

total 

solids.

2.40

.25

IP 19

2.74

10.53

1.01

8.64

17.74

40.40

.69

1.88

100. 00

SiOz- ...........

Fo203 .. ..:......

Ah03 .... .......

NaCl ...........

KCl ............

CaS04 ..........

CaHsC2O0 .......

MgHjCjO....".

Hypothetical 

combination.

.0146

| . 0015

.1625

fll ftfi

.0742

.2341

.1009

.0066
172 WASHINGTON LABORATORY.

WATER FROM SPRING AT M'LEANSBOROUGH, ILL. 

[lleceived from S. W. Heard; analyzed by R. B. Riggs. Stated in grammes per liter.]

so4 . ................

CO,.. .. ..........

01 ..................

Si02 ................

A1 203 . .............. 

Ca.......... ........

Mg..... ............

ATn

K. ..................

H, bicarbonate. . ....

Found.

3. 0040

.7008

.0345

.0142

trace. 

.5420 

.44158

.2888

.0115

5. 0426 

.0098

5. 0524

Per cent, of 

total solids.

59.59

13.90

.68

.28

10.75

8.86

1 73

.21

100. 00

KCL. .........

NaCl .........

NajSOi .......

 MgS04 . .......

CaS04 ........ 

CaC03 . ......

CaHaCjOu .....

Si02 ..........

Hypothetical 

combination.

.0220

fltQR

.8433

2 93<in

.9166 

1924

.7903

.0142

5. 0524

WATER FROM LEBANON, LACLEDE COUNTY, MO.

[From a well 1,000 feet deep. Received from Hon. R. P. Bland; analyzed by L. G. Eakins. Stated in

grammes per liter.]

SiO

A1203 - ..............

Fe...... ............

Ca.... ..............

Mg .................

Na...... ............

Cl ..................

H, bicarbonate ......

Found.

.0112

. 0032

.0320

.0163

.0127

.0048

.0034

.2872

Per cent, of 

total solids.

:(. 90

5.68

4.42

1.67

70.69

1.18

100.00

SiO

A1203 . ........

NaCl .........

MgS04 . .......

MgH2C206 .--.

CaH2C2Oc ...-.

NaHC03 ......

Hypothetical 

combination.

. 0112

nnoo

.0917

.1315

<M7n

.0066

.2872
MISCELLANEOUS ANALYSES. 173

TWO SPRINGS AT HOMINY HILL, ARK.

[Received from Hon. A. H. Garland. Analyses liy J. E. Whitfield. Stated in grammes per liter.] 

A. OLD OR UPPER SPRING.

Fo.Al..... ........

Br,I ....... ......

BA... . ..........

Cl ...............

S04. ..............

co3 ...... .........

Ca....... .........

Mg ...............

K...... ...........

Na...... ..........

Li ....... ........ 

NH4 -- ............

H, bicarbonate....

FreeCOz .........

Found.

.0122

none, 

none.

.0041

.1117

.0260

.0034

.0040

.0000

trace, 

none. 

.0019

.1693 

.0270

Per

cent, of 

total 

solids.

7.21

2.42

65.98

15. 3G

2.01

2.3C

3.54

i.12

100. 00

Si02 ............

CaH2C2Oo.--.-.- 

MgHjCA-.-... 

KHC03 . ........

NaHCOs........

Hypothetical 

combination.

.0122

.0984 

.0207 

. 0103

. 0219

.1093 

.0270

B. NEW OR LOWER SPRING.

SiOa ..............

Fo...... .......... 

Al.... ............ 

Ur,I,B203 ....--.:

ci.. ...............

S04. ..............

COs...............

Ca...... ..........

Mg ...............

K...... ...........

Na.... ............

Li ................

NH4 . ............. 

H, bicarbonate ....

FreeCOa..........

.0100

trace, 

none.

.0085

.0029

.0108

.0024

.0012

.0036

trace, 

none. 

.0010

.1064 

.0091

9.39

7.98

59.13

15.79

2.25

1.13

3.39

.94

100. 00

Si02 ............

CaSOa .......... 

CaHjCzOs....... 

MgHjCaO,,------

KHCOs. ........

NaHC03 -. ......

Free CO, .......

.0100

.0121 

.0535 

.0146

.0031

.0131

.1064 

.0091
174 WASHINGTON LABORATORY. I HULL. CO.

WATER FROM A SPRING- NEAR DENVER, COLO.

[Eeceived from Sidney Williams; analyzed by L. G. Eakins. Stated in grammes per kilo. Specific

gravity 1.063, at 20°.8.]

Si02 ..............

Cl ................

S04-..............

Al.Fe"...- ........

Ca. ...............

Mg. ..............

K. ................

Na. ...............

Li ................

co2 ...... .........

Album. NH3 ...... 

Free NH3 . ........

Found.

.0290

1. 5862

jq Qfi7K

.3214

7. 7461

.1331

6. 8006

trace.

60. 5839

.2101

.0050

Per

cent, of 

total 

solids.

.05

2.62

72.56

.53

12.79

.22

n

9*i

100. 00

KCL. ...........

NaCl ...........

NajS04 .........

MgS04 . .........

CaS04 ..........

Si02 ............

Hypothetical 

combination.

9<U9

2.4143

18. 0629

38. 7306

1. 0929

.0290

60. 5839

MATILIJA HOT SPRINGS, NEAR SAN BUENAVENTURA, CAL.

[Received from Dr. Stephen Bowers; analysis by R. B. Riggs. Stated in grammes per litei.]

Si02 ..............

Si03 ...... ........

r*}

so4 . ....... .......

CO,..........:....

Ca. ...............

Mg.. .............

Na

K. ................

Found.

.0088

.0412

.8768

.0169

.0579

.0650

.0034

.0325

1. 6481

Per

cent, of 

total 

solids.

r>9

2.51

1.02

3.51

3.94

.21

33.11

1.97

100. 00

KC1..... ........

NaCl ...........

MgCl2 ........ ..

MgS04 .... ......

CaS04 ..........

CaC03 ..........

CaSi03 .... ......

SiOj ............

Hypothetical 

combination.

flfiOO

1. 3876

.0068

flfl7Q

.0160

.0965

.0629

.0088

1. 6481