ABUNDANCE AND DISTRIBUTION OF CERTAIN

ELEMENTS IN SPHENE

by

EDWIN ROBERT ROSE

SUBMITTED IN PARTIAL FULFILLMENT

OF THE REQUIREMENTS FOR THE DEGREE OF MASTER OF WEc SCIENCE

~QjX~w 4

at the

MASSACEUSETTS INSTITUTE OF

TECHNOLOGY

August, 1959

Signature of Author t...... Departmenyof Geology and Gp6phytes, August 22, 1959

Certified by ... Thesis Supervisor

Accepted by -rre.06...... l Chairman, Departmental Cowmittee on Graduate Students ABTRACT

AfUNDANCE AND DISTRIBUTION OF C)RTAIN SLMTS IN SPHESN

by Edwin Robert Rose

Submitted to the Department of Geology and Geophysics August 24, 1959 in partial fulfillment of the requirementa for the degree of Master of Science

The trace element content of accessory aphene from granitio rocks was investigated to determine if genetic similarity between igneous rocks can be detected by such means. This study also supplies considerable data on the trace element contents of spheneso

Analyses were made using a grating spectrograph on a Wadsworth mount- ing. Quantitative determinations were made for iron, chromium, zirconium, neodymium, lanthanum, cerium, samarium, gadolinium, scandium, vanadium, yttrium and tungsten in twenty-Uthree samples from northeastern North Amer.- iea. Semi-quantitative estimates were made for aluminum and strontium whenever present.

A standard was prepared from one of the aphene samples. This standard was then used as a "measuring stick" in the determinations of the analysis elements in the remaining twenty-two samples. The original concentrations of the analysis elements in the standard was determined by use of the ad- dition procedure. In connection with the addition plots, use was made of a ratio of the intensity of each analysis element to either oalcium or titan- inm; usually calcium. This ratioing of intensities improved the addition plots in most cases, making it easier to determine the original conoentre- tions of the analysis elements in the standard. It is estimated that the error involved in some of the determinations may vary from about ten per- cent to perhaps as much as twenty percent. Different element s will have different errors.

It was found that lanthanum, cerium and neodymium were geohemically coherent as were samarium and gadolinium. Cerium and lanthanum showed an inverse relationship to yttrium. Samples highest in chromium seemed to be lowest in iron. Chromium, soandium and tungsten concentrations were low in all samples. Iron was always present in high coneentrations, averaging about 20,000 ppm. The remainder of the analysis elements with an oceasional exception were present in quantities less than one percent (10,000 ppm). Manganese, yttrium, and neodymium values generally fell in a range from 3500 to 6000 ppm, Gadolinium, samarium, lanthanum, erium, zireonium and vanadium values lie for the most part between 1000 and 3500 ppm. Eleven of the thirteen samples from New England showed signifisant similarity to one another. This group, containing most of the New Rngland samples, is distinctly different from the rest of the samples. Similarity between three samples from Ontario is noted, Analyses of two samples from Quebee also show a distinct relationship to each other. The results seem to indicate that trace element conteat of ephene can be useful in determining the fact of genetic relat ionships between igneous rock,

Thesis Supervisor: William H. Dennen Associate Professor of Geology C0oaNfTS

Aoknowledgments ...... 7

Introduction . .. . 0 ...... a . a . . . a a a . a a - a 8

Purpose . . . . * . * * a 8

Previous Work ...... 9

Selection of Analysis llements and Lines ...... 13

Spectrographic Preparation ...... 17

Sample Preparation ...... a . a . a . .. * a 17

mixing ...... 19

E71lectrodes . * ...... 19

Photographic Materials ...... a ...... * 20

Photometry ...... a 20

Spectrograph ...... 20

Aring Conditions .. o...... - 21

Sector ...... - 21

Sources of Error ...... 22

Analytical Procedure ...... 29

Method of Analysis ...... 29

Graphical Procedure ...... 31

Calibration Curves . 31

Addition Plots ...... 31

Working Curves ...... 36

Discussion of Results ...... 39

By 3lauent ...... 41

By Sa2ple ...... 55

Swary of Results and Conclusions ...... *O. 72

Recommendations for Tture Work...... 78

Bibliography ...... - .. . - 79 TAaM

Table

1 Analysis Lines used in Addition Procedure ...... 0 . 9

2, Sample Locality and Percent Contamination ...... Compounds of Analysis Element a used in

Addition Procedure ...... 0 . 0 0 . 9 30

4 Concentration of Analysis Alements in Samples . 0 .. 0 0 0 40

5 Ionic Radii of Certain Klements ...... 9 .. 0 . 9 73 6 Determinations of the Elements 'by

Various Analysts .. . * ...... S . 0 . 0 .. 77

FIGURES

Figure 3 Variation of Arcing Time with Sample Weight ......

Addition Plots for Fe 4383 A ...... 3 Addition Plots for Fe 4260 A ...

4 Map of Sample Localities ...... ** . ... .* GRAPES Graph 1 Concentration Plots for Iron, Manganese and Chromium .. . . 42

2 Concentration Plot for Zirconium . . . , ......

Concentration Plot ftor Vanadium . . . 45

Concentration Plot for Yttrium . .,...... 46

Concentration Plot for Cerium a nd Lanthanum ...... 47

Concentration Plot for Neodymiui ...... 4...... 49

Concentration Plot for Samarium ...... 51

Cone entrat ion Plot for GadoliniuM . . .52...... *

9 Concentration Plot for candium .. * * * . ... . 53

10 Concentration Plots for Samples 3011 and 3055 ...... 56

11 Concentration Plots f or Samples 3014, 3058 and 3071 . 58

12 Concentration Plots for Samples 3080 and 3139 . . 59

13 Concentration Plots for Samples 3051, 3080 and 3061 . 61

14 Concentration Plots for Samples 3082, 3063 and 3079 . 62

15 Concentration Plots for Sanmples 3081) 3082 and 3485 ... . 64

16 Concentration Plots for Samples 3069 and 3069 ...... 65

17 Concentration Plots for Samples 3084 and 3085 ...... 67

18 Conoentration Plot for Sample 2C93 ...... 68

19 Concentration Plot for Sample 3C13 .X ...... 69

20 Concentration Plot for Sanple 31 38~. .. .0 ~ . 70 ACKNOWLEDGMENTS

The author expresses his sincere gratitude and appreciation to Dr. William H. Dennen, thesis supervisor, for his suggestion of the thesis possibility and for continued suggestions and advice during the course of the entire thesis investigation. INTRODUCTION

Purpose The purpose of this thesis is to investigate the possibility that the trace element distributions and variation in sphene might be used as a means of establishing or recognizing genetic similarity or dissimilarity between granitic rocks. To date little trace element analysis of sphene has been done and thus little is known concerning the trace element con- tent of sphene. This investigation will furnish considerable data on the

abundance and distribution of certain trace elements in this mineral.

The usefulness of trace element distribution as a possible means to group and separate igneous rocks of similar and different histories is based on the assumption that elements present in trace quantities do not

effect the cooling of the magma. It is important that one choose elements accepted into the ephene structure that have varing concentrations in dif- ferent magnas and that this variation of original concentration be re- flected by the relative proportions of the same elements in the sphenes. Sphene was chosen as the analysis mineral for this investigation for two main reasons. First, considering its formula CaTi(Si0 4 )0, and the previous work done (to be covered later), it appeared that the mineral would furnish ample opportunity for substitution of trace elements in its structure. This is quite important since in an investigation of this type it is desirable to have detectable amounts of several trace elements present in order to establish some understanding of the significance of the results. It is impractical to attempt to make determinations of trace elements in a mineral which admits non-formulary constituents only in quantities below the detection limits of the method used# It is also useless to investigate a mineral which is, so to speak, a trash bin for a great number of elements which enter its structure without any selection, and in a great variety of concentrations.

A second reason for choosing sphene as the analysis mineral was the

availability of over twenty aphene samples separated from granitic rocks. These samplea were from rooks used in a program of radioactive age studies

in the M.I.T. Department of Geology and Geophysics. In connection with

this program, granitic rocks from northeastern North America were collected,

crushed, and ortain minerals of which sphene was one, were separated

(Hurley and Fairbairn, 1957). Of course, the fundamental consideration

behind this availability of sphene, is the widespread occurrence of sphene

as an accessory mineral in granitic rooks.

Previo s Work Review of the literature showed that little work has been done on the

trace element constituents and their quantities in sphenes.

Fersman (1926) reports analysis of a sphene from a nephelite syenite.

This analysis shows 1700 ppm of cerium and yttrium oxides and about 1200 ppm of iron oxides both ferrous and ferrio. Also reported are trace quan-

tities of magnesium, sodium and potassium. Another article by Forsman

(1937), though not seen by the author in supposed to include some data on

sphenes. Bray (1942), states "sphenes are notable for their high rare-

earth content, as well as high aluminum, iron, manganese, chromium and vanadium." The work which Bray did on the sphenes was qualitative and

thus one cannot estimate what "high" means. Bray himself points out that

this is a relative term for each element and what is high for one element may be low for another.

In a study of four sphenes, one of which was the rare-earth-rtch variety, keilhauite, Prince (1938) reports from about one to not quite four percent iron oxide. In each of the "normal" aphenes he also found about six percent aluminum oxide and several hundredths of a percent of nanganese oxide was reported in two of the sataplse. In the keilhauite variety, Prince reports 3.58 percent (35,800 ppm) for the total of cerium and yttrium oxides, about six percent ferrie oxide and over seven percent of aluminum oxide.

Bahmae (1946) reports quantative analyses of six sphenes, three from nephelite syenites on the Kola Peninsulb, one from a limestone, one from a gabbro, both of these from Finland and the sixth specimen from the Urals.

For the rare-earth group of elements he hs values reported for lanthanum, cerium, praseodymium, neodymium, samarium, gadolinium, dysprosium, erbium, ytterbium and yttrium oxides. Values for these oxides range from a trace to about 1200 ppm, with neodymium, lanthanum, cerium and yttrium running in quantities several times larger than the concentrations of 100 to 200 ppm for the other rare-earth oxides. Other elements determined in oxide form by Sahama include: tantalum, vanadium, aluminum, iron, ebromium, magnesium, zirconium, strontium, barium, manganese and niobium. Niobium oxide values vary from 300 ppm to over 15,000 ppm. Tantalum oxide values are 300 ppm or less. The values for vanadium oxide are of the order of about 800 ppm. Ferrous iron oxide values lie in the neighborhood of 2,000 ppm, zirconium oxide values average about 600 ppm, strontium varies highly, from 40 to 4,400 ppm, while barium oxide varies from 50 to 500 ppm.

Niobium, tantalum, vanadium, iron, zirconium, strontium and barium were found in all six samples. Values for aluminum oxide are reported for only three of the samples and very from 500 to about 4400 ppm. Chromium oxide values are reported for two samples with an average value of 150 ppm. Other elements reported are magnesium, manganese, sodium and potassium. Of all these elements only vanadium, chromium and zirconium were analysed for by spectrochemical techniques.

Sahama (1946) also included an analysis of another aupposed sphene. This supposed s7hene contains about 9600 ppm of yttrium oxide, 1900 ppm of cerium oxide. These values are considerable larger than those for any of the other specimens, and this sphene is likewise much higher in tantalum and iron than any of the other analyses. The total iron oxide value is reported as 26,000 ppm. According to Sahama sphene can be used as an indicator of the bulk composition of the rare-earth elements in rooks.

In their book, Goehemistry, Rankama and Sahama mention reports of europium in aphene up to 340 ppm and that it may contain up to several percent of columbium oxide. They feel that the yttrium rare-earths are characteristic of granites, while the cerium rare-earths usually seem to be enriched in nepheline syanites. It is also pointed out that aphene is one of the main seats of radio-activity in igneous rocks.

Coluabium is reported in quantities from 1,000 to 10,000 ppm in aphones analysed by Jaffe (1947), yaffe investigated sixteen sphone samples using spectrographic methods. He found iron, aluminum, and fluorine in all samples and columbium in about half.

Goldsebmidt (1954) notes a sphene variety containing about ten percent tin dioxide. He also mentions that the calcium in $phone is frequently re- placed in part by yttrium, the rare-earths, uranium and thorium and that one to two percent niobium is found in some sphenes replacing the titanium.

In twenty-four sphene samples, sixteen of which were also used by the author, Hurley and Fairbairn (1957) determined uranium and thorium ooncentrations. The average thorium ooncentration was 540 ppm and the uranium content averaged near 300 ppm. The minerals ziroon, apatite and epidote from some of the same rock samples were also analysed for uranim and thorium. It was found that the sphenes contained more uranium and thorium thian apatite and epidote, but less uranium and thorium than zircon,

Molybdenwa concentretions ranging from 34 to 400 ppm have been re- ported by rabinovich and associates (1958). Of the minerals they analysed, aphones had the largest molybdenum oontent. The highest values were from sphenes obtainod from areas near molybdenum mines. The method of analysis was spectrographic. Selection of AnAlysis lemeuts and Wines

It in necessary in choosing analysis elements to pick elements which might be expected to be present at least fairly commonly in detectable

quantitias in wphenes. The selection of onalysis elenents in this work

was done using three primary guides. One was the consideration of which trace aleaents ware of suitable size to substitute for one of the major

elements. The second guide was information available from previous work,

Thio gUide however, was only a rough general guide. The third guide was the qualitativc analyis of sphone 3085, the standard. This was the mst irportant step in deciding on the analysis elements. It was noticed in the study of the previous work that while the widespread occurrence of rare-earths in sphenes was noted in most cases, only in the case of Sahama (1946) was there any major breakdown into the individual slements,

On examination of the spectra of aphene 3085 numerous rare-earth lines were identified. These included lines of neodymium, lanthanum, cerium, gadolinium, samarium, ytterbium, erbium and praseodymium, The rare-earth elements chosen for analysis were neodymium, lanthanum, cerium, gadolinium and saiarium. The other rare-earths were not chosen as analysis elements because of the great difficulty in recognizing the individual lines of the different elements, due to near 'oincidence, primarily with other rare-earth lines. These other rare-earth lines were also of very low in- tensity and thua were assumed to be much more likely to be present only in quantities near the sensivity limits of the procedure. It should be noted here that in the case of gadolinium and samarium, it was still quite dif- ficult to distinguish between the lines of the two elements, since in the region used they are very close together. In order to furnish some measure of a check on the correct choice of lines, two lines for smarium and gadolinium were chosen (see Table 1).

Other elements found to be present in sphene 3085 and chosen as

analysis elements were chromium, iron, manganese, molybdenum, scandium, vanadium, yttrium, tungsten and zireonium.

Table 1 lists all lines that were measured for use in constructing the addition plots, their rated intensities as tabulated in the M.I.T. Wavelength Tables, and the wavelength and intensities of significant lines that interfere with the particular analysis line. All lines picked were the most sensitive lines of each element, which also hed the minimum of interference from other lines. Also considered in oases where inter- ference of some sort seemed unavoidable, was what element was conflicting with the analysis line. No analysis line was chosen that had a conflict with one of the mwjor elements calcium, titanium or silicon. Every attempt was alao made not to use analysis lines which conflicted vith a line of another analysis element. In esses where this was not entirely possible, the analysts line was picked whose conflicting line had the lowest in- tensity rating. The only elements where it was impossible to avoid choos- ing enlysis lines with conflicts were molybdenum and neodyuium.

Molybdenum 3902.93 is the only important molybdenua line in that region of the spectra investigted. This line, with an intensity rating of 1000, had a major interference with iron 3902.94C with an inteaity rating of

500. An attempt was made to estimate the contribution of the iron to the intensity of this line, through the use of an intensity ratio of the iron line to another iron line, however, it was found on subtracting that portion of the intensity calculated to be due to the iron line, one was left with a negative intensity for the molybdenum line for all twenty-three Teble 1

Analysis Lines used in the Addition Procedure

Interfering Intensity of Line *Intensity Lines Interfering Lines

0 4222 80

Cr 4254 1 5000

Fe 4383 1 1000

Fe 4260 A 400

Gd 4251,74 E 300 Sm 4251.79 A 200

Gd 4282o09 A 150 Or 4262.13 A 40

Le 4333 A 800

Mn 4031 E 500

Mn 4034l 250

Mo 3902,96 1 1000 Fe 3902.94 E 500

Nd 4303.57 A 100 Fe 4303.58 l 25

So 4246.83 A 80 Nd 4246.88 A 10 Se 4374.5 A 100

S& 4256 A 150 Zr 4256 1 25 Nd 4256 40 Sm 4329 A 300

Y 4379 l 200

Y 4374.94 1 150 SM 4374.98 A 200

Y 4398 A 150

W 4294 A 50

Zr 4239 1 100 I , , *From U.I.T. Wavelength Tebles. aphene samples. As a result molybdenum was dropped from the analysis ele*ents, Neodymium 430.5'73 also had a conflict *ith an iron line. The contribution of this Iron line was corrected for, as will be described later, end yielded meeningful results. SPECTRIGRAPHIO PRIPARATION SaMle Preation

As mentioned earlier, the sphone samples used were available to the author as minerals separated from granitic rocks. A list of the samples, their location, the type of rock from which they came and the estimated percent contamination is given in Table 2. These separates were derived from rock samples of about fifty pounds, which were crushed and concen- trated by gravity and magnetic procedures (Fairbairn, 1955),

The author took twenty-three separates and crushed each sample in a stainless steel mortar. The mortar was cleaned with distilled water after the crushing of each sample was completed. That portion of each sample which passed the two hundred mesh screen and was retained on the three hundred twenty-five mesh screen was used in the analysis. The samples were crushed this fine in order to free the included impurities from the ephene. This fraction of the sample then was run through a Frantz iso- dynamic separator. Each sample was run through several t imes with varying amperages and rates of feed in order to remove a maximum amount of con- tamination. Of course, some samples showed little or no improvement since the original contamination was so low. Estimates of contamination were made under a binocular microscope. In all oases more attention was paid to eliminating opaque and dark impurities than quartz and similar minerals, since one would expect the opaque mineral to contribute much more heavily to the elemental contamination than quartz. The processing of the crushed sample through the Frantz separator also had the important effect of elimi- nating any contaminAtion of iron due to the crushing in a steel mortar. After cleaning the samples an estimate was made of the percent con- tamination. This was done by spreading several hundred grains on a small Table 2

Locality, Rock Type, Other Accessory Minerals, and Uatimated paercent Contamination of Samples Analysed

Sam- Rook Type Locality Other Accessory Zatimated ple Minerals contamination

5011 Granite Leavitt quarry, 2 miles Biotitemagnetiteapa- 6-quartz W. of Leominster, Mass. titetourmaline,ziroon 3055 Qranite Hallowell, Maine Biotite,MUsovit8,ap8., 3-quartz fluoritemonazitszir. 3014 Granite Ourry quarryMaas.,2 . Biotitechlorite,epidote max. 9- BS3 of Wrenthem sta.Madf apatitefluorite,ziroon quartz 3058 Wuartz Sprucehead Island, Maine Biotiteepidote,apatite, 7-quartz sonzonite tourmaline, zircon 3071 Granite St. Gideon, Cue.-Lake Bio. ,chlor. ,amph.,magn., 2-quart St. John area ilannepd.tour.fluor.zir. 3080 Granite On route 198, 2 mi. N. Biotite,ohlorite,magn., 5-dark min, bit. Desert, Maine ilwn.,epidoteziroon and quartz 3139 Granite Route 11, 13.5 mi. Z. of 2 Mt. Laurier, Que. 3051 Grano- North and of N. Attle- Chlorite, ilmenite, 5-quartz diorite boro, Mass. epidote, zireon_ W05 Granite Mt 1Waldo, Maine Biotitepyriteapatite, 3-quartz tourmaline, zircon 3061 Rhyolite Moosehead Lake, Maine on Biotite,ohloritexagn., 4-dark min. route 15 amph.,epd.,fluor.,ziroon and quartz 3062 Granite Route 201, 5.5 mi. S. of Chlorite,magnetite,epi- 9-($ quartz 0aokman, Maine dote, apatite, zircon i dark min.) 3063 Granite Hollingsworth & Whit.Rd. Biotite, chlorite, epi- 0 6mi.W.from rte. 201, Me. dote, apatite, ziroon 3079 Granite On rte. 1, 1 mile S. of Chlorite, epidote, aps- 3-quartz (rapakin) yonesboro, Maine tite, zircon 3081 Granite Brriefield,Ont.on out- Amphibole,garnetiagn., 6 skirts of Kingston, Ont. apatite, tour., zircon 3082 Syenite Kingston Mills, Ont., Biotite, pyrite, magn., 2 6 mi. N. of Kingston liln., apatite, zircon 3485 Alaskitio Hope Lake, Kenora Dist., 2 Granite Ont. 3067 Syenite Brome Mt., Quebec, on Biotite,museoviteilmen- 4-quartz Iron Hill Road ite, apatite, zircon 3069 Tingusite St. Josef's Blvd., Amphibole, magnetite, 2-quartz Montreal Bast apatite 3084 Granite Gaspe Nat'l. Park hiway Chlorite, magnetite, 4-quartz Porphyy 7 mi. S.of Gaspesie,Quel tourmaline, zircon 3085 Granite W. and Mountainville, Bio.,ohlor.,amph.,pyrex, 0 Deer Is. Quadrangle, io magn.,epd., apa., zircon_ 2093 Quartz Dauphine quarry, Birch- Biotite,ohlorite, apa- 6-pyrite and Diorite town, Nova Scotia tite, zircon quartz T013 Granite Blanchard quarry, 1$ m1< Biotite, magnetite, 4-dark min. WW. of Uxbridge Sta.ass, fluorite, zircon 3138 Granite Rts. 58, 14.1 mi. W. of 12-opaque fine Dn Mt. Laurier, Que. or dk, min, ------1- ____ I 1 lip 1,0 MOMPO

grid under a binocular microscope, counting two to three hundred grains, and recording the number of non-sphene grains in this count. Due to the

extremely small size of the grains used, it was not possible in the time

available to determine what the impurities were. That portion of the

impurities that were opaque minerals is listed with the estimates of con-

tamination in Table 2, Quartz wherever discernible has also been noted,

Mixing

All mixing was carried out using a small agate mortar and pestle, both of which were scrubbed with cleanser and then well rinsed with dis-

tilled water before mixing each sample with either carbon or additive

oxides. In the case of the samples to which oxides of the analysis ele- ments were added, mixing in the mortar was carried on in the mortar for at least thirty minutes. During this time the sample was swept into a

small pile in the center of the mortar at least six times* This procedure was followed in order to get a uniform mixing of the additive oxides with the sphene standard, The rest of the mixings consisted of mixing one part of the addition sample or pure sphene sample with two parts of carbon by weight. The mixing with carbon was carried out for at least five minutes with at least five coning procedures.

Electrodes

Bach sample was run in duplicate. It was found in preliminary quali- tative work that one eighth inch electrodes with a cylindrical cavity one sixteenth of an inch in diameter and three sixteenths of an inch deep was the best available size to use for the sample electrodes, Spectrographic- ally pure graphite electrodes were used for all samples throughout the investigation. The twelve electrodes used for the addition procedure were weighed before and after loading of the samples. The variation in the weights of the samples in these electrodes averaged about give percent. None of the other electrodes was weighed.

Phograhic Materials

Kodak 103-0 spectrographic plates were used in all cases. After arcing, each plate was put in a developing tank for four and a half min- utes at a temperature of twenty degrees centigrade. Then the plate was fixed for at least fifteen minutes, usually longer. Finally, the plate was washed for at least thirty minutes.

Photometry

Measurement of line and background intensity was done with a Hilger non-recording miorophotometer. Measurement of both line and background was made on all analysis lines.

Spectrogaph The analysis instrument was a twenty-one foot, 30,000 lines per inch concave grating speetrograph on a Wadsworth mounting. This instrument has a dispersion of about 2.5 A per millimeter. The good dispersion of this instrument was the basis of the choice of this instrument. The near coincidence of many of the rare-earth lines requires a large dispersion in order to get maximum possible separation of the lines of the different elements. The region used in this investigation lay from about 3900 1 to

0 4500 A. A alit width of 0.015 inch and alit height of about 6.0 milli- meters was used. Arcing Conditions All samples were arced to completion using anode excitation at about seven amperes. The electrode separation was about seven and a half milli- meters. One eighth inch spectrographicelly pure graphite electrodes con- taining the sample were used at the anode. The counter electrodes used were three sixteenths inch spectrographically pure carbon rods, sharpened to a fine point. Counter electrodes were changed after each sample and resharpened for later use. The average completion arcing time was about one minute and fifty seconds, with a variation of about five percent. The variation of arcing time is to some extent related to the amount of sample arced (see figure 1). However, this relationship was not determinable.

It undoubtedly depends on many other things also, such as matrix, amperage, electrode size, etc.

Sector In order to reduce the intensities of certain lines to the point where they could be measured quantitatively, a sector was used. An eight step sector with a factor of one-half per step was used for the addition pro- cedure on sphone 3085 and for three other sphene samples. A newly prepared sector with a step factor of one-fourth was found to be more useful, and was used on all the remaining samples. This sector had five steps. What is meant by a step-factor of one-fourth can be explained as follows: assuming oonstant intensity over the ontira area of the sector, the first step allows the passage of all the light, while each succeeding step per- mits the passage of a quantity of light equal to only one-fourth that allowed to pass on the preceding step. SOURES OF ERROR

There are two general types of errors involved in quantitative spectroehemical analysis. They are those inherently present in the sample and equipment used, and those introduced by the analyst.

In the first group are included errors due to contamination of the samples, development of the plates, non-linear step factor, and due to im- purities of standards used in the addition procedure.

14 Contamination: The estimates of percent contamination are listed

in Table 2, The average percent total contamination is about four

and a half percent. However, it is very important to notice that

in at least ten of the sphenes nearly all of the contaminating

material was quartz. One would expect quartz to contribute very

little to the contamination in the elements being analysed for. This is especially true when quartz is compared to minerals such

as augite, hornblende, or hematite. Hematite for instance con-

taina seventy percent iron, and a twenty milligram sample with a

one percent contamination by hematite would have 7000 ppm of iron

due to the hematite alone. This is very considerable contamination

and is an extrem example. Hematite is quite unlikely to be

present as a result of the separation procedure used. Most con-

taminating materials will contain many times less of the con-

taminating elements than hematite contains iron. Quartz can be

expected to make essentially no significant contribution to the

contamination of the semple in any of the analysis elements. On

the basis of this consideration and the observation of ten sam-

ples, whose only visually detectable granular contamination was

quartz, the estimated average effective contamination is about

22 0

two and a half percent. This lies well within the error introduced by the analyst.

2. plate Develoment: 7Errors due to development are extremnely smsll

on the same plate. TrIrors from plate to plate due to variations

in the plates and in the development of each plate are thought to

have been largely compensated for by calibrating each plate in

three separate wavelength regions and by the use of comparison standards on each plete. Mrror due to this source is considered

to be negligible in relation to errors introduced by the ana- lytical procedure,

3. ?rror due to Non-linear Step Factor: As explained earlier, a step sector with an assumed linear step factor of one-half and

later one-fourth derived from the g sometry of the sector was ueed

during the invostigation, Actually, however, the intensity of the

light in the are varies with the position in the are gap, and thus the intensity of the light reaching different steps on the sector

varies (sen Dennen, 1949), In order to minitize the error from thia source, intensity readings were made on the same stop wherever

possible. However, this was not possible in many cases and thus

since the factors of one-half or one-fourth were assumed, error

has resulted. Based on the work of Dennen (1949, illustrated in

figure 11 of his manuscript) concerning this problem, light from the center of the are was as accurately as possible caused to fall

along the slit. Dennen found that the intensity in the central

portion of the are was the most nearly constant. In this way it is felt that the error from this source was minimized. It has

been assumed in this investigation that this source has not

23 contrIbuted eignificnntly to the error, 4. Error2 due to lpurity of Standards Useod: Oxides of the analysis

elen~ats t Teprepnring the additton standrds are in generRal

quite pure and contributn errors which are very definitey negli-

giblo, and actually in most cases lie below the detection limit.

This is the case for the oxides of zirconum, iron, yttrium, vanadium, tungsten, chromium and scandium used in this study. (The oxides are listed in Table 3.) Rowever, in the case of the rare-earths, it is much more probable that larger errors, signifi-

cant ones perhaps, may have been introduced due to impurity of the

oxides used in preparing the stendards. The reasons for this lie

basically in the great nimilarity of the various rare-earth ele-

ments and thus the greater ease with vhich they substitute for

one another., The kind or degree of contnxmination of the rare-

earth oxides used is not known. It is known that they nre old,

however. It is felt that error from this oiwoe, especially in

the cases of samarIum and gadolinium may be real, Wit since no date is available on the nurity of these oxides, it was not pos-

sible to make any corrections and it was assumed that only the

analysis eleent of the oxide was present.

In the second group are errors introduced in weighing and mixing of additive oxidesloading and arcing of the samples, measurement of line in- tensity, construction of curves and errors due to loss of unvolatilized samples

1. Weighing irrors: All weighings of the additive oxides were made

to the nearest tentit of a milligram. rror due to this source is certainly considerably less than a percent. 2. Mixing Yrrors: Mrrors due to non-uniform mixing of the oxide

eAddtive is untknown. The mixing roceAdure described ;asrlier is

conidered to hrm rerAered error tron tM.- sou:c to be nlw i-

cIble.

3, %ror due to Loading and A'ircing of the Sprles: From twelve

lofided electrodes used in the addition mocedure it is es:timated

that the error in the sarple weighta sroed is of the order of

five percent. This Varetion in sample weights, of course, Is

also reeponsible in come measure for variation in sroing tire

and thus exposure. As mentioned earlier the arcing time showed

about P five percent voriation elsa. The nature of the relation-

ship between sample weight eid aroinr tine is not knotn, and was

rot investigated in this study. Eowever, somr indicetion of a

relttonshlp between variations in san-le 'eight and aeiri time

ray be seen in figure 1.

4. 2Wrors due to Measuremeont of Line and Enckgrotud Intensittes:

?rrore firm this source are, fror reneral erperience in the Cabot

Lraboratory at Y.I.T. where this work ras carried out, considered to be of the order of one percent.

5. Error# due to Loss of Unvoletilized Sample: Errors due to this

souree are unknown, but considered to be small, leas than s per-

cent, The raing conditions and weight ratio of sphene to carbon

used gave a very steady end smooth arc, with very little sputter-

ing. None of the samples used in the analysis had any significant

noticeable sample loss. All semples were areed to completion.

6. Errors due to Construction and Use of Curves: Errors from this

source can be introduced at three stages in the particular 10 X 10 PER INCH

1- 1

- t

4.1

-44 +4- -+

4 -. -.-

- -- -T - * - - * - I . . .---.-.-- ,------

tt

-t +. t-- T-V- .- - -7

1 -. , -- -

- - I -4- - -

- --. ---- t ---+-+ --+ - 7 7 7 7 Yt7~ 7 - k7--V-+-- -11- t T I 7 - -<17 7tw

V 4_ _-_ _- 4 - -- - + ------_ _ ------,~ - t :: - _ _- _-_-- _+ -_ *_--_ - I4i 1~. 4 1-r t- - >77 ''.4. -I 4,

CA1 14k 4y7/ r/uip.c/y 7ne -Seconds procedure used in this investigation. Errors are introduced in

the plotting of the addition curves used to determine the original

amiount of each element present in Sphene 3085. These curves also

introduce error efter plotting, in the interpoletion to determine

the original concentrntions of the various elements. This problem

is discussed under the section deaJing specificlly with the ad-

dition procedure. Tt is sufficient here to note thnt errors in

this part of the study '411 here en imnportant effect on determine.

tions in all the saM'oltes, stince it is by the standard (3035) that

the concentrations in al the rest of the semples are determined.

The sfftct will be a shift of all determinations in the same

dtire'ction frrom- somw aRolute v'ue,

A second rlaco where errors 3re inrtoduced th-ough graphical

procedures is in the plotting and the use of calibr9tion curves.

This error, w.hile pronbl not an ,ritirO or as generalized in

effect as the error involved in the eddition plots, could be

ocalif ant. It ia sfilt, howeviir, ie to the construction of rmny such curves, that the slopo of these uirrea is subject to a comparativaly sanll arror.

The reywaining graphical orror is thtt involved wi the work-

ing curves Cor each elensat. Thie also is disicussed in more de- tail *lSewhereB.

No aotual oatimate of the error du to the construction and use of theoe ourvta is available. Uowever, it seems reasonable to expect that an error of fru rive to ten pereent &ay be intro- duced from this uoarce...... ------

It is estimated that the total probable error involved in the deter- minations reported lies between about ten percent to perhaps as much as twenty percent. Different elements will have somewhat different probable error. While these sound like, and are, sizeable errors that need to be allowed for, it is important to realize that the importance say of a twenty percent error quantitatively speaking is dependent on the general level of concentration of the particular element. Thus with a 100 ppm level of concentration similar to the values obtained for chromium, the actual value lies between 80 and 120 ppm. While in a case such as iron with a general level of about 20,000 ppm, the possible values range be- tween 16,000 and 24,000 ppm,

28 ANALYTICAL PROUD(DURE

Method of Analysis

In order to make quantitative measurement of the elements of interest, it is necessary to construct a "yardstiek" using one of the samples. Once this has been done, this standard an be used to make determinations of these same elements in the rest of the samples. I chose sample 3085 as the standard aine it contained no visible impurities. The addition method was employed to detemine the original concentrations of the analysis element a in sphene 3085.

In this method an oxide mix containing equel or nearly equal amounts by weight of each of the fourteen original analysis elements was prepared.

A list of the sources of these analysis elements and the percentage of the source that is made up by the analysis element is given in Table 3. This oxide mix was then mixed with sphene 3085 in such a proportion that each analysis element had an approximate concentration of one percent or 10,000 ppm. Then one part of this prepared addition sample was mixed with nine parts of pure sphene 5085. This gave an approximate concentration of about 1000 ppm in each of the analysis elements. In analagous fashion other ad- dition concentrations of 5,000, 2,500, 350, 100 and 35 ppm were prepared.

After mixing these samples one part to two parts of carbon by weight, they were arced in duplicate. Addition plots were then prepared to determine the original concentration of the analysis elements in the pure sphone

3085. The graphical procedure is discussed in the section concerning ad- dition plots.

29 Table 3

Compounds of the fourteen original analysis elements used in the addition procedure and the percent of each comprised by the analysis element

Percent of Campound Analysis Element

Ce20 3 85.A ce

La203 85.3 La

Gd(N0 3 )3 45.8 ad

Nd203 85.7 Nd 56.0 V V20 5

Y20 3 78.8 Y

Mn02 63.2 Mn

MoO3 66.7 Mo

w 100.0 W

ZrO2 71.0 Zr

Cr203 68.4 Cr

Fe203 69.9 Fe

Sc20 3 65.3 So

Sm 100.0 Sm 4' aN - I -- 0.11 A 1 -11 ---- .I -_ -1------ft , W I i9i -I

Graphical Procedure

Three types of plots were used to determine the concentrations of the

analysis elements. These are calibration curves, addition plots and work- ing curves,

Calibration 'urves: A calibration curve has to be used at each wave-

length in order to convert defleetions from the miorophotometer to relative

intensities. Calibration curves for different lines may have different

slopes. A separate calibration curve was prepared for each line listed in

Table 1 on the addition part of this investigation, which was all contained

on one photographic plate. Examiuation of these curves showed that only

three calibration curves were required. One was for use with molybdenum

3903, a second used for manganese 4031 and 4034, and the third was used for

a 0 the region 4200 A to 4500 A, which region included the rest of the analysis lines.

Addition Plots: Two plotting techniques were used for each analysis

line in the addition part of the procedure. The first of these was the

standard addition plot discussed in Ahrens (1955, page 33). This is merely

a plot of the relative intensity of the line of an element as the ordinant

versus the amount of the element added to the sample, on the aboissa, A

curve is then drawn through a succession of these points. Ideally this is

a straight line which is then extended to intersect the aboissa. The point

of intersection of the aboissa and the extended addition curve indicates the original concentration of the analysis element in the sample,

The second type of plot is the same in all respects except that the

intensity of the analysis line was ratioed to the intensity of one of the major element lines, calcium or titanium. These mjor elements were assmed to be present in an essentially constant proportion, This method then is really just the internal standard method applied to the addition plot,

To the best of the author's tnowledge the only previous use of this ratio teethod with addition plots, "we that of Ahrens and Gorfinkle (1951), In this article little more was said of the method other than steting the fact of its use.

In the particular case of this investigation, calcium, camprising about twenty percent of sphene was used as the constant internal standard element for all analysis elements except chromium and zirconium. The calcium line used was 4302. In the cases of chromium and zirconim, titanium, making up about twenty-five percent of sphene was used. Since there does seem to be some relation between the weight of sample and are- ing time, there is presumably some effect also on the measured intensity of the lines, It was hoped that by using this ratio of intensities, that variation in the sample weight in the addition procedure would be com- pensated for and result in addition plots whose points would be the same as if there had been no variation in sample weight.

It is important to note here, as concerns the graphical procedure, that while both of these types of addit ion plots ideally give a straight line, this is not the case in actual experimental work. One important suspected cause of the non-linearity of the addition plots, is that as the concentration of the analysis element increases, the amount of self-absorp- tion also increases. This of course varies with the element. This would have the effect of reducing the intensity of the line at higher concentra- tions and thus result in a decrease in the slope of the addition plot at these higher concentrations. This decrease of the slope of the addition curve with increasing concentration of the analysis *lement, especially at the 10,000 ppm added level, was noted in all oases except twv or three of the ratioed addition plots. In nearly all oases the ratioing of in- tensities is observed to have reduced the amount of non-linearity as com- pared to that of the ordinary plots.

In constructing the addition plots and determining the original con- centrations in aphene 3065, the straight line that best £ittea the curve defined by the lower concentration points () through 5000 ppm added) was used. It does not sem that the ratioing of the intenaity of the analysis line to that of the calcium or titanium line necessarily reduces the varia- tion of the two points from the mean, However, the ratioed type of ad- dition plot definitely does seem to increase the linearity of the addition curve in many oases, This definite improvement is illustrated in figures

2 and 3, which show the results for iron 485 and iron 4E60. As can be seen from the figures both iron lines give larger values for the original iron concentration in sphsne 3085, in the standard addition plot, than they do in the ratioed addition plots. Also in eaoh case the linearity of the ratioed addition curve is increased over that of the standard curve.

This is particularly evidenced in the case of iron 4383, in which case a straight line can be drawn entirely within the envelope of intensity ratio variation at all points of concentration. This ratioed addition ourve determination of iron was used as the experimentally determined iron con- tent of sphene 3085. I have drawn as can be seen in figure 3 the best curve through the ratioed intensity points for iron 4260, which gives nearly the same value obtained from the ratioed iron 4383. - 1 ~:1 7 12> 4-

___ 1' 1 1 1 Sj4ZI dd1f10~7~Pf~,4 fAj'~~Pv

li .3 c

r' 4 -+ _ __ -- -+--4-- *-- - 0.**

4 2 5 - i 5 -: T-T - -

1 i------4 - - +-1 -~ j

- 4 - l4]4 to t11S-4I , T30 T - r - - TTT_ T - -..-- T t - i T ~~1~ I 14~444 4141 * 4 44 - i t4t4 4r ~ 4 tri V 4 4 44-I T -T-I ryt r F-i-ii< (Ti tILl 4 1-A - It4~ Th F- 727K Th1§j{ 1 -T I I I T~J7 I;; .4-4-i ii 4~444. 4 -+--4-----.---. 1 ~ T

* . III rIs . -- '.4 '''IL>: II -

-T- + - - 1

--- , 4-, ------1- -1

_t_ .- -,-..+--. - - - - * -- - ______4 v-- 1

.1. , -Vt-Vt1 1 4i~7 -- 4 p44.

- ~ ~ I 4,44., -- 4 - - ~4 442~+ <4- T t -- t 4-4--t - i~~~777F- - -4 ~4 --+ ::::' 2 1 t

I Caio /,000 000 go.c 3/ S 7 de d Pets rI o -A. - +T.11

--t I 1S j ------T -I

4 I-.. I -d *-~4 II L1 -t'44. t-.V --1 -I r-~-~-

4- ~ -4 -'I

1 {

4- 4 --

t__ 1:11 #7--

_ _--- ' _- ..-.

- - - - - *.--~22A'i~i1 I-*-i

______I_ _

-_ +__-- _ _-+_ ------7------1 _- _--- - - __zi ~~u_ I -- A 1:1:1 17+APTTC 1--- LL4J ± I g- ~L-. -4 000.. . /Co z o00 3, 00 500o /0,000 -L Added in /-f peb- In Mst cases the ratioing did seem to give improved values. There were some ceses, however, in which the ratioing did not improve the curve at all and may in a case or two have made it worse.

Working urves: After determining the concetration of the variouc analyaia elements irL the andard, working curves were establishedc and constructed fur each element. A working curve was plotted for ea:h element on each plate. This was done by plotting points fror three different known concentration levels of the standard for each element on each nlate, The iflope of the working curve for each element as assmed to be forty-five degre$s (Ahruns, 1951). The base experimentail working curve eqas conatructed from the addition data, using all the concentration levels prepred. In most oases the conoontration determined from the addition plots gave a working curve with a slope of nearly forty-five degrees and thus agreed quite well the asamed slope suggested by Ahrena. In the ease of chroa itum, yttrium and gadolinlia, minor adjustments were made in the original con- centrations of these elements in sphene 3085, until the working ourve was within a degree or two of forty-five degrees. The exact procedure used in this adjustment is as follows. When the angle of the working ourve is nuch greater than forty-five degrees, the original concentration used for the working curve was too high, while an angle less than forty-five de- groes indicates that the original concentration used was too low.* This procedure was used in detail with manganese, which is discussed below.

In the case of mngenene, two analysis lines, Vn 4031 and Mn 4034, were chosen for purposes of furnishing a check throughout the invostige- tion. The original concentration of manganese in aphene 3085 as determined

*Personal communication from Dr. W. H. Dennen. from the best addition plots, was 4700 ppm from Mn 4031 and 3800 ppm from Un 4034, For both lines all the working ourves for all the plates used

were plotted for each of the two assumed original concentrations in aphene

3085. In all oases exoept the working curve from the addition material

for Mn 4031, the angles of the curves for the 4700 ppm coneentration were

considerably greater than forty-five degrees. On the basis of the above

mentioned criteria the 4700 ppm value was regarded as being too large.

The angles of the working curves for the 3800 ppm concentration were in

all except the case of the addition plot for Mn 4031, very close to forty-

five degrees. Thus 3800 ppm was the concentration value used for manganese in pure sphene 3085.

In the determinations of the analysis elemntiats from the working curves, only one line of each element was used. Selection of the line used in each

case was based on considerations of apparent sensitivity (as revealed by

the addition plate) and aininwa interference. The only exception to this

general method of selection was manganese, In the ease of eanganese, the working curves indicated that Mdn 4034 gave more reliable intensity values for the remaining twenty-two samples. Thus, for these samples, intensity values for tn 4034 were used in preference to those of An 4031. The analysis lines used in the final working curve stage were: Fe 4385 A MA 4034 Y 4398 A Sm 4329 A Gd 42522 V 4379 A Ce 4222 A Or 4254 A Zr 4239 A Nd 4303 A S 4374 La 4335 A W 4294 A Molybdenun was discarded as an analysis element in this $tage, when it was found that overcompensation had occurred for every sample when a correction factor was applied, ISCUSSION OF RSILTS

The concentrations of each analysis element in each sample are tabu-

latod in Table 4. 'eeh value shown in the table is in all cases, except a

few, the average of two determinations. Also given in Table 4 is the

average peroent deviation from the mean or probable error for each element, This figure was calculated for each element by dividing the deviation from the mean of each pair of determinations, by the raean itself, and then

totaling all these deviations and dividing by the total number of samples

for which two quantitative determinations were made. This answer was then oxpressed in percent. Thus in the case of chromium the average percent deviation from the mean is 6,76 percent. This means that any reported de- termination for chromium has a fifty percent chance of being within 6,76 percent of the correct value. The error of the averge of twc determna- tions is then simply the probable error of L single determtination divided by the aquare root of' two, i.a., 6,78 /VW for chromium. It was not possible to make quantitative deteriminations in all cases. In these oases the elements were not detected or at best just gave trace indications.

The beat that could be done was to take a rough estimate of the neximum pos-ible concentration. This was done in all cases exoopt one for tungsteu and numerous times in the case of siandium.

Th avsrag~e of thu two determiations for each elenent of each sample are plotted both. by clemant, graphs 1-, and by sample, graphs 10-%. Smi-

Lgarithnic paper has ber used in the plots in order to accommodate the wide differencue in conxentrtlon, emd vntain raative variations of the elements. The results wll first te discussed by element end then by semplea. Table 4 Average Concentration of Analysis Elements in Each Sample (All vaue ,given in parts per million) Sample Fe Mn Y V or Zr c La Nd [ Gd W 4383 4034 4398 4379 4239 42221 433 4303 4329 O262137 4294 3011 8250 5200 16001o0101360 680 500 340 27201 165011650 140 3055 9300 1930 2320 8601600 1000 490 470 2450 1220 1390 475 ND 3014 21350 615o 11400 470 28 4450 550 530 2120 4900 5000 510 3058 i615o 3650 3720 1080 70 490 200 260 1400 2100 2050 130 ND 3071 20350 410o 7850 220 28 52o 320 275 1910 5800 3950 <75 ND 3080 27500 4620 22000 650 165 2250 820 450 3780 9450 5800 980 ND 3139 24000 5320 4120 300 18 2280 1360 1660 2500 3020 2950 130 ND 3051 24200 6400 14850 440 26 750 1160 520 2680 7800 5900 '75 3060 21100 5950 9550 600 78 580 1620 950 4050 4500 4000 360 ND

3061 20400 3900, 63o0 860 100 2o800 1030 700 1750 5700 3900 280 ND 3062 18250 5300 3640 760 31 2350 4250 4020 8350 3980 1980 160 ND) rae 3063, 18150 4780 "4100 1060 67 2800 4020 2180 8500 6500 3850 210 ND 3079 22300 4050 1365o 880 85 820 4780 1780 11200 5450 3700 380 ND NI 3081 20750 2760 3700 570 125 3120 3600 2290 6100 3650 2080 <75 ND 3082 20800 3350 2420 130 22 1900 148o 1330 1880 1700 1100 00 ND 3485 18250 2680 1860 860 91 2380 8150 3980 10350 5250 2060 475 730 3067 21950 5170 2120 310 36 5900 3580 3550 4950 2600 3820 <75 ND

3069 15500 2750 99511040 23 390012850 2680 4550 1450 2420 100 ND 3084 13000 620 740 1060 92 1760 3820 2280 5150 2000 1500 210 ND

3085 15900 3800 2700 800 70 3100 4200 3000 4200 1850 1800 150 WD 2093 1165 19140 2480 9140 635 2180 820 8700 1550 2020 1650 '75

3013 15250 8550 15500 240 38 18900 100 100 970 2200 COO 3138 51500 I1750 ho0 1160 16 2280 1340 1000

1. Iron: Iron (graph 1) is present in all samples. The iron content

varies from about 8,000 to 28,000 ppm, with the exception of over

51,000 ppm in sample 3136. It is almost a certainty that much of

this last value is due to contamination, as indicated by the ezti-

mated trelve percent contemination consisting of opaque grtins

(Table ?). Most of the iron values seem to lie in the neighbor-

hood of 20,000 ppm. On* can notice some degree of imilarity in

the shpe of the Curves for gedolinium (graph S), sameriuam

(graph 7), and iron*

2, Chromium: 0hromium (graph 1) to clso present in all samples,

Chromium values en much more vsriable prnportionately than iron

ard rer grent deel lower, All the semples tnalysed contrtned

lees ter ?00 ppm. The erjoritr o+f the Yrlu- , e may be asen

from either Table 4 or graph 1, are less than 100 per. It is

noticed that the three samplee containing the highesteoncentre-

tions of chrorium also have the three loest vslies of iron.

These sanples are 3055, 3011 end P,091 4

. Manenrtese: Mangenese (gryph 1) is nroesnt in all a'mpos, with

moat of the lvalues lying in the range of 4000 to 6000 ppm, There

zmeerrs to be "eneral eimilsrity in the sbaps of the crvtes ffor

manganese (graph 1) and gadolinlum (grenh 8),

Zironirm: Zirconium (graph 2) was found to be prsent in all

afsnrien. The variability in concentration is rather high. About

half of the values obtained lie between 1800 and 3000 ppm. An

unusually high conoentration of almost 19,000 ppm is reported for

sample 3013. It rould seem likely that some of this is due to tj

...... 77 4 444 tl 4- r4 ---IT-- -4 ...... IliL.IkL h 71-' 7 4 -1 +tj t,+-,- T I, T :I t kill A 41.,1; j I-Ir f4t +4t

I T t tT l t4 4 + 'TI rI i Tm 1, i 1 T1 1 1

t r- -f4+t 71 4 4 1 T 7 T 1 ; i w U"* 4 t4 69ve q -

--T 7 q II. . I - .- I I. . r I . I I I -- i'+++ t1t A!:! 4-1 -i 11 6 - i 4 1 t-'4 1 I"-.

- , I I.. ! tt+ hhL~7i7 ITI I I I I I . ... "I I ill' if I fil-l-l

Tr~ K~22of, +--4~i4ii~' 4 I ~ I ! I '';. I I 44 42..- 27<274- T±--4 ilit1 si

v~~r J, + + 7 7- -T T 4" T T 17 j' !

7 T *2 - IqQvf lot J44 t - tT if A

4- 4 -

+ ic 4

-t--- 7 T it + i 1, 1 r tl:. will TT I T 1 t4 -7- t--t- -sot

4 liz t 4 +t 4-4-- -t4-

-- 777 T"l r 4+4 L4 it 4-l 7-1 4-4 177~7~7i- -N If Or O~~~~~~~~~h~~ ( (Cn~O U W W~~ J N v C' m a) r- (C it) 1 (1) - 0 -ODN (D if) I (Y) - C) a) r% 0 U) lill l 0' 0 t0 W4 L40 4 U 0) -4 VI4 N

-. t------+ .4 7~71j7' 7 4 ir-711171172 1. 1- -.. --...-. t t - - . .. .

4-t -4- J-

S dOlp 4. . .,..-. 724' 4 - +BOE v +

4-1 - . tL- - 0-

t$ -4i sg8,f ITO

T T r

IL -E - h.-

-t IC 4t4 t T-12-.2t.Ab

Wil - -,1 1'0F Plof ? it t. i i T I4 + tTt- ~t 'Ht kt rj TTliTT++it " r' . . I ~ .~4hK7 ., ~~zzzt~T

t ww

Q -7: -- ___ ~ K 1 o y t4

-14 p4- L7 H ~1 z-.7 - -- R E ;4-, '0E - a r L') I - ) Or- ID wJ 11 - 44 CD !I. ( m1 It oontamination, perhaps by zircon,

5. Vanadium: Vanadium (graph 3) was found in all samples and varies

from about a 100 ppm to about 1200 ppm. Most of the samples had values between 800 and 1200 ppm.

6. Yttrium: Yttrium (graph 4) showe a wide range of variation from

about 700 ppm to about 22,000 ppm and is present in all samples.

Most of the values lie in the range 3500 to 6800 ppm. It is po.

sible that a few of the very high values may in part be due to

contamination as all samples with high values have at least three

percent contamination.

7. Lanthanum: Lanthanum (graph 5) was found to be highly variable

in concentration and was present in all samples, teept for a few extreme oases the values lie between 300 and 4000 ppm. Lanthanum

generally seas to have values which are the inverse of yttrium,

i.e., in general when a sample has a low yttrium concentration,

the lanthanum value is reasonably high and vice versa. As may be

seen from graphs 5 and 6, there is a definite parallelism of the

ooneentrations of lanthanum, cerium and neodymium. When a sample

is low in one of these elaments it is also low in the other two.

8. Cerium: Cerium (graph 5) was found in all samples and was highly

variable in oonentration. The values determined ranged from

about 100 ppm to about 8000 ppm. There seems in general to be an

inverse relationship between eerium and yttrium values,

9. Neodymium: Neodymium (graph 6) varies over a range of 130 ppm to

about 11,000 ppm, and was found to be present in all samples ex- cept two, which is discussed below. ) (A) 4. Ln a) ( _ja L 0 OD ) w N ( 0 ) '4 W a;i 0 N 0 M 0 301/ ~ )'4 _4 ~

L -

+- +-

I ,,'I * II - ~+.--r±- ,

77211..... +L~I .42411 i 7- it I

-1- -+ --t I l _H1 -4-+ 4_4 + +*+ I±2,I2,kd 4 7'-.-..-4j 4 : 4 i. 4 .~ '.

* 44.5. ------

3OGO. '--4--A. 1. .. T 44-.4+A44.V ~2~ 1. - 4 rr 44

-- t -- r- .4 -i4 - -t -t -t -- 4 -+ 44 4

1-T j" j i 1.t 7 f ot _7T rTYL~ 7TT17T~4 T 44-~~T 74.4221Tt4-.4 T.2I~2

30(*7 -4 oI~ ffi _ 1224 + - .4 4-1- 44 4* ftf t

7i F N 1 44n 444 i_4 I h Ti 4 P . ? - c:7- - r' -

...... fl tT 44 44--'. 44; 4

- I . ,. . '- I' I ,, . ~'- I'' -4~~~~ . ATI. '-'I-.,- -i r. "- Coic eta/4cP,0 A" ts 40pac Iia,1"0 T- - T 1T- 4- It 4- 77/7-

-4.4 - -4 ---

aT -1 -- - -, 44 +4 .-- + 4 +

~I- t4 TtTU - t -T t1

1 T -

7h - - . -IL t-- H f 4 + - T n H9 T T 00TT 4 .

4 i +-

9 0 E nt i i f

-T - r

tt

-t ---- _

4 -

ri t T t -

t + t- +

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fir+ , ++ -T- t--* w 4 o:, ,jm D ------. N W 41 V1 U) 1N 4I ~I W 1,- 1 T . ! 1 ! -- .. . I TI 1,. , 301 I I . si L I . I ILI-, I ! I I .1 I I' ! ; I I I I :: ,, "I , . .1 -_ ----i,--' _--t! T I .,,444_i+ -f- .1,.., _ : : I 1 , , - , - -.. . _. . _ .. ;41. -- I -. _ . . +" - 1- - + 4_4,4 ! .. - ; I 11 I -, I- , ! ij%I I I. 1. -- - ., I + __-- _4 - - --- . - - , 1 j- - r t, , I , -_-t I.. - , ... 1 1 _ 4 4 . I 1 tl4t I I !Il 111 . I I I : I L I I pI I i&.' -;t , -- - I . -- , 4 11 .-; . I :: --- !It11 I444' ,j ,I "II I 11 L I -.- t-- , ,+.++--1 , ." - ______- _ - -, . . 4-4+- -t . +-I- ; - f+-_1 j .+ -- ___,.___ , II I. , ,-- l , I "I'llIII I I jil 1- ._ j - _4 ,.4-I , ... 44 , 4- 1 , , -+. I , -1I I I . I I I I , , , 7 !,!t I I .1I---_ l---- I I I -- -- t-- '! I I - ,I1 11.1 , _44H LI __1 _: ;4 I.i +-t4- , _F I ;_ +_14.4 4 . T_ to' 4' - 4 i -- _-, - - . .-- - 1 1-+i,- I + -- 4---+4 , , , 3056 --.-1,---I., - t - - " 1_ ,4. _ 44,4 + i I , - --- ,- 4 , . + , - -t - j I I ----- _- II I . I -- __,- - . .. , + +.i . : . I 1!1 I - 1 _ _ -- --I tr - - 4-. +4 , I , I ii :7.1 - - -- . . 4 - ' I _-, I i I'! 4 4..-- - +--r III- -i ' ' T'4 I , . - !- i- ; 44 -- -1-T ,' : : :4t It, I I 1. , , I , ,, 1 ______4 ___ .1 .-..t_ , ___ .1, T,,- Ii .. .1 I I & i r I - . I -, i I I i . I I I I I I t+ ., I ' I ! , '' ; 11 .. , ; . , : , ,, II7 , I. . I I L , , ,_II I . j _l .1 - I II I- I - ; , i i ! I+I : -tI I - -I l .- 1I 17 - i II _, 1L , 1 ,, i . I : I i,, . I .:L I ; I 1, I I I : 1 I I 1 . I . I, , I I I _ ; .. I . I I I I ! I 1 , I ; 7: , 1 'P , 2 1 1 1 1 I j I ; : , l - :11 1 'I4 ! - - L , I . I, !I;; ., J. ll I I . - , I j.. T 7 , , I II I i I , : , I l i ! i 1 I : I: : ,ill _ .4 - !_ , . ! 30/If _ _ 1 -.- _ - ". - 4, , , , ,+ . - I 1 l.....,, , - __ - _" _" t _-__' I-- * 0 _!I ,.I: _ "I , t4-1-I , I -+-t 4-4 -J4 - - -4- --_" +-- -- .I-- I r - I j :: I -*II ill ':I I , -I . __I__- I I , , . : t " - 'i.. I I I I . -. I; , - . , " ., , , l . ... I - -.I--. -. - + - _ _ i I i I I , 1 7 j! -1,- f-- --+- 1 ! , ..11 :: I '! I : ill !I ! _. ._ _ - I j I J_,+ 1 .. ''if - i ""I , -+-+ __,__ _ ,I ! , ,T,, I L , ; t !! T -- --- ._,,44- ,4 ""I I I " I q d 11 , 'Tli :,; iji T ; i : . 1 :: 1 1!1, ", :.: , __ - 4. 144__. 4 4 . .I I . I ; , . i i , i ! L I , I .. I ,, .. , I TI j I ;IIj 11 I .- I + I , , , . 1 , , I I t l F ____ I .. . . I t . _.t " , . L -- jL +_ -- -- I I 'I'le - I__ I4 , _. : , , -" , I I j , .j I I 1 1, , ,; , I , ! , I I * , , I t I ,T_ ,,

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'' ,,, '" , I4" , 1. : , :11 ---- i ' ' 7 - I - - l ! !lOill"I ; I ". -4-+ 14 -4- . 1 ' _ +-- t-4-+ 1 F , f I l I ..- -- I i _ " , , I I I 11 T I I . .k I I l, l2_ . - __ _-+ +1 4, q I i . , , . . -- I __ , T I I ; --+.- -:' ,::It:t-j-4, I . - - I 11 I - -T d -. t _t L - . -- - -- . _.." -- 4-44- -, - i- I , -_--r -r- t , . ! _-,- I j I I p I I I. -I4 iil , , I II II : ; , ,t -1 i I , I ...I .11'...... I I ..- . - l't ! I - f 4 , 41 I 7 :1 I1 . I .I.+ I I.. - -t . - . I . . - 4 F - 4f ;i I p ,lI i, ..l,7 . 3,060 - _1 i . I , j !I ___ _ 4 4_, _t 1 t4l C I I i I , I T1 ! , jr I I i I 11 Fq I I_ , , - I , I I ; I Y ;, , , ,,' , , . , , , . _.. , , ,, . , , , , _ -1 - i . 4 I - _ ; , t ; ; : : : . I I [7I + -, r -- . . I t i ! ,T :; I- i l 'I , . ,i 4 4 'I d , I I I I i -I . lit - -4 , ; , : '; ! I L : j : I , . . , , I I , , : , : 'Ic 4I I .-- I , i I.. I: i.; I I. - + 1-1- - I I- . ,-I . 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I .- I . I . I ' L , , I I I__ - I , I . I II I , , I I , I I I I i t I I I I I I +, - - " , " ;_, _,,- i -4 'I ,4- . -4 t- - +t - , ,. __ ; I . I . I !Ili ! ! . I : ; I I I. I; 1 I I '" _ - __ I -- __ __ - ___1 oo p . I I I I I , I I I .'.'I -4 4- .;4 1, ; . , , i- ;;; I ---. I ' L " r , I I I L I , I i -,+ L - - -- t-4 I , -r, I ." - , .11 -- t___ - i 4 _r - - I I I -"-+ - j 1 - I .- I I I . .30 ?2- _,I-.------,-4- ---I , , : 11, Hl! L1 i ; . -4I I -'' L- 7 , I i 1 __4__4__4_4_."I . , . I.. ; , . 1.I I ___ . -t , +11-r i Tr I71 11.11i .117 d -- t T T- -T- -j --! j 1I i , 11 1 z,Ij;1 I .. i . ! I I : , ;!i II I ! .Ili.lll ff "I II II .11 Ili 1hi I I i I I . L I I .. 1_1 4_ ; - iIll . I __ --- - , T",M-4 ,4 "I'll'... . ,l -- -- . - - 7- - +- - -t- - , 1 -14- - t-- ! ! _-- I .. ... I . I': -,--+ -- -- _ I . ', - . !: . ... I . 4 . . ----I-"-. I . I -i ;_ . -tt4 I I . I . I I I I + I . I . . ! I -!t-I I 1 4I, . .r .. d . ... . ; I!tTll, : : I -- . : ! 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" !- . , . + . . 1 - 4, 4-.. -t -t- t- ; I : -1. 1 I I jh 4!! _, -A ..... I . I I .. j , ,: + 4 .--- +_ _":_4..._. - . '4 _,__:__ ;t_, 4 4--. 4 . I , :N i i I i ii- . I I i I I . I L I - j : - , 1 3 0 84 1 - , -. I-, I ,-- . j 1._.; 1 !L. . , ::I . : .. I I . ! I 4I -- i -I __I 1 1 - , I : 4 4 IL. I-. i, !.I , .II'll 4.i 4 " i 1'.i 1-. ,11-.1 -_ ;;; i L L ,!,; I . 17,... .- ".,_14 - - -- , I __I -- , .. ,, I I " - f ; T !I 1 : : I I ! I ! ; I . I I 1 1 i , - 77T,lii ; -4-, ; ; ; : i i: . i ; . I , I , - Lj j . I . .. , - , - ." ...... -- I . I . _' I, ; : I . I !Ili : I ;_-r - I! . I I ; , I I , I I ! i I ! I i , i , I I I I I i 11M ;- - , +_____ - q T-7 - I I I . , p : I LIA-1I 1 ,;:, :,.i . I I I I I .1 I .I i I : ji t il',' I T__ , ) , ' . I, 1I , ,! ...., ..., , I? , ,.... "I I i I .1T Tt1i il-tt'l I .,Tl "i ;i rTI ,.*1 , , ! __- _,.___.. +.. I1 1.1- !..- jL4A I I ' - . , - I . . 11 I .. L 1 L d d L I I .. -1-4-111- .1 1 i - ,,-,I- , i. ! 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I . ,I I +1-- - - , + . , __ 7, I ! : : I : I .. I .. I . . . - , - i : I' _ .", P - + , 1 4 1 I I . ---- r . . -- -I.- 441 -4I .. !--' . ; , - -. -- I , : d , I ; ; , 4 : 4 1 4 , : . i L ! . f I . ! . __ . I I .I I _ _.. _ir 4 4*o -114 i + I . 1. : - - -- I t;IIIII : . I ...... 30 13 1__'______,___ _, _, * '-+*- , I i, :. _' .-I ' ...-.-- - ;' . ;:j L ! T_ I I I I : .: ::!. .I 1. .' : __+ T , I - --- __ I , : ; . ;; , " -4 v . I - 4 I , 4 I I I : I I ; I i i , i4 I.. ; I I 1 . I .- j .. I 11 I - 7 ,if , _ 11 , I ;I I I .I f. .! -;. : _ , t - t + . - , - TT_ , , . 7 1 . . . .-I . d ..-:I .; llf i I i 144* _ : . : I I .. I . I I . I I - . - I I I I . I . iI I I I ., ! .. - If I I L . I , 1 ii : , , f'. i- -- :1 ! I I I I i,-l 4 Ir- T I litii, . I . . - - I . ; ; 1 l ; i t I -f- ; , i ! : i i t;.,jjl:j ; I !, , - i : , , I : I : .: ; L, f , ' : -; ' I - I !. A- 111 i . illi- i k I I . , , " , : ,.! , '., I , L I I : i i i I .+ _...... t + -- , - q i + " 'I , . I ; , .. I4 -:-,. I -; * J.. 'L 11 . i .- . , . 4 4 - I + t'l j L,I I I I . I - - - i _ I, fI , ! ! L .- I W - -- 11. _-L-r.ff L j . , a _',_ - ., ! : . q, , t L Ii I , , - 1 , , I - - -j I ' " t. _4 lt ! ; I j 1 1 1 .. . I , I .... I ; I 1 - i '. L I i I . I i ; I ,,, : I I . q i I I I . ; I l j . . , , 7 i ;, , I I . , I i - , -11 1 11 I IIt

I I - ., I I - , I ...... As mentioned earlier Nd 4303 has a conflict with an iron line

at about that same wavelength (see Table I)# In order to remove

that part of the intensity of this lino due to iron, the follow- ing procedure was followed.

A samiple containing a mixture of ferric oxide and quartza was

arced, Then the ratio of the intensities of Fe 4303 to Pe 4383 was calculated. Since the F 4383 intensity was known for each

sample, it then became theoretically possible to coalulate how much of the intensity of the line at 4303 was due to iron. This value was then in each case subtracted from the measured intensity, theoretically leaving just the intensity due to the neodymium present.

In all cases except two this procedure gave positive intensity values, which are meaningful. However, in the ases of samples

3013 and 3138, negative intensity values resulted, This certainly indicates that these samples were quite low in neodymium relative to the other samples, and it has been assumed in this study that they were also low in absolute concentration. The negative in-- tensity values, which have no real meaning, do indicate that there is some sort of an inaccuracy in the correction factor used. It would seem that there has been some overcorreotion to give these negative values. Thus it is probable that all the samples have been somewhat overoorrected# Since most of the samples already have high neodymium values, the elimination of this overcorrect ion would simply increase the peaks for this element seen in the sample plots. In the cases of samples 3014, 3061, 306?, 3082 and 3085, + If ". - I.- , I.I + ' , .;.119- --.. "I ' , " f.-t .I t- . -t . , i . . 6. -- - +--

. LIO. 1 VV& I? -1 "O '2 I

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I . .. 44--l" _."-- -- - r - , _,-L, , ". - L L_. - -_' , - 44 I, , I , Ir r I r _ :Ii ; ; ' I 1 ' .I 't L 1 ,': ";T __" r 6 1 1 . . -t - , -- -- -,--- T , t 4'It,' -' 4, -i , %1,i ' ' ' ' 1' +-' - - i ' ' '. I : ; r :I j : ,7; , ' I : l 1 : 7 r I I : I I I 6 i I l, ,.II i , . : I , ! : II : ; , I. : I Ii ; , : ' -_-. - ' I , ,r I I - I _II i i ; , I1; I; t- I I ;i ;i I;tI i II , I. 1 - , I j I i I II ; II , : i , , 1 11 i , , 1 I I , I ; :j l , I I LI . l .. I : ! , I II 1 j I , ; I , I t I r j I i I I i i 'j; I r I I , ; I ;I I I ,1 1 I .. r Ili :I I II : I .I t : OUI I I I I I I I . i _ _ . , I , ; r . : ; j - r r r "I I ir II I II I ' i I ' I 4 ' ' , Y : ; ;I I i I ' j ! : i p I I L . I I . ! ! ; i 1; , t I , 1 ' I ' L f : t , r , I I .I . ; i , 1 i i i I , i . t -i I I I , r , I I , , , I i p i I . I r . 1 T i I I j I , , , : ; i ; ; :; 1I I , i I I i I ; i ,II ! I I I I I . i , i II I i I I I i I Ir , I I 1 ; ; Il ! ..: : I. I : 1 1 , i- r t T: I 1: I ..! ; 1: ' l ' i : L .. II 11 1 ; ' ; , 1; Ii I ; I I I 6 - If : . , i , ; : , r ! , ,I : 1 I I : : I ! , I r I 1 1 ! 1 , , ; I f ! i I i 11 i , . : : ! i I : : I I I I I 1!1 ! I f , ! I I ; .. Ili i 11I i i i I I I I i I I 1 ' l ;1 ! ! ' ! .I 1 11 11 i 1 . I , I ! . . t ! . ; ; I I I . t i I l , I 1 1I i ; I N N , , I I II I I I ; 11 1 1 1 i .. I I i i i I I ! ! 'II i I I I I ; ! ! ! i i ! i I II I ii I I ' , ! . LL 11 -t I i 1 1I I I i, r . i I -- 1 i I I 1 I : L; : , . j I I I 1 i I i . I i . . , , , . , , , ' , , , I I . I . I . I ; ! I I I ; I ! ! i Li ; I I I 4 i I , . '; i i i I i 1; :__ ! ! I I : . I I . i I ! I : ; ! i I I ; i 11 I ! I i : i 1 11 1 1 I I I I1 1 I I ; t , j T Till I : ; , , I IT IT I TI I;I I I I II .l , - - I 1I 11 i j.. 'I" 4 i i j : ' 11 . , ! l!; : I , ! 1 3: I ; . ! ! ! , ! -t - ! i I I 1 !! I I I 4- . - I I 1 I 44 i I I I : -T ; : ! +._ II , I1 !I ! ! ! T i I I I ! i I ;;, I iil:!i! ! I I I I I .:H ; I I .' , I I . -i- -44 - . : I , -- ;;7 ; I; -. I ;.;. ; 7 . : I T I - I I . .. +."+.- .. I I -o i I I +. . - .. ;; T . I :i f i T ; i I ; ...I + I I . I . I ..I71 : : I I :: :.i I ! , I i , , ' , ! . , . : ; , , , i , i i i. . I i ,,i I t I i , I ...: ; I , I [ .' I I I I I I . I . I I : I : I I 1 . , . I i I o : I l I . . 11I i : -i I ; I i : .- i 1 . ; i l , : . ; ii 1 1 1 - i ; t 4 1 I i ! i I I i i I I I i I !' 1. 1 i 1: : : i I i ,: 1: 1; 11 I i ; i , j i; I I ; : f ! . .I . I ; : . I 1 , ! ! ! 1" ,: I I I I I .. !I . i: I I J I I ! I I I I i I it I ! I i I , , I I I i I ! li! I M ! , : : ;1 : : I . I I I I I I I I t I I , ; ! ! : I : 1 i 1 . .. - ...... _1 I ! I - + - * - + - 1 +- I + . t I : - - - I t t .i ",ILI ILL I I I I I i I i i . I II ! . . ; , i i i * 4 , , - , I T ; I , r , 1I +_ 4 +4 ' i ! ! ! - - 1 __ 4 4 4 4 1 - 1I; .it_" 4+_ : 1 +-4-+ -+-4 : f I I i I .. , . 4" __ -' -. 111 ... 1 ..... ' + A + - - . r 4 11 . ,+It -_ ++- -t; ; ' " - ',,"' T - ., - - , 7: I. 1 - + I 44 r IT- I - -, ._ . 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I _ + ' 1 -t t - 4 --- . - + , - - I "- . , -- - ;- 'i

_ __ ' i 'L - I I ...I I , .. . _ - - . .- " - - _+- - , . - Li -' -T_ -- 4-- I -__ , ' I I I : I , . I in 'tI - ,N ' In , N ~~ ~ ~ ~ - ) r ID - III. I .~ (9) III - 0) m r, ID in I 0) //Of I-

i I ., ;l r ; ; 1 if_ ' 'rf ' 1 , ' + 4 ' ' ' 4 i44 ' I 164"" lm" -1 , , -, -- ; 4 ; -- , 4- - - iw i-r-4- neodymium, while reasonably high, does not constitute a peak, but

might become a peak value in these sample plots if not overcom-

pensated. Thie would eliminate one of the more common discrepancies

noted in the discussion of results by samples, However, both 3013

and 3138 would still be low in neodymium relatively speaking,

10. Samarium: Samarium (graph 7) wae found to be present in all san-

plea and varies from ap proximately 1000 to almost 10,000 ppm. In all except two or three eases, the concentrations of samarium and

gadolinium (graph 8) parallel each other. In addition to the gen-

eral parallelism observed in graphs 7 and 8, one notices that the

actual conentrations of each of the elements are in many oases

similar numerically.

11. Gadolinium: Gadolinium (graph 8), like samarium, was present in

all samples and varies over a range of 1100 ppm to about 6000 ppm#

12. Scandium: Scandium (graph 9) was not detected in seven of the

samples. It is estimated that the concentration of scandium in

these samples is 75 ppm or less. A trace amount of scandium was

detected in three other samples and are tabulated as having values

near 100 ppm. The remaining samples have values varying from 130 to almost 980 ppm.

13, Tungsten: Tungsten was detected in only two samples, The non- detection is estimated as indicating that lese than 200 ppm of

the element is present in the sample.

Semi-quantitative estimates have been made for strontium and aluminum. The strontium estimates were made using line Sr 4215.5 and the aluminum estimates were made from line Al 3961.5. Sample 3069 has an estimated P30)-4a 0a Wa m N~ CD (J01D .4 0 01 j T o

- - -; -4 n - 22I2~27~7- t-4 +4 -4, AL4 - -+- - a.

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~3I~7~4 7-4f- 4~ --- -+4~4 ~ -+ 44 ~4r4--"~ - ~-~-~-.-. 4 h4

3051 - - -t , -- ~ ~~ - + 9.- 3i'4O~ uTa --- + H++- I 7 - .- t4 -- T-4.- _ _ Z tT Ti T.2 21V~rrn -tt? - .. -+- --- -.. % i~ L+ 4 ..- ' 3 - . -- T_7 T - - tt - _14_ -4 -4_

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4 tt t' t

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ink.-tIll.- 11 t1l, a -7 im ft CoCent ia /oi in 2600 ppm of strontium and sample 3139 an estimated 1200 ppm, None of the other samples showed any detectable strontium. A. of the samples eon- tained aluminua, estimated to be present in quantities of 10,000 to 20,QQ ppm in each sample. Diaoussion of Results Q Sample In this presentation and discussion of the date by samples, I am attempting to determine by trace element analysis if any of the sphenes might be from genetically related rooks. Reasonable evidence of genetic similarity or relationship between two sphenes and also presumably between the two rock sources from which they were separated, is taken to be a parallel relationship between the plots of the concentration of the ele- ments in each of the two samples. It seems reasonable to expect that two

*phenes from genetically related rocks would illustrate similar relations between elements. It seems well to point out here that there may not always be complete agreement or similarity due to the errors involved in the determinations, but that a general similarity is necessary. If two samples have nearly the same concentration of the elements, one might suspect they came from not only from genetically related sources, but that the sources were also in close geographical proximity,

The samples are discussed by groups erranged on the basis of the author's impression of significant similarity end relationship, The only relationship among the samplesof the last group is that they have little or no similarity to any other samples in the author's opinion,

In the first group are samples 3011, 3014, 3051, 3055, 3058, 3060,

3061, 3062, 3063, 3071, 5079, 3080, and 3139. In general these samples have high peak concentrations in yttrium, iron, neodymium, samarium, and gadolinium. Samarium is usually higher than gadolinium. These samples also have minimum values for scanuium, lanthanum, dhromium and tungsten.

Cerium is often nearly as low as lanthanum. Closer similarity between some of the semples than between others was noted within the group. The - o-, ------,. - It . I I I . I ! , - t 4." .- ,- - . .- . - -- --. I . ------. 4 t 1, I I In fill 4 1j. V1 N 1 - N UP 41 ui W1 14 W W - I rv w 43- ul V) li, IL - rj , w #- I, V - w -- . 1= I . I I I i I , - ,:: ; : i i . I I : , I , , I , 1, i -1, TI , , , , [ I : 1I ! I I , i I , m , i t I -- ,--- -. +I ------,-+ -- - 4,4',,i t I , I , , j , I ''I I I I I I'll, - - - - I - - "- *.r" ------4- -+.. ! 1 1, - +... -4 - 4. - -- -- . : :, , I : . -- + - Il -r , 4-- i.- I, - T------i- -I, 1 . I l! tii; ''! : , f ; ; "I I 11; I i 1 1;, ; t i .4p 1 , ".4 ,; , :Idii1- 1 .Lk --oil -!- if., io 11; . ! i ! I , I t I .II, ii I! Ii H -11,.; I . : I .. 1. I'! ;- . A l 1, ! I ,.'! : , - - -1- IITT I ! , ! , I I I ! : : ; I - , r : ; ,,- - - - ... - : I I I t ---- - I I- ! , '' 4 1 , , "I'll", -t -- - 4+;+ - , .. = :t IT: I I , I I -- -. - r 'Idif - 4- I I 11 i rr L r I . I ,"I , -4- - I -- + - , -fI- .r- -- -- 4-4--1 +, - 4 . -1 " --- ,I I I - t- 4 -+r t-1 - I...... z l : i 1 i f i 1 i 1 1 I I ,, r : " I ; I r- t I 1 -4i ! 1 , - f t , , I I I rr 4444I I I I --r------I : Ii .- .! -1.." - .---I-- - +-..-+-' I - -r" -. i 4-- I .. I - : ; I i I : i . 'I ;,li'l! i .. L - I- . 4 .- +- , ;, T,t --- L- .. , I r - ! f, , II I , , , I i II ; !I L/ I y .11-- - ; Ir j: fI i i, - o 4 -+-.o.-- .." , I , ; I , , - 1 ; : , . i I p ll ! I i I: 1 ; I . I, ', I ,. , ! Irij 'I , , 't r I : . . +1, . 1 5 illoi I I : I : , ; i I I I ,. I ., I , , ; II I I I Ilil. l-JII I! i I II I I1I -- I A I .... ! I ; L I . I I I I i I. r I j I 1 1l -i : : I, I;I I. . ,--1 .1 7 I I - I I I I - I i4o. I , . , , II I ; I I I I I ,4 ! : -1 1 I I I I ------Ir- -'- . I I i I I , i I 11, : tttI :::: . I i I , r I - I ., , I I I I i j , ! , . I "I .. I 11 .....I -- i -,-,. - 1 ! , 1 4 +4 i I I - -,-+-- .. ' --- - W+ I I .. I : i : . I I "-+. I : I I I I ; I , -- 1 4 I I ; 1 oI f------1 1 . - , I I 11 .. I ,r I I 11 . I I . - -> - f------.,- _o_ I -' ' 4-, 1 I -- - -- +-- 4- -- -444 +14 j . I I I, I - - +4 +4 -- r " i & , . I I I -. . -;Ti- I I I , r , , ,- I . 4 1 - 4 , 1I I I II .. I -- 4- --- , * I I 1 I I I.: I . : I l i . __;wt; I I .i-.4 1 I , ., I, ! ; i I r I I r j Ir ... I I; 1 . : t I ; 11 : i , . -.--- o-- tI 1 1 11 1 ; , I. ! , II : :: " + - ., iL-IL 1.I - . .... 4 - i ! I I .. i ; I i I : i , .'.11 - , ! 4 -- "- , ,'+ .-,* ," I 1.-+-o---. -+-4. I- - i :: .. I H.-I I 1; - 1. A .:: i 'I I.:IfT , i 1. i 1 I : i ii ; :4 i I I ;i , - "., . l ! I '' -- - -L--. -, - ' ! I ;;I -Lil I - , ' . , , I 1111,; - -- 4-4 - +I --- ,- - + -- -- ," I i ii + : 11"Ii'. "I + I, r 11 - ! -= ",',""I'll", II I i1 I f T ,A I I -1I-, , 4-1 it : I - -tw +--t 1 1 I - , , - I I : : j , , T 1 i 4 I i i i +41, , I!;rj ! ;i! : ;j I : -', - I 1 c I ! ! - .. .: : I , -t- I i 4 , I f , , ;, j , , r I : ! I ! ! i 1:: , I II I. .. . !I :jjI I TI :1 11; I a 1 I ; , , ., . i i i i I 1 , - ; ; I I I , I I i I II , I I I , , I I I I 1; ! : N l I I I I I ; 1I I , I ; ; I; : I1 ; : , ! I ; : ! ; 11! , , i A; : I I I I I . I i i I I , ! , I I I I I I I I I 11I.N 1 I : ; -- - I I I I --, II ..4 + , I i ; - 4-i4+4 1 1+ -, I i I I ... . , 11 I , i ,I: "t - I ; -, ------r -+ --;- L . I ., I . ' r , , I ... - . "I Ir --+, - ! , , I--- - -t - A t ; I ! I .! ! 1; - - ! . , ,, ! - -- , , 1.4 1 . r . If I ----;I - I -.: I ; : -1I : ; :I I! ; - 1."i I "II- r I I , -. - .--- - I I , - . I , i I .1 11, I && -- ; ; i: I-+ I I I 11

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I4,-*4 , ..- 4 I- - H-4+ . I- I,+' -- ! -. 4-1--. 1-, 4-- 4 -- -. t--+.- . !.;!I -444- o: I., :ii ki :If;!! I I -I I -" -+- 1: , I ; ; - I , ' r 1.; 1 qj . 11 1 :I I II I I f - i ;I :1 ! i I , W 7-, I' : ,I L' . I t - I I I ;.1 - I L, i i II I ;i 1 ! I; I :1 i i 1I I I L I,' L ,' Ii I , - 1 ' I 1 1 1I-t. II I I I .- - ' . .'' , L , , ...-H I . I . ...-I "I1 i ,1 I ,1 1 11 1 ! , 1 1 1 ! 12 1 I i 1 1 1 Ii 1a I1 4 I 1i ii , I J L , i I 0 ; i 1, 114 I I , I I 1i 1 i I 1 1 j ! j j :I II, . I I 11I ; I 1 II I1;II; I 1; ,I I i I I . , ,;, , I ' .. ! . I ; i i ; 1 ; v I i i i 7 , 4 I i I.. ; I ; ;T II bI . I : ! I ! ! .. % 4 1 4 I -- - I I -! I - 1 9 : : I . r . I I . . ., , . . r , , . , T . I , , . r , . . r. i . -+- I r - , - . . I I 9 IT I !!! I IJ i 1 ; i ; i ;i! ! I; ; . I o , , L I I r ' t , ; . l , . , , : . : , I 1 . I . I I I I I I I , I . .. I I I I .. ! z I : ---t L L I I L .LI L r .-F IFT-.I -F:I -,,-! : I'IL -, ' ' I ' ' : .:I -11 ..I , I - I . ! I I I . .111 .1 -- I 111'11 !!il"2 ; ,7, !! ,I 11 ! v , I ' I I i11 -r-- I 7 , , . i ! :I : I 1:i!::Ollf7:: K 1!I Ajl l ! , , ; I I I - r-?- 1i f 1 !I, ;!I I ! I If ! I -,, !! !! 'i L ' ;l:k' 1 : . J ..... , , I ... I I I !;j -- -- I -,, -1 , - --I - '' + .-, I , -- , . - - ' I , , , 1 1 ! .! + ; i 11 ! . I , I , : !I !. i !::,Jill!. . ii! i W l: i L ! I I, 1 -- 1 -, . -= -,-U I , -.- I. 1 - f-- ! -- - - - _ _ -.- - 4 1 ------. .- . I . ' L: . II I 1 1. ------i : I 1 : ; ! i I 1I . .--!, ! !- -I .. . --- I 1 ; , I ! II I . tI I I I III I I ; .I !! I , iI I . I L I . ; . I ; 1 11 i Ll .'" I - - I+ L - , I --- I-- - I I i I -1 ; I.L . I 1 , ; I , I ',_j , L 'L;I : . I ll - , I - , - , - * , -- . II I .I .- , - , rI , II L , I.j I L ;' I , I.; 1 j 4 LLL ----. . I I ! I f I I I ' ------ro -- .- , . + - . , -- -I -- , . , , ., .. ; . *1 ; -I " I . I4 1I ; ;i- i ; 1I r r... , . I : I I i 1 , II i I 6 I - 1111 11 I b I k. - I, ! ' ;L ! : l: : iI !I :.I I I ; ; i i : ; I I : ; : I ') : : ; I ' 11 ! I : 1 : : ; ; : .1. :4, ; i i ; i ; : ; I I L t - , : 11 4 , I : I j 1 ' : ! : 1 I ! i I ! ! 1: i : :i : : I I . , i ; ! i ! 1 1 . I . I I I ! ; i I : ; I I L ; : I I 1 i ; 1 : : : : f I ; I I : i : ; I -- " , ., I , ; I I I I : b- I . , I I I j I . 1 7 % L I 0-11hol, I i - i , I II I - +14 I I I I I i , ; i , -; - i I ; I , i , , , I I . I -I I , . I I I I .. I . I I , ; ; i , . , , ; -1 . - , - ; 1 ---; - , I - I . - ---I i : i -T--- ' -rI +,* * _:-L.- I - z ! ! i , ; ! 1i I ; 1! I I :!I! : I Ir I! : r i 4 r Fj I !_ 'I 1 1 I I II ; 1; I I; !I! -tL ;; , -!, II1 -" 1 1 ! 1 i I ! : ; ! i ; I T I . I; ; -+ +i+ I I I ! I I 1l ! i 11IT I i I I I; I II I I :; I II i i ; i I ! + I 1. - --- i . I I - rt .I 4 r -f---+-. I--_I__t -,_+r f_ -'t-++ -ti+ *1 + - , . - -4-1-1--+-1-t-I 4 -o 1-fT4 - tH , t 4H I IT+11 -, . T I -- -I --.-I - I I, - ! .. 1-, : -Ir I" T .+, I; I; i ; 11 .f f i , - , i- -+- -+ -- 4 -4 -+-t I t .i II I ;1 11 If I , , I --" 1, - ; i I ; r I I ! ; I I , it.-0- 4 ! ! I I I I , ! ' I ,! ILI II I r lIf 11 I "I I H i ! r : "I , r r 6 .... I I I ; i I , I , t I iI .. ' I 11-"IT ' I !!! 11 .. TI + _ .4 1 1 1 .I I _ A : ! -- -t-t--t- t -++-ti-+. b I . I .. ---- ...... ------I . I I ...... I - I I i I I - I I I ! bbb I I T- 4-+ , ! ! ! - ., - . : I 11 - ii ia! 1 1! ; . . I I I 1: , I ; , L -. I I I I I ; .I o1 I. I I I I I 1 I I 7- . .4.-+ - , ; L ' ;;;; . I .....I'll, r ' : I ' , - I I ! I I I I i : !-.- I I I I I ! I I : I -- - .1 ; - ' 7 I I . I I i I I ; : i 7 . I I ) I , I , . . . I L k! : I i I ,-" : I ; , 1,* -, ; ; , I i ; I I I . I . 1 Li i ; I ; . , I . .I I ! I . I , I ! : ! : I : . I I I iI .4.1111, I I I - -i -, I :,04 , , I * ff . : . I . L . + i ;! 1 I 5; I r: 0 L i , I I . I : II I 7 : I : I ...... , - , I r I r I . , . I I . a 4 0 , . . I I ' 'I I 1111111111 "I'll fiff 4 I , ; I i I II I ; ,I 1I - 1 -- r ' . L I I . I I I . : _ - I I _, . - dI , 4 " I I I I I i I y : b I I .114-- rT-,77I I I I 14- + 1-1-- -t- -4 4- +-4-4- 4- - i -4- 44 4 i I T-If I i I . I ! I I . I I I 1 I I I . . ! i ! I I I ! I I . I , I i I I I . I ;I I I I T I , , : : : i , : ;; I ; T1 ! -4I A4- 4- - 4 + + 4-p,-f +4L4 I+- I4 " I , ; I I I t.- t r , , I I , I , ! ; , : I ; I q , : To i I I ; I I -;I;,. -- 4 - -- . I I I . I I I I I I . I I b . ! : 1: ; : .. IL I . ; Ib t I- ! ;1 I i III I1 I ; i I I . I , I , I .I- -4- I II I 1: I: . ! , I I1 : , 1 : , : ! ! I I ! I ; I .. I I I I I I ! ! LI , 4 I I I I1 , I , I , I ...I ...L .. j I I , 1 1-4-4 T ; i . I I I I I I f T-,r ! ; 1I ! I i I 1 t I , ! i I I I I I ; I i I i I i I1 1 1 ! f 1 If 41 r . , , . , -T *-r- I I I ! 1I .1 ! , I1 I 1 .1 1 i ,I I I. 1 1, I I! 1 L 11 1 i I . ;. ; I I I I i I I ! f I i r I: ! : ! ; . i : 4 ; l ..11i I r-,-+-,+r I i "' , l I I 1 i 11 I I 1 -I I - r - , - , I i IN I i 1 + +--I+ I , 1 . , I , . I I : : I i i f I I 1 I I -+- -- I I i -it - I Ilit4l I .I I I I I ! I I . , , 1 to I : I . I ! I f I I I II I I , - I I I I . I .....' r : . I I , I I I I I:: I, II Ir i i r , ;b ; i I T : ;; Ii1 ; I; i; ! II I I I I ! ': I I II b : 1 , ! I ! I I - : 1 I, If- I I I , : I I t -1I : I! ' I : , ! !! I : -i ;! i. i I I I - , , rrrrrr L I ;I t : I ; I ; I . I r ",;I I ! i1 !I ,i ;i iI I -t --4 i 4to 1I I I i ; I; I I1 1i ;- "!if !I , I 1 i i I I;I I I i;; ; ii 1 i II I II , I it I - . I,j L III II ;I I I j J1 I11 I I i T I I I b r , ,!: I I , I I ! i;i !It Ii I; I , 4 I i . I . L I I I . I - I 1 I z 1 , !!; I I if .T :: !I7 1; I t -- . ------I .-. -t- i 4 , . 1 4 I L------I -4.--0 I I - - I -- I ------, , I L . I b 4 -- - t4 I . -- L -l L , , I Ij L ; L I I , 4 L , ; t , , , I I ! I I I I ! It II 1 f I I 1i I I1 , 1 II I I i ! . ; f 1; ; I I , I I r i 1! II I I I , 4 i I; ; 1 1 i : I : I . II I I I I I -- .- --I , : i I , ... L. 717! -- , -" 1 t - , i !i i ii : I , II I ,I 1 1 , i . 11 -.... + :- 4 I I - -- l .j- I I I . ; . 7, rr + I . I 114, I I . , , I; I r I . 4 4 . I I ; . ; p I q : . : : i : I I . : I i ; ; . I ;! 44 1 i4 - -4- ! ! ! , I ; I I I L . I , : : . , I: I i , : ; - -4 I .... I I , . ,. . , ! I 4 I I ...... , I : I 11I ! I - I ! I it ! :: I , -- -t -" 4 L -- - 4 - I -;--7;::::; 4 11,I - - -- r -T- , - I I - - " ,--, .- f . " t + ! , 1''. +,t..f --I-4 ,1 IT.-! I *, I " II -- m I 11111511111..... z I I I , I I ,; I I I if!, I![! -H I- t I L . I I I 11 -I- I , I ; :l, . 1 " j'' ! I . . , . I :: 1 , 1;;;:!i:4 I : ; : . I .1 !t + ++ . I I . .- ,,, ., 1 .; I :::I 1 i ! . , 1 1 i . ; I .: -;m4 --111 -i- , ! , I i . II .. I I . I I ! L - L . LL i ;4 I i L . I It I T k I - I i I -, , .- , i I I I ,L I ; . . ! , I .L , , , , I .i I . ...''. :- I : , . 1 ' )I ' '!: I om 1 7, 1 1 1 .. : : : ; ; ! ! i],!:!1:; ! Ii- ...... I I .I .j J1 11 .i 11 i 1 1 1111 : I I T 9 I I I 1 T ; t- . 4 ! ;; I + I ' : "4, j,*.r:;= . , r . b . I I , 1b : , I LL i r I i : : . r , , - , . 1 T I . ': ! i I . I r : I . ! : I I . . 71, :Ii-M 6 1 : I : ! ; 7 1 I b I I r I , L I . , I . i . :: i : ; I . ; ; ; i ; ; . I 1 . , - ! : ! ! : ; I ; ; ; :: : : l I - - I 7 I ; I . .I ! . . ! , * I I I I I r ; j I LI I I L ; : ...... * 1 i ! , 1 1 - I I I I I I I i I I I 1 * t i+ -1, t4- - .. I I 6 b I .. L : ! L I I i - - I I . I L I I I I I I ; I i 4 1 1 ; I : 4 6 i -44444- ' i of;if - L L -- ..-- -- I b ! r , ! -- . . ; + +-I I - . I I . ! I .. I d d + d - , . ' ' ' I , L . ., I .: I I I I . .. I . " ; I .- I: I I ; , ! , I -- 4 - - - .- , , " , . --- I - -,j- 4 -r-,!. ,- I ' ' ' L. _ I 1 . +- - b, - ,T+ 4 .4 . - r -4 -- ,-- -- -1 - -+ -- , ! - - - - ... r . --t 1,I ! I . b. I + . I I ; i - ' I I ; . . Ii,4 ; . I, ; , I I ; : 1 1 ; I i ; I , .. t-*-- - I i 11 , ,, ... , t . j1 1 1 I . , I I , , j , I I , , . ; . I , !------i.--4-- - . 4-4- 7, 1 -" *" r 4 . " -i-- " 4 I r +-I- I 4-+ - - -- 1 ! ! +- 4*44,- .... ;; ;': .I 1. . T T- T- T - - ---.- I . II I - .1 ... d, I . . i t . I I I I . i L .. : I i d -- -- II I : I : I I i I . , i . , - . I , ! , ' ; 1 L I L : j ! I ' . ' + ! : I i ' : " . . ! ! I . I . I ; :I I :: I I q I I I I ; , : I i--- 1 4 im: 644 I -4,."4 .-. -- t-- .-- -,-- I 1 - i i I i I , I ---- - ! ! - -"4 - * - L , . "-1-4I ; I , I : I : I L , L 1 i , - ; ..r ; %3, r . I I I I I L : , I . , ; . , . I I I L I I I ' I , j . I : , I . . 11 , I b L I I I ." ! : : j : ; 1; : ; , I II I , ; :; : : I , : I I I 1 i I ; t ; I . i I i I I I I . I I I ; i ... . i . I I I ; I : 1 : . , : ; I : ..! I I - , . I I ' I I L . 7.... I ... I .. r I . b , . : I . : . , . j. IL I r. .j I I . ; , ! I . , !, , ; j r : I t ; :; I !I .... I I + ' ; I ; ; : * . I T ; i ! .. I I . : I I i . I , 4 , ," 4 4U411ai 111 L 1.,Lm,4.. f4f : 1 , t I, 4-,-,!I I , I I I i , I I : I I; ; I I . I I I i , I : ; , : I I I I I ;! -I I ! i;i I 7 : : * , I 1 - Z ; .6 , ; j b : L , ,I : : ! ;-,A ... ! i'11, - - I I ; I ,,it . v I I ; ! " 4 ; I ' I Z - -1-+ , -- -j- - , r -4 -I4. 'j. U - 4 , - -- . 777 7. - -1- I! , II , t II :1. I j . ; , .P : r .Of: . t .I I - A - " - 4 I - -, - i' . I ., I I : i i ; j : , I ;: I -1 -L-4-4 .! I q ! r 4 L I , I , ! L , , , I -, : I , i I ...I I I I -74 -4 t ; I I ; I I . , 1: i I I I : ; ; : I I ' r + ,, r4f I . I : . r i r i , I . 4 r 1 LL L !- t - I -- +1 1 Ii W ,4 L + , - , - _j 4 .+ 44_ - 4 4 j444+ r . 4 : :tqi +H'f--+ . L ... I I 4 I ! t t- T : i I +1 .4 16- ++ + . +- I + I j '4 " 4 ,4-4- I +4 , , + i-t 1- I i --H -H+ 41 .,I - 1 -I I 4 I : 1 .. , -f- 4 ;;-.l .. , I 4iw-- I I i .... I ...... , , - I I'!" ,I I i ; L I I It 1: , i; ..,,I . q IL ; t4 I , i , , II I ; , -- T 'T++. - % - -- 9 I I , , ;;;; I 0 7 i , " " 4 ! r - I 4f - 44 . , r r I I 4iw . - , i ; rJ4 - , I ; -. r . I -. + - I . : I a " +-,i-"4-1+ = = I , , .. I : T I I , -" i L I I i ! : i I : ! ! I : i ! 1 1 11 L I I T;L . a . 4 1 a: I -1 -. -- I I I ! , , : I- l I 11 I : I I I ;, I - 7t I . , , , . , ;, I , : A I ; I T I T i l : II TI 4 i , i .1 4 4 ! ; : - : , ;,i1 :i , I ;; ; I:tj4L f ,; i i 4 4 , ------.--.-j Ii;- . i j , i ; I I of4"4-, - .. . . I ; I I .. ;j . 1 ; . I I . ; -tf . I 1 , , ' ' L' ' .. d . , I , j r , I . r ; ! 7 , - T I i I i I w ,--4 i 1 ; ; 1. I I I I I I I I I II I II - I I I I I T 11 I I A I 1 I I & i 0 1 1 0 1 1 1 r o14+O+ I i ! I i 1 1 " LLL"I . L , r-- - . I . 7 i i I . , b ..I .... : , d, '4+ - - - I . - - -. " " +Ht1v If t IT t 7 o-tt" I I --- - - , , I.- . L - I I + I . I I .I . Ld .. I , , L I 1 I , . r TI "' I . I I . d . I L : i ! - 7 T I T , , I I I I , . .. 'I L 1 ,, , 11 I I1 iI * I ; ; I i 44 , I I I I I , TI I I If I . I It -- ! . . " , ' ' - I I I -.- I -- I, I I I . I I I , d , I . i iil -L! . , 1h I " 4 , .- -I- I -L-i - -4 I-1 . r I '1- -14.14I4 . L. .; -L-11 I - -I r" ..1 , I .--I LJ"I-' j '. # ! -"IL! .- L -- - - L ...... I - I , ddI I ' . - d

(1Conceitea.ijoly i4 a c ~r A ep- /4fj//jo samples of this group will be discussed in relation to these apparent

closer similarities within the group primarily for convenience, as it is

felt there is a significant similarity between all of the samples of this

group.

The first subgroup of group one contains samples 3011 and 3055 (graph 10). There appear to be two distinguishing characteristics of these same. plea. First, both have decidedly higher chromium values and decidedly

lower iron values than any of the other samples in this group. Second, the peak concentrations, while agreeing with the general case for the

group as far as elements are concerned, are considerably lower than the

concentrations of the same elements in the rest of the samples of group

one. This Is especially noticeable in the cases of yttrium and iron, In the case of iron both of these samples have less than 10,000 ppm, while the

rest of the samples all have at least 16,000 ppm,

The second subgroup of group one contains samples 3014, 3058, 3071, 3080, and 3139 (graphs 11 and 12), These samples are distinguished from

the other samples except those in subgroup one on the basis of their cerium

values, which are nearly as low as the lanthanum values and in the cases of

3058 and 3139 are somewhat lower. The first subgroup also possesses this

quality. The second subgroup was separated from the first on the observa- tion that in subgroup to the samarium and gadolinium values are in all

cases greater than the values for neodymium, -while in subgroup one the neodymium values are in all cases greater than both the samarium and gadolinium values. Sample 3014 (graph 11) shows a dissimilarity, with a peak concentration for zirconium. Thie, if not a real variation, could be due to too large a zirconium value or too small a neodymium value, It - -- - - I I - I - N) (A) 4 (1 M -j OD(D - N w 4 Lq 0 -4 OD 0 - N W th lill, 1 ., (1) t, 0 0) 'i 'm w 6 1 . : ; . 7 i i ! , . I I I : ; I I ' T , I I L ! : I14 I . I p, , , I ; I ) I t i i . 1 , i 1i ; i t , : j ) !j : , i; , -4- 1I: 1 I . -I , : 1 , , i i , H :1:11 ,: , I i : 1 . -l j 1 ; - ,! I; I . , ; i .; r . --- - I - 4 -r- - .- " + , ti.7 . -- - . -,-- t--f-4-44 i j i 1 ; 4i ! , r 'i . I . ! 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might be due to contamination by some zircon, as we notice from Table 2. that this sample has an estimated nine percent contamination. It should also be noted that the scandium values in aamplea 3014 and 3080 (graph 12) are higher than in most samples of this group,

The third subgroup of group one contains samples 3051, 3060, and 3061

(graph 13). This subgroup differs from the first two in that the cerium values are substantially higher then the lanthanum values. This subgroup differs from the fourth and last subgroup in that the samarium and gadolinium concentrations are substantially larger than the neodymium con- centration. Sample 3061 has an apparent discrepancy in a peak value for zirconium, which may be due in part to contamination. This is not neces- sarily true, as it can be seen from graph 2 that this value for zirconium is in the general range of zirconium values.

The fourth subgroup of group one contains samples 3062, 3063, and 3079

(graph 14). This subgroup differs from the first two, in that it does not have a minima for cerium. It differs from the third subgroup by virtue of the fact that samariua and gadolinium values are lower in each sample than the neodymium value. In the case of sample 3062, the lanthanum value does not show a minima or low point, but was determined to be slightly greater than samarium. This is the only discrepancy within this subgroup, and it can be seen that if this lanthanum value (4000 ppm) were lowered by twenty- five percent this discrepancy would be eliminated. This percent change is not too much greater than the estimated ten to twenty percent possible error. It may well be that this relatively high lanthanum value is due to contamination. The estimated nine percent contamination could conceivably account for an additional 2000 ppm of lanthanm above that normally present --. )...(p......

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The above mentioned observation about the similar quantities of the analysis elements present would seem to indicate that the rocks from which these samples came are very closely related. They may be from the same igneous body.

The second group contains samples 3081, 3082 and 3485 (graph 15).

This group like the first group has peaks for iron, neodymium, samarium and yttrium. There are minimas for chromium, scandium and tungsten. This second group differs from the first group in that the zirconium, neodymium, cerium and lanthanum values all are greater than the gadolinium values for their respective samples, Also the lanthanum is rauch higher relative to samarium in this group than is the case in the first group. Sample 3082 is slightly out of phase by its lack of a peak for neodymium.

The third group contains samples 3067 and 3069 (graph 16). Here again chromium, scandium and tungsten are lov and iron is high. Other general patterns present in the other groups are changed. Cerium and lanthanum, while not attaining peak values, are quite high relatively. They certainly are not low values. Also the samarium concentrations in both oases are significantly lower (about 1000 ppm) than the gadolinium values. It should be noted that these samples show different relations as regards zirconium- neodymium and vanadium-yttrium. However, their general similarity otherwise 4LP CB Ci) ~ (11 O~ 'J~'fl- a) 0 -

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L . ,7; 1 T ; -H I . , . 11 I I ; ' ; r I : ' , - I i I 4; . I I I I I i , . I I I I . i , i 1.; , ; : I I ., :I I. I I I I : : . ;' .. . . , L , tI -, +- : I ill 7 -! I ' 'IT" I I -; ; I i ! I r+ I I i . : ' it IF i .! I ! I I I I ; . !;.' -tl-'.-r I : T ' I 1 ! L 1 r L! I I ; . , , i I 1i I I i -+++4- ' I , I ; ! -, : ; ! ' ! I ; ; ! ' I i I I 1. i f if, I ! . ,j I i I : ! ! ! ! i, ; L r I -- -- I I I . , , . -' - . - -,-r t- - + I - I I I I i ! I I I I ( I ; I I 1 , I ! ,I 4 1 1 -- -- , .- , -, -, - I r-r-r- i I 1 , Ir - -- - - , I ., I I I LLLL r i ; i I : ; t I 11 ii ! It I 1i p - ; : A I 11 , : : ; - : ' i ' 1 i j I I I I i I I I ' I I I I ;

- , T"

Q) 0tco 0)r- 0 n -( 1 11 m N - 0) a) fl- 0 ' M I m - 0) (D r*- 0 if) I M - PR

is quite apparent.

The fourth group contains samples 3084 and 3085 (graph 17). This

group differs in the occurrences of minima within the group of elements

zirconium, noodymiw, cerium, lanthenum, samarium and gadolinium. The lowest value in both samples is found to be thrt for gadolinium. This

value is not overly low in relation to most of the 'bove mentioned ele- ments. The similarity between these two samples could be more striking,

Sample 3084 has peek values for neodymium and vanadium, which 3085 does

not. It would be possible with an adjustment or two for each sample in

group three and group four, to bring the curves of these samples into gen-

eral similarity with the samples of group two. The author, however, sees

no justification or reason for doing so. In samples 3084 and 3085, for

instance, a decrease of 400 to 800 ppm in the samarium concentration would

bring these two samples into similarity with samples 3067 and 3069.

In the fifth group are samples 2093, 3013 and 3138 (graphs 18, 19,

and 20). The samples of this group show no overall similarity either to

each other or to any of the other samples. The zirconium value of nearly

19,000 ppm in sample 3013 is thought to be due in pert to contamination,

This value is about 13,000 ppm higher than the next highest zirconium value, Sample 3013 is also notable for its very low values for neodymium, cerium and lanthanum, Saml 3138 (graph 20) is similar to the samples in group one with one

very striking exception, namely a very low neodymium value. However, it

should also be noted that this sample has an extremely high value for iron, over 51,000 ppm. This is more than 20,000 ppm greater then the next highest

iron value for any of the other samples. " w 4 0 ) Ja)Q-

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41) W - w uj 1- %) U) M V) - 0) CDr- ID tn 14 m

::: , ------It is quite probable that a 'major portion of this value Is due to contamination, estimated to be about twelve percent, a.l of whioh consists of opaque grains. The problai of overaoApensation in the correction of the neodymium line was discussed earlier, However, it is possible that the overoompensation was unduly severe here due to the exceptionally high iron value., It is, of course, impossible to know if 5138 would show any greater similarity to group one if this overcompensation was eliminated. Sumary of. Results and Conclusions

Results indicate that sphenes are generally low (up to several hundred ppm) in ohrorium, scandium and tungsten. Elerients present in the middle range of concentretions from about 1000 to 3500 ppm, include lanthanum, ceritm, gadolirium, samarium, zirconium and vanadium. Present in somewhat higher concentrations are mangenese, yttrium ani neodymium. All the above elements were only occasionally present in quantities greater than a per- cent. Iron values are very much higher then any of the other elements studies, averaging about two percent. This is as might be expected due to the greater geochemical abundance of iron as compared to the other elements.

A portion of this high value for iron doubtless is due to contamination,

Aluminum, while not determined quantitatively, is estimated to be present in the range of one to two percent.

There very definitely appears to be parallelism between the values of lanthanum, cerium and neodymium present in sphene. A sample high in one of these elements is also high in the other two. Samarium and gadolinium also shoi very striking parallelism. These relations are as might be ex- pected from considerations of ionic radii (see Table 5), An inverse re- lation is noted between iron and chromium in cases of highest chromium or lowest iron values. Lanthanum and cerium show an inverse relationship with yttrium.

Of the thirteen samples of group one, chosen as having significant similarities b y the author, eleven are from New England, end two are trom

Quebec. Of the eleven from New Rngland, three are from Massachusetts out of four samples from that state, and eight are from Maine of nine samples from there. The only Maine sample not listed in group one is the standard I low00"

Table 5

Tabulation of Ionic Radii of Certain Elements

Element Valence Radius Element Valance Radius in OA in OA Ca +2 1.06 Ti +4 0.64 Y +3 1.06 Al +3 0.57 La +3 1.22 Cr +3 0.65 Ce +3 1.18 Fe +2 0.83 Nd +3 1.17 Fe +3 0.67 Gd +3 1.11 V +3 0.75 SM +3 1.13 V +4 0.61 Mnn +2 0.91 Mo +4 0.66 Sr +2 1.27 Mo +6 0.62 U +4 1.05 W +4 0.68 Th +4 1.10 Si +4 0.39

(From Appendix Stillwell, 1938 and The Handbook of PThysics and Chemistry) 3085. The locations of the samples eroqpt for 3485, in far western Ontario, ean be seen on the map of sample looalities (figure 4). The samples of group two, 3031, 3082, and 3485 are ell from Onterio. Samples 3081 end 3082 are within ten miles of each other, while 3485 is about eight hundred miles away. Sinilarity is also noted between semples 3067 and 3069, which also show some geographicel proximity. The remainder of the samples show rela- tively little truce element similarity and no geographical relationship.

There thus does appear to be some definite geographical grouping of the samples, with New England being by far the most obvious group. The reason other geographically groupings are not so obvious may well be due to the much fewer number of samxplea from these areas. The grouping of samples by similarity of their plots for the thirteen analysis elements, vould seem to indicate that trace element analysis of sphenes can be used, given enough samples from an area, in correlating rocks that have some genetic and geographical relationship. It is possible that this is due only to the general selective nature of sphenes, selecting the various elements in certain proportions to each other in nearly all cases. It would seem, though, f rom ti fact that only little more than half the samples (group one) show general similarities amongst themselves, while the rest seem to be signifioantly dissimilar from this group, that there is soma genetic relationaship indicated. The author concludes that trace element analysis of aphenes may be helpful in establishing due fact of genetic relationship between rocks. Of course, additional work is necesaary, as will be suggested briefly under recommendations for future work, It is concladed with respect to procedure, that the use of intensity ratios of an analysis element with a similarly behaving element present in ryure 4. p of SaPmpi/e Lo ca/ities nearly constant proportion in additionplcts is quite helpftd. It was

found in this investigation that this intensity ratio in ILost orses ixm-

4 proved the addition plot E,9 making thmr more neerlxy linear and thus making

it easier to

: tatulation of elements and their concentration runges in sphene by various analysts is presented in Pable 6, Table 6

Elements and their Concentration Ranges in Sphene by Various Analysts

(All values given in parts per million) Oxide of 3"Shaa Prince Element Rose Element (1946 ) (1938) (1959)

19p03 0-19,100 9500-61,700 Fe 8250-27,500 FeO 1000-6900 0-10,700

Zro2 500-1100 1100 Zr 500-5900

cr 2 0 3 100-200 Cr 15-635

La 2 03 200-500 La 100-8700 0o 100-8150 Ce203 600-1900 35,800 2203200-9600 Y 740-22,000

Nd20 3 600-800 Nd 500-11,200

Gd 1100-5900 Od203 100-300

SagO3 100-300 Sa 970-9450 MAO 100-800 0-500 Un 620-8550

V205 50-1100 v 130-1160

v 200-750

30203 300 So 75-980

A1203 0-44,400 Al 10,000-20,000

SrO 40-4400 Sr 1200-2600

tNb205 300-16,000

Ta206 100-1?,500

Pr203 0-200 Ob (1)500-10,000

25-1270 Dy205 0-200 U (2)

r205 G-00 Th (2) 40-3150

Yb203 0-100

(1) Taffe (1947) (2) Hurley and Pairbairn (1957) TT - - -1--1 . i...... I ...... I I , 0 1 A ' - - I

Recorennations for ?uture Work

Analysis of the rocks tron shioh z4amples of sphene came for major elents tuld furnis usefufl information. Petrogrcphic stuzdies of the roA and spho would Ulso be helpful if tine and purposes of the study permit. It vould be very helpful in an investigation of the type reported in this thesis to oheek the detemnhat ions of ecl element by a different oethod, ooectlily for thi standardl. Quantitetive deterninations in the ztanaard are the ones needing the iost verification, oince these values are used to determine the values in other samples. The above ouggestions for additional work would furnish greater confidence and reassurance in the result s obtained and thus also in the interpretationsmade.

However, more important purposes wauld be served by analysing ad- ditional aphene samples and establishing greater geographical density of trace elements analyses for the mineral, especiafly in areas from which few aphenes have been analysed. In order to draw any really well based conclusions concerning the topio of this thesis it is necessary to have a statistically significant number of analyses.

Idven more significant and indicative would be a similar trace element analysis of several accessory minerals from each of the rock samples. If several mineral phases indicated that certain rocks appeared to be genetie- ally related, one would be much more confident in his conclusions. 23LiOGURAIy

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