U.S. GEOLOGICAL SURVEY CIRCULAR 957 

Mineralogy and Instrumental 

Neutron Activation Analysis 

of Seven National Bureau of 

Standards and Three Institute 

de Pesquisas T ecnologicas 

Clay Reference Samples 

Mineralogy and Instrumental 

Neutron Activation Analysis 

of Seven National Bureau of 

Standards and Three Institute 

de Pesquisas T ecnoiOgicas 

Clay Reference Samples 

By J.W. Hosterman, F.J. Flanagan, Anne Bragg, 

M.W. Doughten, R.H. Filby, Catherine Grimm, 

J.S. Mee, P.J. Potts, and N.W. Rogers 

U.S. GEOLOGICAL SURVEY CIRCULAR 957 

1987 
DEPARTMENT OF THE INTERIOR 

DONALD PAUL HODEL, Secretary 

U.S. GEOLOGICAL SURVEY 

Dallas L. Peck, Director 

Library of Congress Cataloging In Publication Data 

Mineralogy and instrumental neutron activation analysis of seven National Bureau 

of Standards and three Instituto de Pesquisas Technol6gicas clay reference 

samples. 

(U.S. Geological SuiVey circular ; 957) 

Bibliography: p. 

Supt. of Docs. no.: I 19.4/2:957 

1. Clay-Analysis. 2. Radioactivation analysis. I. Hosterman, John W. (John 

Wallace), 1923- . II. Series. 

TP81l.M48 1987 549'.6 87-600172 

Free on application to the Books and Open-File Reports Section, 

U.S. Geological Survey, Federal Center, Box 25425, Denver, CO 80225 
CONTENTS 

Page 

Abstract . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . 1 

Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 

Geologic setting and location . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2 

Analytical data and homogeneity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3 

Mineralogy. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4 

Trace element contents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8 

Summary .............................................................................. 10 

References cited . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11 

FIGURES 

Page 

FIGURES 1-3. X-ray diffraction traces of: 

TABLE 

1. Flint cia~ NBS-97 and NBS-97b from the Mercer flint clay bed (Pennsylvama) and NBS-97a from the Cheltenham fire clay bed (Missouri) . . . . . . . 5 

2. Plastic clays NBS-98 and NBS-98b from the Oarion coal bed underclay 

(Pennsylvania) and NBS-98a from the Cheltenham fire clay bed 

(Missouri) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6 

3. Three Brazilian clay samples, IPT -28, IPT -32, and IPT -42, and a common 

brick clay, NBS-679, from Maryland . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7 

4-6. Plots showing average rare earth element contents of: 

1. 

2. 

3. 

4. 

5. 

6. 

4. The flint clays normalized to chondritic abundances. . . . . . . . . . . . . . . . . . . . . . . . . 9 

5. The plastic clays normalized to chondritic abundances....................... 10 

6. The miscellaneous clays normalized to chondritic abundances . . . . . . . . . . . . . . . . 11 

TABLES 

[Tables follow References Cited] 

Instrumental neutron activation determinations of elements in NBS-97 by the U.S. 

Geological Survey, 1976 and 1985. 

Instrumental neutron activation determinations of elements in NBS-98 by the U.S. 

Geological Survey, 1976 and 1985. 

Instrumental neutron activation determinations of elements in NBS-97 and NBS-98 

by the Nuclear Radiation Center, Washington State University. 

Instrumental neutron activation determinations of elements in NBS-97b and NBS-98b 

by the U.S. Geological SuiVey. 

Instrumental neutron activation determinations of elements in NBS-97b by the Nuclear 

Radiation Center, Washington State University. 

Instrumental neutron activation determinations of elements in NBS-98b by the Nuclear 

Radiation Center, Washington State University. 

Ill 
7. Instrumental neutron activation determinations of elements in NBS-97b and NBS-98b 

by the Department of Earth Sciences, The Open Univemity. 

8. Instrumental neutron activation determinations of elements in NBS-679 by the U.S. 

Geological Survey. 

9. Instrumental neutron activation determinations of elements in NBS-679 by the 

Nuclear Radiation Center, Washington State Univemity. 

10. Instrumental neutron activation determinations of elements in NBS-679, IPT -28, 

IPT -32, and IPT -42 by the Department of Earth Sciences, The Open 

Univemity. 

11. Instrumental neutron activation determinations of elements in IPT -28 and IPT -32 by 

the U.S. Geological Survey. 

12. Instrumental neutron activation determinations of elements in IPT-28 and IPT-32 by 

the Nuclear Radiation Center, Washington State Univemity. 

13. Instrumental neutron activation determinations of elements in IPT-42 by the U.S. 

Geological Survey. 

14. Instrumental neutron activation determinations of elements in IPT-42 by the Nuclear 

Radiation Center, Washington State Univemity. 

15. Instrumental neutron activation determinations of elements in NBS-97a by the U.S. 

Geological Survey, 1976 and 1985. 

16. Instrumental neutron activation determinations of elements in NBS-98a by the U.S. 

Geological Survey, 1976 and 1985. 

17. Determinations of lithium in clay reference samples by inductively coupled plasma 

spectroscopy and flame atomic absorption spectroscopy by the U.S. Geological 

Survey. 

18. Averages of laboratory means for NBS-97 and NBS-97b. 

19. Averages of laboratory means for NBS-98 and NBS-98b. 

20. Averages of laboratory means for NBS-679 and IPT -28. 

21. Averages of laboratory means for IPT-32 and IPT-42. 

22. Provisional averages for the 10 clay reference samples. 

23. Elemental ratios for averages for the 10 clay reference samples. 

24. Provisional means for samples normalized to the grand mean for an element. 

25. Certified values of the major and minor oxide contents from Certificates of Analysis 

for four NBS and three IPT clay reference samples. 

IV 
Mineralogy and Instrumental Neutron Activation 

Analysis of Seven National Bureau of Standards 

and Three Institute de Pesquisas Tecnol6gicas 

Clay Reference Samples 

ByJ.W. Hosterman,1 F.J. Flanagan, 1 Anne Bragg,2 M.W. Doughten, 1 

R.H. Filby,2 Catherine Grimm,2 J.S. Mee,1 P.J. Potts,3 

andN.W. Rogers3 

Abstract 

The concentrations of 3 oxides and 29 elements in 7 National 

Bureau of Standards (NBS) and 3 Instituto de Pesquisas Techno16gicas (IPT) reference clay samples were determined by instrumental neutron activation analysis. The analytical work was 

designed to test the homogeneity of constituents in three new NBS 

reference clays, NBS-97b, NBS-98b, and NBS-679. The analyses 

of variance of 276 sets of data for these three standards show that 

the constituents are distnbuted homogeneously among bottles of 

samples for 94 percent of the sets of data. 

Three of the reference samples (NBS--97, NBS--97a, and 

NBS--97b) are flint clays; four of the samples (NBS-98, NBS--98a, 

NBS--98b, and IPT-32) are plastic clays, and three of the samples 

(NBS--679, IPT-28, and IPT-42) are miscellaneous clays (both 

sedimentary and residual). Seven clays are predominantly kaolinite; 

the other three clays contain illite and kaolinite in the approximate 

ratio 3:2. Seven clays contain quartz as the major nonclay mineral. 

The mineralogy of the flint and plastic clays from Missouri 

(NBS--97a and NBS--98a) differs markedly from that of the flint 

and plastic clays from Pennsylvania (NBS-97, NBS--97b, NBS--98, 

and NBS--98b ). 

The flint clay NBS-97 has higher average chromium, hafnium, lithium, and zirconium contents than its replacement, reference sample NBS-97b. The differences between the plastic clay 

NBS--98 and its replacement, NBS--98b, are not as pronounced. 

The trace element contents of the flint and plastic clays from 

Missouri, NBS--97a and NBS--98a, differ significantly from those of 

the clays from Pennsylvania, especially the average rare earth 

element (REE) contents. The trace element contents of clay 

1 U.S. Geological Survey, Reston, Va. 1 Washington State University, Pullman, Wash. 8 The Open University, Milton Keynes, United Kingdom. 

1 

sample IPT -32 differ from those of the other plastic clays. IPT -28 

and IPT -42 have some average trace element contents that differ 

not only between these two samples but also from all the other 

clays. IPT -28 has the highest summation of the average REE 

contents of the 10 samples. The uranium content of NBS--98a, 46 

parts per million, is very much higher than that of the other clays. 

Plots of average REE contents of the flint and plastic clays, 

normalized to chondritic abundances, show that the clays from 

Missouri differ from the same types of clay from Pennsylvania. The 

plot of REE contents for the miscellaneous clays shows that the 

normalized means for the elements lanthanum through samarium 

for IPT -28 are much greater than those for the other miscellaneous clays. The means for the elements europium through lutetium are similar for all three miscellaneous clays. 

INTRODUCTION 

The trace element contents of clays have been 

published only sporadically since 1950. Kerr and others (1950), in their reports on the American Petroleum 

Institute Reference Oay Minerals Research Project 

49, gave spectrographic determinations of 24 trace 

elements in 4 kaolins from Arkansas, Georgia, South 

Carolina, and New Mexico. Hinckley (1961) determined boron, gallium, and manganese contents in 

several kaolin samples from Georgia and South Carolina. Erickson (1963) analyzed several flint clays from 

Pennsylvania for K, Fe, Ti, Zr, Cr, and Ca, and Keller 

(1968) reported that Fe, Mg, Ca, Ba, Sr, Ti, V, Zr, Mn, 

Cu, Ni, Zn, Ga, Cr, and B are present in detectable 

amounts in flint clays from Missouri. Flanagan and 
others (1977, table 1) summarized published data on 

some trace element contents of U.S. National Bureau 

of Standards (NBS) samples (flint clay NBS-97 and 

plastic clay NBS-98) by Shimp and others (1957), 

Grabowski and Eunice (1958), Turekian and Carr 

(1961), Oark and Swaine (1963), Filby (1964), Taylor 

and Kolbe (1964), and Ball and Filby (1965). 

The first two clay samples from Pennsylvania 

(NBS-97 and NBS-98), of primary interest to an 

expanding refractory industry, were certified in 1931 

for their major and minor oxide contents. When the 

supplies of these two samples were depleted, they were 

replaced in 1959 by NBS-97a and NBS-98a from 

Missouri. In 1983, Hosterman and Flanagan collected 

two more clay samples, now NBS-97b and NBS-98b, 

from the same area in Pennsylvania as the original NBS 

clay samples (NBS-97 and NBS-98). They also collected in the same year a sample of common brick clay, 

NBS-679, to be added to the roster of NBS reference 

samples. All NBS samples have or will have certificates 

of analysis listing their major and minor oxides. 

Among the available reference samples are three 

samples from Brazil whose major and minor oxide 

contents are certified. The Agrupamento de Materials 

de Referenda (Reference Materials Group) of the 

Instituto de Pesquisas Tecnol6gicas do Estado de Sao 

Paulo, Brazil (IPT), was formed in 1975 with technical 

support from the NBS. Since then, more than 30 

different reference materials have been certified, 

including metals, minerals, cements, and the three 

reference clays from Brazil, IPT -28, IPT -32, and 

IPT -42. Certificates of analysis for these samples were 

issued in 1979-81. Data for the IPT clays have been 

included in this report for comparison with data for the 

NBS clay samples. 

The chemistry and mineralogy of the seven NBS 

samples and of the three IPT samples are discussed in 

this report. The 10 samples were analyzed by instrumental neutron activation (INAA) at 3 separate laboratories. All samples were analyzed at the U.S. Geological Survey (USGS) analytical laboratory, Reston, 

Va.; eight samples were analyzed at the Nuclear Radiation Center, Washington State University (WSU), 

Pullman, Wash., and six samples were analyzed at the 

Department of Earth Sciences, The Open University 

(TOU), Milton Keynes, United Kingdom. The mineralogy was determined by X-ray diffraction at the USGS. 

In addition to confirming previous estimates 

(Flanagan and others, 1977, tables 3 and 4) of some 

trace element contents of the flint and plastic clays from 

Pennsylvania and Missouri, the data in this report 

increase our knowledge of the trace element contents 

2 

of clays from different geologic settings. Because of the 

potential distribution of the NBS and IPT clays, the 

samples may serve as reference materials for studies of 

the trace element contents of other clays. 

GEOLOGIC SETTING AND LOCATION 

NBS-97, NBS-97a, and NBS-97b are samples 

of flint clays used in the manufacture of refractory 

brick. Material for NBS-97 was taken from the Mercer 

flint clay bed, the Pottsville Ibrmation of Pennsylvanian 

age, from a mine located on Morgan Run, Decatur 

Township, Oearfield County, Pa. NBS-97a was taken 

from the Cheltenham fire clay bed, Cheltenham Formation of Pennsylvanian age. The sample was supplied 

by the A.P. Green Fire Brick Co., Mexico, Mo. 

NBS-97b is a sample of the Mercer flint clay bed from 

a Harbison-Walker Refractories Co. mine on Anderson Creek, Pike Township, Oearfield County, Pa. The 

material for NBS-97b was sampled from a stockpile 

near the mine. The mine was not accessible because it 

had been backfilled to conform to the environmental 

regulations of the State of Pennsylvania. 

NBS-98, NBS-98a, and NBS-98b are samples 

of plastic underclays used in the manufacture of refractory and face brick. NBS-98 is a sample of underclay of 

the Oarion coal bed, Allegheny Ibrmation of Pennsylvanian age, collected from a mine located at Templeton, Pine Township, Armstrong County, Pa. Sample 

NBS-98a, taken from the Cheltenham fire clay bed, 

Cheltenham Formation of Pennsylvanian age, was supplied by the A.P. Green Fire Oay Co., Mexico, ~o. 

NBS-98b is a sample of the underclay of the Oanon 

coal bed obtained at the Harbison-Walker Refractories 

Co. plant at Oearfield, Oearfield County, Pa. 

The clay for sample NBS-679 was collected from 

the Maryland Oay Products, Inc. (formerly the Washington Brick Co.), pit at Muir kirk, Prince Georges 

County, Md. The clay is used for making red building 

and face brick. The very plastic brown clay, which is 

more than 11 m thick (Knechtel and others, 1961), 

occurs in the Arundel furmation, Potomac Group of 

Cretaceous age. Iron ore was mined from the Arundel 

Formation from colonial times until about 1911, and a 

furnace at Muir kirk was operated almost continuously 

from 1847 to 1912 (Miller, 1911). The iron ore is 

primarily siderite, FeC03 , which occurs as balls an~ 

irregular nodules that are removed when the clay IS 

mined. 

Reference sample IPT -28 is from Ananindeua, 

Para, Brazil, near Belem (lat 1°13'S., long 4S017' W.) 
in the Amazon Delta. The clay deposit occurs in an 

unnamed unit of Tertiary age that contains clastic 

sediments, claystones, sandstones, conglomerates, and 

laterite. Approximately 2 million metric tons of clay is 

mined annually from this deposit (Azevedo Branco, 

1984). 

Sample IPT -32 is from near Sao Joilo de Meriti, 

Rio de Janeiro, Brazil (lat 22°44' S., long 43°27' W.). 

The clay occurs in alluvium of an unnamed formation 

of Holocene age. The alluvium consists of fluvial, 

marine, and eolian deposits. A small amount of this 

plastic clay is mined annually from this area. 

Sample IPT -42 is from near Sao Simao, Sao 

Paulo, Brazil (lat 21 OZ8' S., long 470J6' W.). The clay is 

in the Piramb6ia Formation of Triassic age. The formation consists of sandstones, minor claystones, siltstones, and conglomerates. Approximately 3 million 

metric tons of the clay, which also contains some ball 

clay, is mined annually (Azevedo Branco, 1984). 

ANALYTICAL DATA AND HOMOGENEITY 

Some of the analytical work on the 10 reference 

clay samples was designed to test whether elements in 

the new samples, NBS-97b, NBS-98b, and NBS-679, 

were distributed homogeneously among bottles of 

samples. The remaining data were obtained so that 

meaningful comparisons could be made of the trace 

element contents of the types of clays from different 

geologic settings and geographic areas. 

Hosterman and Flanagan prepared the new clay 

samples for the NBS by the same method used to 

prepare USGS rock standards (Flanagan, 1986, p. 31). 

After the entire bulk of a powdered clay sample was 

mixed thoroughly in a "V" blender, a portion of about 

10 kg was split from the bulk material. Approximately 

one-half of the 10-kg portion was then sub sampled into 

60-mL bottles that were labeled, numbered, and distributed to the USGS, WSU, and TOU laboratories for 

analysis. The other half of the 10-kg portion was 

reserved for future chemical and mineralogical work. 

The remaining powdered bulk of the three new samples was delivered to the NBS. 

To determine the homogeneity of elements in the 

three new NBS samples, the USGS, WSU, and TOU 

laboratories were asked to analyze 1\\Q portions from 

two bottles of each sample. Not all laboratories 

reported four determinations for every element in each 

sample. Some determinations are missing because the 

counts for an element were lost during data processing 

or because the value calculated from the counts for an 

3 

element was below the lower limit of estimation. INAA 

data were obtained by the method described by Baedecker and others (1977) for the USGS, by Filby and 

others (1985) for WSU, and by Potts and others (1981, 

1985) for TOU. In addition to the four determinations 

for an element, the mean, the F ratio (see below), and 

the error (within bottle) standard deviation calculated 

during each analysis of variance were computed (see 

tables 4-10). 

fur comparison, some USGS data obtained in 

1976 for the four older NBS clay samples (NBS-97, 

NBS-98, NBS-97a, and NBS-98a) have been included 

in this report. These 1976 data consist of six determinations for each sample (data for two portions from 

each of three bottles). Because the tests for homogeneity described here would be based on determinations 

on four portions of any new NBS sample, data for 

bottles 1 and 2 of NBS-98a (Flanagan and others, 

1977, table 3) and data for bottles 1 and 2 of NBS-97, 

NBS-97a, and NBS-98 (Flanagan and others, 1977, 

table 4; USGS unpublished data, 1977) were randomly 

selected for inclusion in this report. To furnish more 

data for the older samples, the three laboratories were 

requested also to irradiate four sample portions from 

bottles of the older NBS samples so that comparisons 

could be made with approximately the same number of 

determinations per element for each sample. 

Hosterman and Flanagan received from Brazil 

only one bottle of each of the three clay samples 

IPT -28, IPT -32, and IPT -42. They divided the contents of each bottle into approximately equal amounts 

and sent a subsample of each clay to the three laboratories. The laboratories were requested to irradiate 

four portions from each of their subsamples. 

The analytical work to test for the homogeneity 

of elements among bottles of the three new NBS 

samples corresponds to an experimental design having 

a single variable of classification-the bottles of a 

sample. The calculations of the analysis of variance for 

this design are discussed in many textbooks on statistics 

(for example, Dixon and Massey, 1951 ). The test used 

for homogeneity of an element is the F ratio calculated 

during the analysis of variance. If the calculated F ratio 

for an element equals or exceeds the value in statistical 

tables at some preselected probability, it may be concluded that the element is distributed heterogeneously 

among the bottles. 

Two hundred and seventy-six F ratios, having 

degrees of freedom (d.f.) of 1 for the numerator and 2 

for the denominator, were calculated for the elements 

in the new NBS samples (NBS-97b, NBS-98b, 

and NBS-679) (see tables 4-10). Excluding six F ratios 
that exceed F0 .

95 (d.f., 1,2)=18.5 and that are marginally significant (see tables 5, 6, and 9), seven F ratios 

exceed F0 .

975 (d.f., 1,2)=38.5, and four ratios exceed 

F0 .

99 (d.f., 1,2)=99 (see tables 5 and 9). Normally, 

these 11 F ratios that equal or exceed the value for 

F0.

975 or for F0 .

99 might be considered evidence that the 

constituents (elements) are distributed heterogeneously 

among the bottles. However, these constituents were 

measured by two different spectroscopy systems at the 

WSU laboratory. Data measured by one system yielded 

significant F ratios, whereas data for the same element 

measured by the other system yielded ratios that were 

not significant. Such conflicting conclusions about the 

heterogeneity of an element may have resulted because 

the WSU laboratory irradiated and counted 100-mg 

sample portions (Filby and others, 1985). The USGS 

laboratory customarily irradiates 500-mg samples in 

the TRIGA reactor in Denver, Colo., because the 

larger sample portion yields more activity and the data 

are more reproducible. 

The significant F ratios calculated from data for 

chromium, thorium, scandium, and samarium measured by WSU spectroscopy system 1 for NBS-97b (see 

table 5) indicate that these elements are distributed 

heterogeneously. These conclusions may be due, however, to the relatively small differences between duplicate determinations for an element in each bottle. If 

one squares the differences and then sums the squares, 

the error mean square obtained is very much less than 

the mean square for the variation due to bottle means, 

and a significant F ratio is obtained. However, the 

percentage differences between averages of the elements by the two systems are 2.3 percent for chromium, 1.1 percent for thorium, 1.3 percent for scandium, and 1.0 percent for samarium. These small 

differences may be accepted as evidence that the four 

elements are distributed homogeneously. 

MINERALOGY 

The 10 clay reference samples were analyzed by 

X-ray diffraction using copper (CuKa) radiation. Small 

portions of the clay samples were reground in a mortar 

and pestle to ensure a uniform 200-mesh size and were 

made into wafers having random orientation. Each 

wafer was mounted in the sample holder and rotated at 

a rate of approximately 60 rpm during exposure to 

X-ray radiation. A goniometer traversed at a speed of 

1 o 2 6 per minute with a counting time of 1 second, thus 

resulting in a digital count every 0.02° 2 8. An X-ray 

trace was made from 3° to 70° 2 8 for each clay sample 

(figs. 1-3). 

4 

Figure 1 shows the X-ray diffraction patterns of 

flint clays NBS-97, NBS-97a, and NBS-97b. NBS-97 

and NBS-97b are from the Mercer flint clay bed 

(Pennsylvania), and NBS-97a is from the Cheltenham 

fire clay bed (Missouri). The X-ray patterns show that 

these samples contain more than 95 percent kaolinite 

and only traces of boehmite, illite, and chlorite 

(aluminous). The major difference among the clay 

samples is that the Missouri sample, NBS-97 a, has a 

slightly lower degree of crystallinity than the samples 

from Pennsylvania. This difference is evident by comparing the area between 20° and 25° 2 8 of the three 

X-ray diffraction patterns. The peaks in this area for 

NBS-97 and NBS-97b are much sharper and more 

clearly resolved than those for NBS-97a. 

Figure 2 shows the X-ray diffraction patterns of 

plastic clays NBS-98, NBS-98a, and NBS-98b. 

NBS-98 and NBS-98b are from the underclay of the 

Oarion coal bed (Pennsylvania), and NBS-98a is from 

the Cheltenham fire clay bed (Missouri). The X-ray 

patterns for NBS-98 and NBS-98b are almost identical. They both contain about 50 percent kaolinite, 35 

percent illite, and 15 percent quartz. NBS-98a contains approximately 75 percent kaolinite, 15 percent 

quartz, 10 percent illite, and a trace of chlorite. The 

mineralogy is consistent with the chemical analysis 

data presented in this report (see table 25). NBS-98 

contains 25.54 percent Al20 3 and 3.17 percent K20, 

whereas NBS-98a contains 33.19 percent Al20 3 and 

1.04 percent K20. 

Figure 3 shows the X-ray diffraction patterns for 

the three Brazilian clay samples, IPT -28, IPT -32, and 

IPT -42, and for the common brick clay sample from 

Maryland, NBS-679. The X-ray diffraction pattern of 

IPT -28 indicates that the sample contains 95 percent 

kaolinite and 5 percent quartz. Chemical data presented in this report (see table 25) agree with this 

mineral composition. The diffraction pattern for 

IPT -32 shows about 80 percent kaolinite, 10 percent 

quartz, 5 percent illite, 5 percent feldspar, and a trace 

of smectite. Chemical data in this report (see table 25) 

are consistent with this mineralogy. The X-ray diffraction pattern of IPT -42 indicates that the clay contains 

80 percent kaolinite, 15 percent quartz, and 5 percent 

illite. Again chemical data presented in this report (see 

table 25) are consistent with this mineralogy. 

The major components of sample NBS-679 are 

kaolinite (30 percent), illite (25 percent), mixed-layer 

clay (25 percent), and quartz (20 percent) (Knechtel 

and others, 1961). A minor amount of goethite is 

present, and smectite and feldspar are present in trace 
NBS-97a 

NBS-97b 

I 

NBS-97 

--~-~--~-~-~-rT ~ 

I 

20 10 

DEGREES 26 

FIGURE 1.-X-ray diffraction traces of flint clays NBS-97 and NBS-97b from the Mercer flint clay bed (Pennsylvania) 

and of NBS-97a from the Cheltenham fire clay bed (Missouri). C, chlorite; I, illite; K., kaolinite; B, boehmite. 

5 
NBS-98a 

w I i 

I 

I 

NBS-98b . I 

U

. I 

I 

I 

. ,V· 

30 

DEGREES 2& 

K 

a 

a 

i I 

I I 

20 10 

FiGURE 2.-X-ray diffraction traces of plastic clays NBS-98 and NBS-98b from the Oarion coal bed 

underclay (Pennsylvania) and of NBS-98a from the Cheltenham fire clay bed (Missouri). C , chlorite; I, 

illite; K, kaolinite; Q, quartz. 

6 
a 

IPT-42 

DEGREES 28 

7 

FIGURE 3.-X-ray diffraction traces 

of three Brazilian clay samples, 

IPT-28, IPT-32, and IPT-42, and a 

common brick clay, NBS-679, from 

Maryland. S, smectite; I, illite; K, 

kaolinite; Q, quartz; F, feldspar. 
amounts. The chemical analysis for the major and 

minor oxides is not yet available. 

TRACE ELEMENT CONTENTS 

INAA data reported for all samples by the three 

laboratories are given in tables 1-16. Table 17 contains 

data for lithium determined in the USGS laboratory by 

inductively coupled plasma spectroscopy and by flame 

atomic absorption spectroscopy. 

The tables are arranged so that data for the old 

NBS samples from Pennsylvania (NBS-97 and 

NBS-98) in tables 1-3 precede data for the new NBS 

~amples from Pennsylvania (NBS-97b and NBS-98b) 

m tables 4-7. Data for the new NBS common brick clay 

sample from Maryland (NBS-679) are given in tables 

8-10, and data for the samples from Brazil (IPT-28, 

IPT-32, and IPT-42) are found in tables 10--14. The 

USGS was the only laboratory to report data for flint 

clay NBS-97a (table 15) and plastic clay NBS-98a 

(table 16) and the lithium content for all samples (table 

17). 

Laboratory means of sets of data for the samples, except NBS-97a and NBS-98a, are summarized 

in tables 18-21. Laboratory means and their averages 

for NBS-97 and NBS-97b are given in table 18, those 

for NBS-98 and NBS-98b in table 19, those for 

NBS-679 and IPT -28 in table 20, and those for 

IPT -32 and IPT -42 in table 21. The conversion from 

elements in parts per million to oxide in percent was 

made, where necessary, in tables 18-21. Because of the 

unequal number of determinations for some elements 

in tables 1-16, the averages of laboratory means in 

tables 18-21 were obtained by weighting each laboratory mean by the number of determinations for the 

mean. 

Table 22 lists the weighted averages for 3 oxides 

and 29 elements for the samples (from tables 18-21 ). 

The average lithium content of each sample (from 

table 17) and the weighted averages for NBS-97 a 

(from table 15) and NBS-98a (from table 16) also are 

included in table 22. In addition, table 22 contains 

summations of the average rare earth element contents 

(IREE) for all samples. All the averages in table 22 

are considered to be provisional because they may 

change as more data from other laboratories become 

available. Table 23 lists 14 elemental ratios for the 10 

reference samples. Potassium was converted from K20 

(table 22), and magnesium was converted from MgO 

(see table 25) to be used in several elemental ratios in 

table 23. Table 24 lists the provisional means for the 

8 

samples normalized to the grand mean for 14 elements 

and for IREE. These normalized means make comparisons among samples more obvious than the use of 

the averages of table 22. Table 25 gives the average 

major and minor oxide contents of four NBS samples 

and of three IPT samples from the Certificates of 

Analysis. 

The K/Rb and the K/Ba ratios in table 23 show 

that the samples from Missouri, NBS-97a and 

NBS-98a, differ from their Pennsylvania counterparts, 

NBS-97, NBS-97b, NBS-98, and NBS-98b, as might 

be expected because of the different geologic environment. The Rb/Cs ratio for the plastic clay from Missouri, NBS-98a, is much lower than the Rb/Cs ratios 

for the plastic clays from Pennsylvania, and the Rb 

averages of the three plastic clays NBS-98, NBS-98a, 

and NBS-98b are greater by factors of 3 or more than 

the Rb contents of the flint clays from the same areas 

(table 22). 

One striking ratio in table 23, Th/U=0.54 for 

NBS-98a, is due to the uranium content of 46 ppm for 

that sample. This value is almost 5 times greater than 

the next highest uranium content, 9.6 ppm for 

NBS-97b. The uranium was probably introduced into 

the clay bed at the time of deposition from an unknown 

source. The Hf{fa ratios of the 10 samples are fairly 

similar (see table 23), except for the high Hftra ratios 

of 9.93 for NBS-97 and 7.70 for IPT -28, which are 

due to high Hf contents of 40.9 ppm and 30.8 ppm, 

respectively. The high Zr and Hf averages of NBS-97 

and IPT -28 yield Zr/Hf ratios (35.8 and 34.1, respectively) that fall within the range of such ratios for the 10 

samples (32.1 for NBS-97b to 45.7 for IPT-42). 

The averages in table 22 and the means normalized to the grand mean in table 24 for some elements in 

the 10 samples show many of the differences among 

the samples. The flint clay NBS-97 has higher chromium, hafnium, lithium, and zirconium contents than 

its current replacement, NBS-97b, from the same area. 

The differences between the plastic clays NBS-98 and 

NBS-98b, also from the same area, are not as evident. 

Some of the trace element contents of the flint and 

plastic clays from Missouri, NBS-97a and NBS-98a, 

differ significantly from those of their counterparts 

from Pennsylvania, especially IREE. The averages for 

elements such as Cs, Li, Ta, Sc, La, Tb, and Tm, when 

considered individually or in combination, can distinguish NBS-98a from all the other clay samples. 

Differences among the REE contents of the clay 

samples are shown in figures 4, 5, and 6. The average 

REE contents were normalized by the data of Anders 

and Ebihara (1982) for C1-chondrites, multiplied by 
w 

~ 500 

~ z 

:::J 

CD 

< 

w 

1-

~ 

0 

~ :r: 

(..) 

......... 

1-

z 

~ z 

0 

(..) 

~ w 

:! 

w 

...J 

w 

~ < w 

w 

a: 

~ 

w 

~ 

< a: 

w 

~ 

200 

100 

50 

20 

EXPLANATION 

e NB5-97 

• NBS-97b 

.& NBS-97a 

La Ce Nd Sm Eu Gd Tb Tm Yb Lu 

FIGURE 4.-Average rare earth element contents of the flint clays (NBS-97, NBS-97a, and NBS-97b) normalized to chondritic 

abundances. 

1.31. The plot for flint clays (fig. 4) shows that the flint 

clay from Missouri, NBS-97a, has REE contents that 

are distinctly different from those of the two flint clays 

from Pennsylvania. NBS-97 and NBS-97b show plots 

that are essentially the same except that the data points 

for NBS-97 are slightly greater. 

The plot for the plastic clays (fig. 5) shows that 

the Missouri plastic clay, NBS-98a, has high REE 

contents throughout the entire range from lanthanum 

to lutetium. However, unlike the plots for the flint clays, 

the normalized means for thulium, ytterbium, and 

lutetium are significantly higher than the normalized 

means of the same elements for NBS-98 and 

NBS-98b. The plastic clay from Brazil, IPT -32, has the 

second highest means for lanthanum, cerium, and 

neodymium and the low.est means for thulium, 

ytterbium, and lutetium. 

9 

The plot for the miscellaneous clays (fig. 6) 

shows that the Maryland clay NBS-679 and the Brazilian clay IPT -42 have very similar REE contents for 

all elements normalized to chondritic abundances. The 

other Brazilian clay, IPT-28, has high REE contents 

throughout the range from lanthanum to samarium. 

The plastic clay from Brazil, IPT -32, has a 

number of trace element contents that differ markedly 

from those of the other plastic clays. The lithium 

contents of the other two clays from Brazil, IPT -28, 

from the Amazon Delta, and IPT -42, from Sao Simao, 

are about equal, but the averages of many other trace 

elements in these two clays differ significantly. The 

averages for cobalt, thorium, uranium, and zinc not 

only differ between the two clays, but also, individually 

or in combination, show that IPT -28 and IPT -42 differ 

from all the other clay samples. 
w 

u 

z EXPLANATION 

< 0 

z 0 NBS-98 

:::> 

CXI 

<( 0 NB8-98b 

~ 

a: 6. NBS-98a 

0 200 z 

0 

X IPT-32 

::t 

u 

--~ 

z 

~ z 100 

0 

u 

~ 

z 

w 

~ 

w 

..J 50 w 

j: 

a: 

<( 

w 

w 

a: 

<( 

a: 

w 20 

CJ 

<( 

a: 

w 

> <{ 

La Ce Nd Sm Eu Gd Tb Tm Yb lu 

FIGURE 5.-Average rare earth element contents of the plastic clays (NBS-98, NBS-98a, NBS-98b, and IPT -32) normalized to chondri tic 

abundances. 

SUMMARY 

Mineralogically, the three flint clays, NBS-97, 

NBS-97a, and NBS-97b, differ very little (fig. 1), 

except that NBS-97a has much greater normalized 

IREE contents than NBS-97 and NBS-97b have (fig. 

4). These three clays are composed of kaolinite and 

traces of boehmite, illite, and chlorite (aluminous). 

The kaolinite in NBS-97a (from Missouri) has a 

slightly lower degree of crystallinity than the kaolinite 

in NBS-97 or NBS-97b (from Pennsylvania). This 

difference in crystallinity could be due to the different 

geologic settings of the two areas. 

The flint clay sample NBS-97 (Pennsylvania) has 

higher average contents of chromium, hafnium, lithium, and zirconium than its replacement, NBS-97b 

(Pennsylvania), whereas differences between the plastic 

10 

clays from Pennsylvania, NBS-98 and NBS-98b, are 

not as evident. Some of the trace element contents of 

the flint and plastic clays from Missouri, NBS-97a and 

NBS-98a, differ significantly from trace element contents of similar clays from Pennsylvania, especially the 

average REE contents normalized to chondritic abundances (figs. 4 and 5). 

The plastic clay from Missouri, NBS-98a, is 

distinguished by its high uranium content ( 46 ppm), 

and it has the greatest IREE contents of the four 

plastic clays (fig. 5). The average contents of elements 

such as Cs, Li, Ta, Sc, La, Ce, Tb, and Tm distinguish 

NBS-98a from the other plastic clays. The Pennsylvania plastic clays contain kaolinite, illite, and quartz, 

whereas the Missouri clay contains kaolinite, quartz, 

illite, and traces of chlorite. The different geologic 

settings of the two areas may account for the mineral-
w 

u 

z 

~ z 

:::) 

CD 

< 

w 

1-

a: 

0 

z 

0 

J: 

u 

1-

z 

~ z 

0 

u 

1-

z 

w 

:E 

w 

...J 

w 

J: 

1-

a:: 

<( 

w 

w 

a: 

< a: 

w 

(!) 

< a: 

w 

~ 

500 

200 

100 

50 

20 

La Ce Nd Sm Eu Gd 

EXPLANATION 

e NB5-679 

U IPT-28 

J;;a IPT-42 

--

~--------------- ----- ------........... ......_......_ ......_ 

--

-...... --__ ~ 

Tb Tm Yb Lu 

FIGURE 6.-Average rare earth element contents of the miscellaneous clays (NBS-679, IPT-28, and IPT-42) normalized to chondritic 

abundances. 

ogical differences. The plastic clay IPT-32 is similar to 

NBS-98a in mineralogical content, but most of the 

trace element contents of IPT -32 differ from those of 

the other plastic clays. 

The miscellaneous clay samples, NBS-679, 

IPT -28, and IPT -42, are all from different geologic 

environments, and so no mineralogical relationship was 

expected. The normalized .IREE contents (fig. 6) 

show that the light rare earth elements lanthanum, 

cerium, neodymium, and samarium are enriched in 

sample IPT-28. Only minor differences occur in the 

rare earth element plots for NBS-679 and IPT -42. 

The lithium contents of the two Brazilian clays 

IPT-28 and IPT-42 are about equal, but the averages 

of many of the trace elements in these two clays differ 

significantly. The averages for cobalt, thorium, uranium, and zinc differ between IPT -28 and IPT -42, and 

these averages also distinguish IPT -28 and IPT -42 

from the other clays. 

11 

REFERENCES CITED 

Anders, Edward, and Ebihara, Mitsuru, 1982, Solar-system abundances of the elements: Geochimica et Cosmochimica Acta, v. 

46, no. 11, p. 2363-2380. 

Azevedo Branco, P.C., 1984, Principais dep6sitos minerais: Conceitos, metodologia e listagem, in Schobbenhaus, Carlos, 

Almeida Campos, Diogenes, Derze, G.R., and Asmus, H.E., 

eds., Geologia do Brasil: Departamento Nacional da 

Producao Mineral, Minist~rio das Minas e Energia, p. 

359-428. 

Ball, T.K., and Filby, R.H., 1965, The zinc contents of some 

geochemical standards by neutron activation and X-ray fluorescence analysis: Geochimica et Cosmochimica Acta, v. 29, 

no. 7, p. 737-740. 

Baedecker, P.A., Rowe, JJ., and Steinnes, E., 1977, Application of 

epithermal neutron activation in multielement analysis of 

silicate rocks employing both coaxial Ge(Li) and low energy 

photon detector systems: J oumal of Radioanalytical Chemistry, v. 40, p. 115-146. 

Clark, M.C., and Swaine, D.J., 1963, Some trace element contents 

of National Bureau of Standards reference samples numbers 
1a, 98, and 99: Geochimica et Cosmochimica Acta, v. 27, no. 

11, p. 1139-1142. 

Dixon, WJ., and Massey, FJ., Jr., 1951, Introduction to statistical 

analysis: New York, McGraw-Hill, Inc., 370 p. 

Erickson, E.S., 1963, Mineralogy, petrographic, and geochemical 

relationships in some high-alumina and associated claystones: 

Unpublished Ph.D. thesis, Pennsylvania State University, 190 

p. 

Filby, R.H., 1964, The contents of several trace elements in some 

rock samples: Geochimica et Cosmochimica Acta, v. 28, no. 2, 

p. 265-269. 

Filby, R.H., Nguyen, Son, Grimm, C.A., Markowski, G.R., Ekambaram, Vanavan, Tanaka, Tsuyoshi, and Grossman, Lawrence, 

1985, Evaluation of geochemical standard reference materials 

for microanalysis: Analytical Chemistry, v. 57, p. 551-555. 

Flanagan, FJ., 1986, Reference samples in geology and geochemistry: U.S. Geological SuiVey Bulletin 1582, 70 p. 

Flanagan, F.J., Schwartz, L.J., Rowe, J.J., and Dorrzapf, A.F., Jr., 

1977, Available clay and feldspar reference samples as standards for archaeological pottery studies: Geostandards Newsletter, v. 1, no. 1, p. 61-66. 

Grabowski, R.J., and Eunice, R.C., 1958, Quantitative spectrochemical determination of barium and strontium: Analytical 

Chemistry, v. 38, no. 8, p. 1374-1379. 

Hinkley, D.N., 1961, Mineralogy and chemical variation in the 

kaolin deposits of the Coastal Plain of Georgia and South 

Carolina: Unpublished Ph.D. thesis, Pennsylvania State University, 215 p. 

Flanagan, FJ., 1986, Reference samples in geology and geochemistry: U.S. Geological SuiVey Bulletin 1582, 70 p. 

Flanagan, F.J., Schwartz, L.J., Rowe, JJ., and Dorrzapf, A.F., Jr., 

1977, Available clay and feldspar reference samples as standards for archaeological pottery studies: Geostandards Newsletter, v. 1, no. 1, p. 61-66. 

Grabowski, R.J., and Eunice, R.C., 1958, Quantitative spectrochemical determination of barium and strontium: Analytical 

Chemistry, v. 38, no. 8, p. 1374-1379. 

12 

Hinckley, D.N., 1961, Mineralogy and chemical variation in the 

kaolin depositS of the Coastal Plain of Georgia and South 

Carolina: Unpublished Ph.D. thesis, Pennsylvania State University, 215 p. 

Keller, W.O., 1968, Flint clay and a flint-clay facies: Qays and Qay 

Minerals Bulletin, v. 16, no. 2, p. 113-128. 

Kerr, P.F., Hamilton, P.K., Pill, R.J., Wheeler, G.V., Lewis, D.R., 

Burkhardt, W., Reno, Duane, Taylor, G.L., Meilenz, R.C., 

King, M.E., and Schieltz, N.C., 1950, Analytical data on 

reference clay materials: American Petroleum Institute, Preliminary Report No.7, 160 p. 

Knechtel, M.M., Hamlin, H.P., Hosterman, J.W., and Carroll, 

Dorothy, 1961, Physical properties of nonmarine Cretaceous 

clays in the Maryland Coastal Plain: Maryland Geological 

SuiVey Bulletin 22, 11 p. 

Miller, B.L., 1911, The geology of Prince George's County, Maryland and the District of Columbia: Maryland Geological 

SuiVey, The Johns Hopkins Press, 151 p. 

Potts, P.J., Thorpe, O.W., and Watson, J.S., 1981, Determination of 

the rare-earth element abundances in 29 international rockstandards by instrumental neutron activation analysis: A critical 

appraisal of calibration errors: Chemical Geology, v. 34, no. 1, 

p. 331-352. 

Potts, P J., Thorpe, O.W., Isaa~ M.C., and Wright, D.W., 1985, 

High-precision instrumental neutron-activation analysis of 

geological samples employing simultaneous counting with both 

planar and coaxial detectors: Chemical Geology, v. 48, p. 

145-155. 

Shimp, N.F., Conner, Jane, Prince, A.L., and Bear, F.E., 1957, 

Spectrochemical analysis of soils and biological materials: Soil 

Science, v. 82, no. 1, p. 51-64. 

Taylor, R.S., and Kolbe, P., 1964, Geochemical standards: Geochimica et Cosmochimica Acta, v. 28, no. 4, p. 447-454. 

Turekian, K.K., and Carr, M.H., 1961, Chromium, cobalt, and 

strontium in some National Bureau of Standards rock reference samples: Geochimica et Cosmochimica Acta, v. 24, nos. 

1-2, p. 1-9. 
TABLES 

TABU: 1.-Jnsttumental neutron activation detenninations of elements in NBS-97 by the U.S. Geological Swvey, 1976 and 1985 

(In parts per million, except Fe and Na in perceut. x, mean; ad. standard deviation; -, no data. Four portions from a bottle were used for 1985 data) 

1985 1976 

Dater1i nati ans i sd Bottle 1l' sd 

1 2 

Fe 0.634 0.660 0.664 0.023 0.6~ 0.64 0.6~8 0.01:5 

.674 .688 .67 .67 

Na .0~2 .061 .0~7 .0038 

.055 .058 

Ba 190 216 205 13.4 290 250 2~8 25 

217 198 260 230 

Co 3.24 3.36 3.34 .067 3.2 3.4 3.32 .10 

3.39 3.38 3.4 3.3 

Cr 639 659 664.2 20.6 557 572 576 14.9 

671 688 584 591 

Cs 2.13 2.34 2.24 .oes 2.3 2.3 2.40 .12 

2.21 2.26 2.~ z.~ 

Hf 40.8 40.9 40.42 .39 3B.4 37,7 38.72 .e:s 

40.4 39.6 39.3 39.5 

Rb 24 21.7 23.05 1.14 23 22 24.5 2.4 

24 22.:5 26 27 

Sb 1.29 1.51 1.46. .14 1.2 1.3 1.40 .18 

1.43 1.63 1.6 1. 5 

Ta 4.66 4.19 4.34 .22 4.02 4.15 4.18 .15 

4.25 4.25 4.17 4.39 

Th 36.5 38.4 38.02 1.03 36.5 36.2 36.9 .74 

38.8 38.4 37.9 37.0 

u 7.0 7.3 7.22 .17 

7.4 7.2 

Zn 75 82.1 79.8 3.33 100 104 101.5 1.7 

90 82 101 101 

Zr l ,890 1,760 1,788 68.5 1,380 1,340 1,368 22 

1,750 1,750 1,360 1,390 

Sc 19.1 19.9 19.7 .41 21.4 20.3 20.8 .45 

20.0 19.8 20.7 20.8 

La 26.6 28.7 27.9 .93 32 33 33.2 .96 

29.4 28.0 34 34 

Ce 46.8 50.3 49.95 2.20 57 56 57.0 .82 

S1.9 so.a 59 57 

Nd 17 21 '20.7 1 3.5 18 20 1 19.3 '1.2 

<40 24 20 

s. 4.8, 5.13 5.10 .14 :s.a 5.8 5.8 

~.20 :S.18 :S.8 :s.a 

Eu 1.22 1.28 1. 2' .o:s 1.16 1. 26 1.24 .OS 

1.29 1.27 1.29 1. 26 

Tb 1. 11 1.19 1.16 .04 1. 24 L25 1.2SB .017 

1.18 1.18 1.28 1. 26 

T11 .82 .71 .BO .06 

.85 .82 

Yb 6.20 6.4 6.20 .22 6.4 6.6 6.72 .28 

:S .. 9 6.3 6.9 7.0 

Lu .96 .98 .97 .01 .94 .94 .'15 .02 

.98 .97 .98 I 94 

1 x or ad of three data. 

15 
TABLE 2.-Instrumental neutron activation determinations of elements in NBS-98 by the U.S. Geological Swvey, 1976 

and 1985 

[In parts per million. except Fe and Na in percent. x, mean; sd, standard deviation; -, no data. Four portions from a bottle "Were used for 1985 data) 

1~85 1976 

D•terai nations X sd Bottle X sd 

2 

Fe 1.52 1.47 1.495 0,035 1.41 1. 42 1.402 0.018 

1.53 1. 46 1.38 1.40 

Na .189 .213 .204 .OU5 

.193 .220 

Ba 631 670 652.8 20.2 660 670 655.0 17 

670 640 660 630 

Co 15.0 14.5 14.65 I 37 13.8 u.s 13.75 .06 

14.9 14.2 13.7 15.7 

Cl" 139 U4 135.8 3.3 110 113 112 3.2 

138 132 109 116 

Cs 10.9 10.4 10.65 .29 10.6 10.5 10.82 .sa 

10.9 10.4 10.5 11.7 

Hf 7.82 7.52 7.60 .31 7.5 6.3 7 I 1 .54 

7.87 7.20 7.2 7.5 

Rb 139 153 US.B 2.87 153 HiS 152.8 2.1 

159 15& 150 153 

Sb 1.48 1.50 1. 70 .43 1. 4 1. 3 1.22 .15 

2.34 1.48 1. 1 1. 1 

Ta 2.22 2.23 2.22 .04 2.23 2.19 2.22 .04 

2.27 2.16 2.lB 2.27 

Th 21.6 20.9 21.2 .54 19.5 19.1 19.4 .32 

21.7 20.6 n.2 19.8 

u 4.7 5.2 5.02 .24 

5.2 5.0 

Zn 107 107 104 4.2 127 126 124.2 2.8 

104 98 123 121 

Zr 418 '278 2 355 2 55 320 310 335 26.4 

327 320 340 370 

Sc: 23.5 22.9 23.1 .60 22.9 22.9 22.85 .17 

23.6 22.3 22.6 23.0 

La 73.4 73.4 73.32 .30 79 77 78.:5 2.64 

72.9 73.6 82 76 

Ce 133 130 130 3.56 135 133 134.8 1.26 

132 125 135 136 

Nd 57 48 51.5 3.87 46 :so 48.0 1.63 

51 50 48 48 

Sill 9.90 9.90 9.89 .02 10. 1 10.0 9.98 • 12 

9.85 9.90 10.0 9.8 

Eu 1. 79 1. 77 l. 78 • 04 1. 76 1.74 1.73 .03 

1. 83 1.73 1. 70 1. 72 

Gd 9.3 8.6 9.08 .33 

9.3 9.1 

Tb 1. 33 1.29 1. 31 .05 1. 39 1.37 1.33 .07 

1. 37 1.25 1. 32 1.24 

Ta .62 .64 .63 .03 

.59 .67 

Yb 4.46 4.31 4.51 .26 4.7 4.8 4.8B .17 

4.BB 4.38 5.1 4.9 

Lu .71 .72 .70 .02 .1.6 .62 .645 .04 

69 .69 .60 .70 

1 Correction for fission product interference exceeds 20 percent of the reported value. 11 x or sd of three data. 

16 
TABLE 3.-/nstrumental neutron activation detenninations of elements in 

NBS-97 and NBS-98 by the Nuclear Radiation Center, Washington State 

University 

[In parts per million. Sample portions were counted by two ~ systems. x, mean; sd, 

standard deviation;-, no data) 

NDS-97 IIBS-98 

Sptctrasc!!!l !Ystaa Spoctrscopy SyltH 

I 2 J ,. I 2 i sd 

Fl 6,547 ~,n9 6,680 523 12,6'10 14,820 11,368 1,036 

7,146. 7,on 12,560 13,400 

Ill 573.5 561.7 591 20 1,814 1,971 1,934 99 

1»61.7 ·579.3 1,905 2,04a 

r •·'" 4,!517 4,Ul 240 l4,690 24,730 2:S,062 409 

4,9'2 4,5Z4 25,370 25,460 

A• 4.722 4.461 4.88 .35 4.649 S.J40 4.78 .28 

5.136 5.202 4.863 4.487 

II 22t.9 299.9 281 lB 671.5 703.1 73l 61 

:st9.1 290.0 7~.0 813.3 

Co S.4Bl 3.209 3.40 .22 12.98 13.27 1S.l5 .34 

3.676 J.255 12.11 13.36 

Cr ~83.4 601.9 624 51.2 123.1 121.4 123.9 6.4 

o4t.& 505.4 U3.0 UB.2 

Cs 2.388 2.3~7 2.411 .a 10.20 10.33 10.46 .44 

2.700 2.395 u.u 10.21 

Sa Sl.BI 55.75 54.87 2.1 12.12 33.&0 33.90 2.15 

56.67 55.25 32.84 36.CJ9 

Hf 43.92 l9.11 43.58 3.23 7.222 7.U4 7.67 .lO 

46.80 44.49 7.852 7.755 

Ni 35.99 311.2& 34.11 3.37 53.31 44.73 44.42 6.4 

U.&6 31.34 40.82 28.12 

R~ 22.69 Z5.Bt 24.85 J.SB U:i.:i 150.8 151.4 4.3 

26.87 23.96 154.7 IS4.S 

Sr 143.2 73.1> 1121 2,2.5 100.4 263 71.4 

l44.8 <tOO 360.0 237,9 

b 1.684 1.589 1.63 .15 1.539 1.284 1.S9 .63 

1.794 1.440 2.021 1.5ll 

Ta 3.962 3.475 3.84 .48 2.0&4 !.840 2.00 .20 

4.45f J.449 2.261 1.8~ 

Til 40.05 J9,U 40.24 1.82 19.74 21.09 20.80 .77 

42.88 38.92 21.56 20.83 

u 8.529 7.718 8.73 1.0 7.651 6.006 7.06 .tl 

lO.U '·'" a. on 6.572 

Zr t,toS 979.4 1,256 224 243.4 217.2 2'2 55 

'·"' 1,172 342.2 245.9 

Sc 20.14 19.22 20.11 1.19 21.17 21.74 21.80 .68 

21.79 &9.30 22.76 21.52 

La 29.61 SS.Itl 30.34 .95 &7.08 73.51 71.53 3.70 

29.63 St. 51 70.09 7~.45 

t1 ~7.03 :53.39 ::1 •• 63 3.86 127.3 127.8 lr1.7 4.9 

61.'2 54.17 U7.1 126.7 

Nd 18.67 19.12 28.9 U,7 43.42 63.97 57.00 9.8 

41.5 :S6.29 16.19 64.40 

Sn 4.952 5.173 5.44 •• 2 8.1165 8.410 8.BJ .36 

,,M9 S.211S 9.283 8.&96 

Ell 1.375 1.295 1.36 .07 1.735 1.849 1.81 .06 

1.462 1.316 1.85h 1.799 

Til .M 1.165 1.07 .07 1.027 1.245 1.15 .so 

1.059 1.076 1.213 1.128 

Yll '·"! lt.41B lt.B5 1.14 4.282 4.15& 4.37 .22 8.50~ 5.878 4.675 4.379 

La 1.434 1.266 1.38 .2:S .810 .728 ·" .20 

1.675 1.132 1.184 .859 

1 x of three data. 

17 
TABLE 4. -Instrumental neutron activation determinations of elements in NBS-97b and NBS-98b 

by the U.S. Geological Survey 

[In parts per million, except Fe and Na in peroent. x, mean; sci, standard deviation; -, no data. Error 8d and F ratio are 

from the analysis of variance of the data. F ratios were not significant at Fo.111 ( dJ., 1,2)•18.5) 

NBS·97· MBS·9U 

BoUlt Nl. E:rror F BoUlt No. Error F 

1 2 r sd ratio 1 2 i sd ratio 

f't 0.86~ 0,882 O.I7L 0.007 1.75 1.260 1.1 .. 2.217 o.~l2 2.13 

.869 .869 1.209 1.220 

Jb .058 .062 '.OU .169 .136 .151 .t12 2.95 

.Oll9 (,1 .150 .no 

Bil Z13 217 223.5 12.7 (1 690 670 652.5 40 <l 

224 240 620 630 

Ca 3.&7 3.&6 3.62 .071 <1 16.0 15.3 15.SB .32 (J 

3.53 l.h4 15.43 J5.59 

Cr !27 235 230.8 3.2 1.22 123 114 118.8 2.5 4.62 

231 230 120 UB 

Cs 3.:U 3.40 3.34 .043 5.97 16.0 15.3 IS. 55 .27 l.84 

3.34 3.37 15.47 15.41 

Hf 12.58 12.' 12.62 .11 2.16 b. SO 6.46 6.53 .16 l.97 

12.42 12.6 6.49 6,SI 

Rb 34.2 28.2 32.3 3.5 <I ua 168 Ut.5 3 ,,00 

32.2 34.7 161 174 

Sb 2.06 2.14 2.13 .0-47 1.91 1.62 1.59 1.60 .ou 6.40 

2.14 2.1! 1.61 1.56 

Til 3.97 4.01 3.97 .051 <1 2.02 1.95 1.91 .029 l.06 

4.00 3.90 1.97 1.91 

Tb :U.2 l6.8 36.4 .so (J 20.7 29.5 20.1 .u 1.42 

36.3 36.2 20.0 20.1 

u 7.4 7.6 7.4 .1, <1 J.~ 3.0 ~.~ .7 (•) 

7.4 7.3 3.5 4.0 

Za 73.B 84.8 78,9 5.7 <1 101.9 92.6 95.0 3.7 l.ll 

81.0 76 94.7 1ft 

Ir 530 ~' 500 3~ 2.31 270 2~ 287.8 35 <1 

515 448 ~0 266 

Be 23.1 23.6 23.2 .25 (J 22.7 21.6 22.1 .u 2.n 

23.2 23.1 22.1 22.0 

La 24.:1 24.7 24.8 .27 {1 68.8 ~.7 67.6 1.:16 (1 

25.0 24.9 67.4 .a.s 

I: I 43.2 43.4 43.2 .18 <1 109 102 104.9 2."35 2.75 

43.0 43.1 104.7 103.9 

ld 28 24 :s26 39 38 39,5 2.1 <1 

(40 (40 38 .42 

Sl 3.21 3.31 3.30 .05:5 <I 6.10 6.49 &.34 .17 (1 

3.35 3.31 6.41 6.34 

Eu .715 .7!2 .742 .011 <I 1.09 l.U 1.12 .025 (1 

.737 .736 1.13 1.11 

6d 5.1 5.6 5.7 .60 (J 6.1 5.6 s.a .39 (l 

6.3 5.7 5.5 6.1 

Tb .75 .78 .eo .06 (1 .86 .B9 .85 .os (l 

.81 .BI .87 .n 

ll .72 .69 .61 .04'1 1.22 .~9 .so .475 .100 (I 

.&B .~o .55 .5> 

Yb 4.35 4.t. 4.5B .155 4.81 :S.22 3.37 3.33 .177 <I 

4.46 4.89 3.53 3.2 

L1 .741 .60 .754 .012 (I .s.co .572 .554 .014 <l 

.7CI .735 .55!5 .:S47 

1 x of three data. 1 No F ratio because of a zero mean square for bottles. 1 x of two data. 

18 
TABLE 5.-/nsttumental neutron activation determinations of elements in NBS-97b by the Nuclear Radiation Center, Washington 

State University 

[In parts per million. Samples were counted by two speci:IOIIOOJI'Y systems. x, mean; sd, standard deviation) 

Sptctroscopy System 1 

BoHla Na. 

1 2 i 

Errar 

sd 

F 

ratio 

Fe 7,981 81 284 81 116 110 1.84 

8,102 9,099 

Na 496.3 512~& 511.4 9.9 2.34 

511.4 525.4 

K 4 1 887 4,895 4,946 107 1.06 

4,996 !5,108 

As 9~225 10.78 10.76 1.12 3.48 

10.14 12.91 

B1 245.4 269.4 279 32 

Ca 

Cr 

Cs 

Ga 

Hf 

Ni 

Rb 

Sr 

Sb 

Th 

u 

Zr 

Sc 

La 

Ce 

Nd 

Sm 

Eu 

Tb 

Yb 

Lu 

307.8 283.9 

31545 

~.497 

21310 

214.0 

3.528 

3,615 

S2.3& 

50.76 

13.13 

13.10 

42.22 

26.91 

31.!50 

31.00 

62.21 

121.1 

2.170 

2.074 

3.644 

3.556 

35.73 

35.79 

12.63 

10.9S 

440.1 

411.3 

22.34 

22.44 

22.42 

22.34 

44.75 

44.90 

17.18 

17.65 

2.601 

2.620 

I 771 

.eo9 

.792 

.813 

3.930 

4.392 

.976 

1.185 

3.449 3156 

3.770 

220.4 217 

222.2 

3.412 3.5~ 

3.675 

S1. 86 S2. 1 

53.52 

13.83 n~ 4 

13.4() 

25.97 34.5 

43.02 

31. :sa :s1. a 

33.21 

.9.59 105 

136.9 

2. 267 2. u. 

2.127 

3.682 3.64 

3.698 

311.73 

36.91 

10.76 

10.94 

44&.9 

4lB.2 

22.90 

22.97 

22.91 

23.27 

46.28 

48.31 

13.59 

20.15 

3.543 

3.612 

.818 

I 762 

.794 

.827 

4.825 

5.1'17 

1.204 

1.132 

36.3 

11.3 

429 

22.7 

22.7 

U.1 

17 .t 

3.09 

179 

.81 

4.!59 

1.12 

.16 <1 

1. 1 

.14 <1 

<1 

.22 

11.5 

195 1. 21 

<1 

~OB <1 

.06 4.05 

.10 411 125 

I 83 1132 

20 <1 

118 14192 

1.0 5.89 

3.3 (1 

.04 4 730 

.o~ (a) 

.02 <1 

.30 9.25 

.11 <1 

1 No F ratio because of a zero mean square for bottles. 1 Significant at Fun (d.f., 1,2)•38.!5. 1 Significant at Fo.t~ (d.f., 1,2•)18.!5. 4 Significant at Fo.tt (d.f., 1,2)•99. 

19 

Spectro1capy Sy1t1• 2 

Battle Mo. 

1 2 

Errol" 

ld 

7,734 9,919 ,,300 1040 

9,906 9,745 

524.3 512.0 520 lB 

502.7 541.1 

4,831 4,669 4,775 146 

4,680 4,920 

7.908 8.190 8.34 .46 

8.195 '· 063 

301.2 283.8 275 33 

236. J 277.9 

3.491 

3.319 

20618 

211.3 

3.305 

3.422 

57.38 

54.21 

13.28 

13.42 

24.24 

20.31 

26.91 

29.94 

98.52 

107.7 

1.929 

2.009 

3.157 

3.152 

36.12 

36.39 

11.2' 

10.02 

290.0 

372.3 

22.11 

22.30 

24.14 

22.9~ 

46.41 

4~.50 

21.00 

20.43 

3.163 

3.02B 

.760 

.783 

.948 

.BB9 

4.477 

4.579 

.BUS 

.954 

3.!526 3.!50 

3.618 

211.6 212 

217.0 

3.826 3.50 

3.460 

511.21 56.9 

59.81 

13.69 13.5 

13.45 

21.62 22.0 

21.98 

32104 29.7 

29.97 

157.0 127 

144.4 

2.200 2.0& 

2.119 

3.189 3. 20 

3.300 

36.76 

37.67 

9.93' 

10.04 

356.4 

298.1 

22.38 

22.68 

23.31 

23.97 

46.47 

46.82 

17.95 

21.58 

3.0b5 

3.239 

.825 

.BOO 

• 931 

,909 

4.521 

4.638 

.870 

.897 

36,7 

10.3 

329 

22.4 

23.6 

46.3 

20.2 

3.12 

.79 

.n 

.07 

3.!5 

.19 

2.4 

.14 

1.97 

1.8 

7.9 

.06 

.06 

.47 

.61 

50 

.18 

.u 

.49 

1. B 

.11 

.02 

.03 

,08 

.02 

F 

ratio 

1.04 

<l 

<l 

1.57 

< 1 

3.35 

2.23 

2.12 

<1 

2.51 

<1 

1.97 

12.47 

2.62 

4.09 

1.10 

<1 

3.34 

2.CO 

<1 

<1 

<1 

<1 

4.27 
TABLE 6.-Instnnnental neutron activation detenninations of elements in NBS-98b by the Nuclear 

Radiation Center, Washington State University 

(In parts per million. Samples were counted by two spectroscopy systems. x, mean; sd, standard deviation; S, F ratio significant 

at Fu11 (d.f., 1,2)•18.S] 

Spectroscopy Sysha 1 Spl!ttroiCDDY Sysha 2 

Bottll No. Error F Battl! Ng1 Error F 

8 18 i sd ratio a 18 i sd ntia 

F1 10,940 12,550 Jl,610 433 5.49 10,600 13,410 12,038 381 ~.us 

11,220 u, 730 11,200 12,940 

Mi 1,1&9 1,230 1,225 37 3.73 1,278 1,335 1,328 37.2 (1 

1,210 1,291 1,351 1,350 

k 22,030 22,450 22,752 842 1.48 22,840 24,080 23,8~ 670 (1 

22,450 24,080 24,180 24,120 

As 5.788 5.939 6.33 .67 <1 5.839 7.507 6.92 .90 (1 

6.521 7.061 7.507 6.819 

81 654.9 772.7 709 20 19.56 s 806.4 739.5 773 28 14.65 

671.9 735.4 B45.l 699.8 

CD 14.23 15.13 15.0 .40 4.81 13.82 14.94 14.6 .52 (1 

14.82 15.66 14.83 14.66 

Cr 109.2 115.9 114 1.6 22.28 s 99.82 109.0 107 5.9 (1 

uo.s 118.8 111.6 107.5 

Cs 15.22 16.36 16.0 .26 17.74 14.70 16.11 15.7 .69 <1 

15.63 16.68 16.05 H5.78 

61 24.43 24.87 ~.1 .74 1.88 28.27 29.82 29.6 .79 2.09 

24.73 26.31 29.72 30.46 

Hf 6.539 6.989 6.85 .13 15.69 6.427 7.030 6.78 .28 <1 

6.631 7.240 6.920 6. 751 

Ni 49.19 66.72 57.6 3.2 16.84 42.84 37.18 46.1 8,9 (1 

52.97 61.59 52.50 52.03 

D 160.6 172.4 169 3.5 6.97 155.8 164.8 133 6.0 1.65 

167.4 174.1 165.5 172.0 

Sr 202.5 203,9 208 10.4 1.60 154.5 178.1 205 58 (1 

199.6 224.4 258.6 228.3 s~ 1.520 1.582 1.63 .14 (l 1.435 1.680 1.79 .36 1.61 

1.783 1.648 1.681 2.345 

Ta 1.786 1.869 1.87 .07 2.28 1.557 1.640 1.63 .27 (J 

1.861 1.979 1.688 1.647 

Til 19.18 20.75 20.2 .40 12.82 18.78 20.65 20.1 ·' <1 

19.86 21.19 20.56 20.31 

u 10.30 7.584 8.58 .74 7.09 8.396 7.460 8.19 .44 1.83 

8.822 7.620 8.568 8.319 

Zr 243.2 223.5 243 17.8 3.79 229.2 180.7 193 38 <1 

278.4 228.8 157.0 206.1 

St 20.78 22.25 21.7 .30 16.34 19.92 21.53 21.10 .87 <1 

21.37 22.29 21.65 21.32 

La 54.33 SS.96 SS.6 1.0 7.18 57.16 61.52 60.5 2.2 1.03 

54.14 511.00 61.62 61.79 

Ct 102.9 113.2 109.4 2.6 9.56 96.67 108.7 105.2 6.1 <I 

108.0 113.5 108.8 106.7 

Nd 34.94 37.26 33.5 4.2 (l 31.15 37.99 39.3 7.1 (1 

32.71 29.09 44.08 43.99 

Sa 4.704 4.899 4.97 .23 1.70 4.218 4.707 4.61 .28 <1 

4.881 5.338 4.788 4.719 

Eu 1.127 1.161 1.16 .Ol 1.86 1.047 1.200 1.15 .06 1.40 

1.162 1.209 1.172 1.171 

Tb .708 .960 .8o .u 1.09 .809 .900 ·" .09 <1 

.790 .762 .986 .849 

Yb 3.124 4.109 4.07 .&3 ( 1 3.124 3.300 3.41 .29 (1 

4.905 3.454 3.634 3.594 

Lu .958 .682 .99 .24 <l .IMO .840 .71 .oa 1.28 

1.1e 1.117 .662 .672 

20 
TABLE 1.-Instnunental neutron activation determinations of elements in NBS-97b and NBS-98b by the Department of Earth Sciences, The 

Open University 

[In parts per million, except Fe and Na in percent. x, mean; sd, standard deviation; -, no data. Error sd and F ratio are from the analysis of variance of the data. F ratios were not 

significant at Fo.tli (dJ., 1,2)•18.S) 

NBS-97b NBS-9Bb 

DgUll H£11 Error F Bottle No. Error F 

17 22 i sd ratio 2 21 "i sd ratio 

FeL 1.16 1.15 1.165 0.02 <1 1. 68 1.68 1. 652 0.041 (l 

1. 19 1.16 1.61 1.64 

Co 3.53 3.47 3.54 .065 2.12 15.5 15.2 15.08 .43 <l 

3.65 3.52 14.7 14.9 

Cr 232 231 231.2 1.12 <1 125 123 123.0 2.0 (2) 

230 232 121 123 

Cs 3.32 3.37 3.37 .036 1.23 16.7 u.s 16.28 .49 <1 

3.3B 3. 41 15.8 16.1 

Hf 12.9 12.9 13.02 .19 <1 7.03 6.97 6.930 .11 1.38 

13.2 13.1 6.9 6.96 

Rb 31 35 32.5 2.2 <1 185 183 178.0 8.6 (2) 

33 31 171 173 

Ta 3.67 3.64 3.68 .038 <1 2.03 1.99 1.977 .05 1.33 

3.70 3.71 1.98 1. 91 

Th 36.6 36.5 36.6 .OS 1.20 21.4 21.2 21.02 .40 <1 

36.6 36.6 20.7 20.8 

u 9.6 9.6 9.4 .25 <1 4.9 4.5 4.80 .16 3.60 

9.3 9.2 5.0 4.8 

Sc: 23.5 23.4 23.45 .07 s.oo 23.2 23.1 22.98 .27 <l 

23.6 23.3 22.7 22.9 

La 23.6 23.7 23.4 .50 <1 65.3 65.2 64.62 1.07 <1 

23.5 22.7 63.2 64.8 

Ce 47.7 46.8 47.4 .49 (1 119 118 117.2 3.6 2.29 

47.3 47.7 121 111 

Nd 16. l 16.8 16.75 .60 <1 39.0 38.7 38.50 .51 <1 

17.3 16.8 38.5 37.8 

Sm 3.20 3.21 3.18 I 04 <1 6.66 6.59 6.635 .05 7.40 

3.14 3.16 6.75 6.54 

Eu .82 .at .815 • 007 (2) 1.26 1. 26 1.250 .016 <1 

.81 .82 1.25 1.23 

Tb .81 .81 .832 .04 <1 .92 .91 .91~ .007 8.oo 

.BB .83 .93 .90 

Ho 

T8 .70 .72 .72 .03 <1 .~6 .sa .:575 .022 <1 

.75 .71 .60 .:56 

Yb 4.94 4.90 4.925 .01 9.00 3.95 3.86 3.B~B .07 3.30 

4.94 4.92 3.90 3.72 

Lu .83 .82 .828 .005 1.20 .64 .65 .640 .016 <1 

.Bl .83 .65 .62 

1 Total Fe as Fea Oa. 1 No F ratio becauae of a zero mean square for bottles. 

21 
TABLE B.-Instrumental neutron activation detenninations of elements in NB~79 by the U.S. Geological Survey 

[In parts per million, except Fe and Na in percent. x, mean; sd, standard deviation; -, no data. Error sd and F ratio are from the analysis of variance of the data. F ratios were not 

significant at Fa.tl (d.f., 1,2)•18.5) 

Bottle No •. Error F Battle Na. Error F 

4 1 x sd r&tia 4 1 x sd ratio 

Fe 9.52 9.19 9.35 o.oe:s 6.08 Zr 202 148 184 25 (1 

9.39 9.30 188 196 

Na .144 .147 .143 .013 1. 25 Sc 22.7 21.7 22.4 .27 2.83 

.156 .124 22.5 22.4 

Ba SlO 411 464 34 2.29 La 51.0 50.1 50.6 .36 1.23 

470 466 50.6 50.7 

Co 25.6 25.0 25.25 .u 6.40 c. 98 94 94.5 2.1 3.5lt 

2~.3 23.1 95 91 

Cr 106 102 103.2 1. 5 2.89 Nd 41 43 43.8 2.7 <1 

103 102 46 45 

Cs 9.41 9.18 9.33 .44 <1 s. 9.14 8.74 8.91 .16 1. 39 

9.35 9.40 8.87 8.90 

Hf 4.20 4.06 4.18 .10 < 1 Eu 1.67 1. 61 1. 66 .06 <1 

4.20 4.27 1.64 1.72 

Rb 189 181 184 4.5 <1 Sd 7.8 7.4 7.3 .46 <1 

181 185 7.1 6.8 

Sb .76 .82 .at .025 6.80 Tb 1.19 1.16 1.175 .007 8.00 

.79 .86 1.18 1.17 

Ta 1. 37 1.30 1.34 ,022 3.20 Ta .47 .51 ".49 

1.35 1.34 <1 .49 

Th 14.3 13.4 13.85 .35 1. 28 Yb 3.3 3.3 3.35 .07 (:Z) 

13.8 13.9 3.4 3.4 

u 2.42 1. 82 2.17 .35 <1 Lu .55 .54 .54 .011 4,00 

2.03 2.40 .53 .53 

Zn 114 109 113 3.5 (l 

1l3 116 

1 x of three data. 1 No F ratio because of a zero mean square for bottles. 

22 
TABLE 9.-/nstrumental neutron activation determinations of elements in NBS-679 by the 

Nuclear Radiation Center, Washington State University 

[In parts per million. Samples were counted by two spectroscopy systems. x, mean; sd, standard deviatiou; -, no data] 

Sputroscapy Systu 1 SpactrOICOPY SystH 2 

Battle No. Error F Bottle teo. Error F 

2 24 i ld ratio 2 24 "i sci ratio 

Ft 781760 89,690 83,460 8,420 <1 83,940 86,710 841UO 210SO <t 

89,050 76,360 84,070 82,610 

II& 1,158 1,322 s,m 47 4.66 1,214 1,327 1,282 18.5 145.26 

1,245 1,285 1,226 1,3112 

K 201280 23,290 21,~2 752 6.76 21,820 22,840 21,960 405 139.06 

21,470 22,370 20,570 23,610 

k 8,706 10.14 9.37 .27 14.93 8,356 9.483 8.98 .10 2 105 

8.980 9.665 8.557 9.510 

Ia 471.2 ~42.4 480 66 (l ,,,4 4Cf8.9 506 49 <1 

492.8 412.2 481.3 467.4 

to 21.n 24.87 23.15 2.2t (1 23.01 23.82 23.15 .57 (1 

24.5 21.25 23.09 22.69 

Cr 89.88 101.7 94.5 9.9 (I 93.76 95.23 92.9 2.7 <1 

101.0 ~.26 92.59 89.87 

t:s 8.649 9,939 9.27 .82 <1 9.325 9.230 9.17 .16 <t 

9.757 8.732 9.147 8.970 

Ia 31.25 39.91 341.5 2.3 6.53 33.24 42.89 38.9 1.3 1

44.72 

35.62 39.06 35.59 43.82 

Hf 3.940 4.282 4.09 .37 <1 4.217 4.293 4.21 .07 (1 

4.407 3.7lf 4.172 4.164 

li 40.56 45.94 48.6 7.8 (I ,S,B 43.37 ~2.3 2.4 '30.13 

53.95 Sl.BB 58.9 48.14 

Rb 209.3 204.1 195 16.5 <I 212.3 198.2 194 16 <I 

183.1 184.1 185.2 181.2 

Sr (80 112.1 •1o2 us.J <110 ., 

92.3 102.8 84.78 94.08 

Sb .m .767 .82 .07 6.15 .742 .871 .ao .02 '54.50 

.841 .706 .756 .845 

Ta 1.273 1.254 1.30 .05 1.05 1.174 1.222 1.18 .05 (1 

1.376 1.285 1.192 1.121 

n 12.98 14.47 13.4 1.3 <I 13.64 13.79 13.54 .27 (1 

14.09 12.13 13.49 13.26 

u 5.264 5.434 4.88 .82 <l 6.452 4.177 5.19 1.36 (l 

4.995 3.811 4.297 ~.837 

Ir 160.3 161.8 181 28 <1 165.0 130.2 JS9 12 6.62 

200.5 200.5 144.7 116.5 

k 19.97 22.48 21.06 2.00 <1 21.10 21.7~ 21.07 .59 <I 

22.44 19.33 20.84 20.60 

La 44.9' 50.08 4B.l4 1.59 4.16 48.22 52.83 50.85 .81 146.66 

48.08 49.45 47,92 54.43 

Ct 90.47 102.5 95.5 8.9 (1 97.72 101.5 98.1 2.6 (I 

100.8 88.09 "·" "·37 

ld 37.34 44.35 40.5 2.56 1.80 51.62 47.07 46.9 4.3 (I 

40.24 40.12 43.11 45.89 

s. 7.521 8.593 8.16 .26 8.72 6.836 7.733 7.34 .07 1 149.3 

8.032 8.496 6.942 7.834 

Eu 1.605 1.750 1.il7 .10 (l 1. 713 1.809 1.73 .06 <I 

1.725 1.600 1.697 1.688 

Ttl .863 1.106 1.04 .OB 8.62 1.218 1.253 1.15 .13 <I 

.985 1.207 .982 1.136 

Yb 4.872 7.572 5.43 1.29 1.92 3.499 3.220 3.32 .07 122.15 

4.200 5.079 3.448 3.096 

Lu .942 1.839 1.21 .26 a.ao .893 .494 .60 .18 1.59 

.706 1.369 .m .480 1 Significant at Fo.H& (d.f., 1,2)•38.5 11 Significant at Fo ... (d.f.. 1,2)•99. 1 Significant at Fus (d.f., 1,2)•18.5 4 x of three data. 

23 
TABLE 10.-/nstrumental neutron activation determinations of elements in NBS-679, /PT-28, /PT-32, and /PT-42 by the Deportment 

of Earth Sciences, The Open University 

[In parts per million, except Fe and Na in percent. "'i, mean; sd, standard deviation; -, no data. Error sd and F ratios from the analysis of variance of the data. F ratios 

were not significant at Fa16 (d.f., 1,2)•18.5] 

NBS-679 IPT-29 lPT-32 IPT-42 

Bottlt Na. Error F Data "i Data 'i Data X 

1 2 i sd ratio 

Fe' 12.75 12.83 12.89 0.15 (2) 0.78 0.76 3.33 3.42 1.15 1.12 

13.03 12.94 .75 3.52 1.09 

Co 24.8 25.0 25.08 .27 (1 .55 .52 4.57 4.59 2.87 2.77 

25.3 25.2 .48 4.61 2.67 

Cr Ul 112 uo.s 1.4 <1 140 140 59 62 BO so 

111 lOB 141 64 80 

Cs 9.73 9.82 9.86 .14 (2) 2.96 3.06 1.59 1.56 

9.99 9.90 3.15 1.53 

Hf 4.53 4.62 4.528 .067 1.58 31.3 31.6 18.4 18.55 6.11 5.88 

4.44 4.52 31.8 1B.7 5.65 

Rb 197 S9B 196.2 2.1 1.48 38 39 29 26 

193 197 40 23 

Ta 1.40 1.36 1.365 .002 s.oo 4.11 4.10 3.79 l.BO 1.42 1.40 

l.38 1.32 4.10 3.82 1.37 

Th 14.7 14.7 14.75 .07 (Z) 50.5 50.2 33.8 35.0 14.7 14.6 

14.8 14.8 50.0 36.3 14.6 

u 3.1 2.9 2.95 .07 8.00 4.1 4.2 7.5 7.8 1.8 1.8 

3.0 2.8 4.3 8.2 1.9 

Sc 23.7 23.5 23.6 0 (2) 17.9 19.0 16.2 16.8 19.6 19.5 

23.7 23.5 18.0 17.3 19.4 

La 50.7 50.~ 50.22 .56 <1 181 181 101 106 64.9 64.6 

50.2 49.5 181 110 64.2 

Ct 112 113 111.8 1.5 (1 376 37B 160 160 111 110 

112 110 380 161 109 

Nd so.o 47.4 49.0 .94 2.40 129 129 66.6 66.4 5lt.3 S6.8 

49.5 49.2 129 6b.l 57.2 

s. 9.72 9.61 9.59 .11 <1 17.2 17.4 10.:5 10.8 10.9 10.9 

9.51 9.52 l7.lt 11.0 10.9 

Eu 1.92 1.89 1.91 .007 12.00 2.82 2.80 1.71 1.74 2.81 2.78 

1.92 1.90 2.78 1.78 2.75 

Tb 1.2, 1.23 1.27 .05 (2) 1.19 1.21 1.01 1.06 1.33 1.33 

1.28 1.32 1.23 1.12 1.33 

Ho 1.9 1.6 1.75 1.6 1.9 

Ta .S9 .63 .61 .03 <1 .68 .70 .35 .38 .66 

.64 .59 .71 .42 .67 ·'' 

Yb 4.00 3.94 3.96 .02 6.40 5.22 5.22 2.94 3.09 4.10 4.07 

3.97 3.95 5.23 3.24 4.04 

Lu .63 .63 .ns .007 (2) .89 .90 .45 .49 .68 .66 

.64 .64 .92 .53 .65 1 Total Fe as Fet()1• 

1 No F ratio bealuse of a zero mean square for bottles. 

24 
TABLE 11.-/nstiUmental neutron activation determinations of e~ts in /PT-28 and /PT-32 by the U.S. Geological Survey 

(In parts per million. except Fe and Na in percenL x, mean; sd, standard deviation; -,no data) 

IPT-28 lPT-32 

Determinations _, 

K sd Deter1i nations "K sd 

Fe 0.545 0.535 0.549 0.017 2.35 2.46 2.45 0.074 

.542 .573 2.46 2.53 

Na <.07 .041 <.2 .123 .133 .126 .029 

<.1 <.2 .088 .159 

Ba 275 280 275.5 6.9 356 350 366 17.3 

281 266 370 389 

Co .41 .40 .41 .022 4.26 4.30 4.42 .17 

.44 .:Sfl 4.57 4.57 

Cr 130 130 132.S :S.!2 !2.7 !6.15 S6.1 2.15 

133 137 56.5 58.6 

Cs <.2 <.2 <.2 2.83 2.87 2.89 .05 

<.2 .4 2.89 2,96 

Hf 29.8 29.4 29.82 .31 lb. 4 16.8 16.65 .24 

30.1 30.0 16.5 16.9 

Rb <16 (17 <1o 30.0 32.8 34.4 3.68 

<17 <19 38.0 36.8 

Sb .94 1.07 1.04 .073 .31 .46 .46 .11 

1.11 1.05 .49 .57 

Ta 4.14 4.22 4.19 .078 3.54 3.7~ 3.74 .15 

4.12 4.29 3.77 3.91 

Th 47.6 47.8 48.1 .57 31.3 33.0 32.6 .87 

48.2 48.9 33.0 33.1 

u 3.4 3.5 3.42 .41 4.9 5.4 5.45 .49 

3.9 2.9 5.4 6.1 

Zn 12.8 (6 1 14.1 1 2.3 56.4 59.6 58.0 1. 91 

16.7 12.7 56.4 59.8 

Zr 1,280 1,230 1,258 20.6 660 670 685 26.5 

1,260 1,260 720 690 

Sc 17.0 17.0 17.15 .24 15.15 15.67 15.62 .35 

17 I 1 17.5 15.68 16.00 

La 179 183 182.2 2.22 100.2 105.0 104.3 2.77 

183 184 106.0 106.0 

Ce 314 319 327.0 12.6 13!5 141 140 3.46 

334 341 141 143 

Nd 102 108 111.0 10.4 59 ''~ ,9.8 2.2 

108 126 58 63 

s. 15.8 16. 1 16.35 .56 9.50 10.01 9.86 .24 

16.4 17. 1 9.95 10.00 

Eu 2.47 2.43 2.49 .04 1.47 1. 49 1. 51 .04 

2.49 2.54 1.52 1.56 

Gd 8.9 9.5 9.85 .89 7.2 7.5 7.65 .42 

10.0 11.0 8.2 7.7 

Tb 1.01 1. 04 1.06 .04 • 91 .99 .97 .04 

1.07 1. 11 .98 .99 

Tta .63 .52 .sea .oso .35 <.1 1 • 40 1 .06 

.62 I SB .40 .46 

Vb 4.2 4.5 4.45 .17 2.71 2.84 2.80 .06 

4.6 4.5 2.79 2.94 

Lu .73 .75 .752 .021 .421 .470 .428 .032 

.75 .78 .393 .430 

1 x or sd of three data. 

25 
TABLE 12.-Instnunental neutron activation detenninations of elements in /PT-28 

and /PT-32 by the Nuclear Radiation Center, Washington State University 

[In parts per million. Two sample portions were counted by two spectroscopy ~ms. x, mean; sd, standard 

deviation;-, no data) 

IPT-28 IPT-32 

SpKtroscopy Syste1 SpKtrDiii:D2l Sllihl 

1 2 i lid 1 2 x sd 

Ft 5,240 5,982 5,243 519 22,930 22,940 23,065 298 

4,632 5,199 22,880 23,510 

Ia 1114.5 153.9 183.5 28.4 1,337 1,285 1,316 52 

208.5 207.2 1,263 1,379 

r 260.3 302.7 366 117 6,591 6,510 6,562 89 

373.6 527.6 6,475 6,674 

As 1.675 2.655 1.99 .45 8.213 IJ.7711 7.48 .59 

1.789 1.825 7.568 7.364 

Ia 383.5 348.9 351 36 478.6 481.6 480 8.9 

389.4 311.3 469.1 490.7 

Co .461 .599 .522 .085 4.132 4.355 4.36 .18 

.436 .591 4.584 4.379 

Cr 131.9 137.7 129 10.9 53.18 59.81 59.23 4.31 

113.2 133.9 60.57 63.35 

ts <.3 <.3 <.3 3.046 3.158 3.06 .08 

<.S <.4 3.088 2.953 

Sa 39.76 46.76 44.8 3.5 38 ... 0 42.29 39.47 1.98 

45.22 47.45 37.83 39.36 

Hf 32.42 33.30 31.3 2.2 17.34 17.47 17.77 .43 

28.22 31.41 18.09 18.19 

lti <30 <35 lO 21.75 (235 '25 •• 

30 <35 29.43 <35 

Rb 2.819 (6 14.3 38.52 35.40 37.45 1.60 

5.735 (7 38.91 36.98 

Sr 213.1 271.7 271 42.9 146.8 72.50 108 44 

295.8 315.2 67.04 145.0 

s~ .403 1.039 .94 .093 .555 .643 .60 .07 

.832 .995 .558 .479 

Ta 4.150 3.579 3.7& .29 3.675 3.086 3.42 .3i 

3.766 3.553 3.778 3.140 

Th 50.26 51.19 48.5 3.7 32.11 33.35 33.37 .95 

42.99 49,63 33.65 34.38 

u 7.912 7.317 7.14 .80 8.330 8.584 8.21 .65 

6.008 7.318 8.679 7.2&0 

Zr 968.2 811.2 837 93.8 523.7 474.0 503 33 

820.7 746.3 538.7 475.3 

Sc 17.34 17.28 16.63 1.11 15.29 15.36 15.46 .17 

14.98 u .. 92 15.53 15.67 

La 180.9 196.1 197.8 7.9 109.0 110.6 110.9 3.3 

197.3 196.7 108.4 115.6 

c. 359.0 355.3 339.8 26.7 146.1 153.3 146.6 4.6 

301.0 344.1 143.0 144.1 

ld 10&.9 128.7 118.8 14.3 51.27 &3.67 51.4 5.4 

10lt.O 133.4 57.66 61.17 

Sa 14.89 14.36 15.0 1.03 10.34 8.712 9.23 1.11 

16.52 14.31 9.957 7.927 

Eu 2.621 2.707 2.58 .!6 1.570 1.588 1.59 .02 

2.341 2.644 1.594 1.610 

Til t.U2 1.039 1.03 .11 .852 .9&9 .88 .075 

.an 1.101 .828 .842 

v. 5.135 4.6&5 4.72 .32 3.286 3.115 3.36 .36 

4.353 4.741 3.147 3.880 

La 1.226 .859 .94 .20 .781 .563 .63 .12 

.782 .876 .513 .665 

1 x of two data. 

26 
TABLE 13.-Instrumental neutron activation detenninations y/ elements in IPT-42 by the U.S. Geological Survey 

(In parts per million, except Fe and Na in pen:enL x, mean; 8d, standard deviation; - no data) 

Deterainatians i sd Detarminatians i sd 

Fe 0.690 0.723 0.715 0.019 Zn 24.0 26.2 24.6 1.05 

.712 .736 24.4 24.0 

Ba 213 220 226 24.2 Zr 194 232 230 27 

262 210 260 233 

Co 2.25 2.41 2.38 .083 Sc 16.6 17.2 17 I l .32 

2.42 2.42 17.2 17.3 

Cr 66.0 67.4 68.5 2.19 La 57.1 59.4 59.7 1.96 

70.6 70.1 60.5 61.7 

Cs 1.23 1.43 1. 32 .09 Ce 87 92.2 90.3 2.5 

1.28 1135 90 92.2 

Hf 4.93 ~.OB 5.11 116 Nd 44 49.3 48.1 3.0 

5.09 5.33 48 51 

Ni <100 S11 9.4 10.15 9.95 .48 

9.73 10.51 

Rb 22.5 24.2 22.2 1.51 Eu 2.15 2.31 2.27 .oa 

21.5 20.7 2.28 2.33 

Sb .58 .64 I I 57 1 .061 6d 7.2 2 8.2 

.52 <1 9.3 

Sr (300 Tb 1.06 1.17 1. 13 .os 

1. 15 1.13 

Ta 1.22 1. 36 1. 34 .01 T1 .61 2 .48 

1.32 1. 45 .34 

Th 12.6 12.9 12.8 .14 Vb 3.59 3.71 3.68 .06 

12.8 12.9 3.70 3.73 

u 1. 20 1. 43 1.34 .12 Lu .522 .522 .524 .oo~ 

1. 26 1. 45 .523 .529 

1 x or sci of three data. 11 x of two data. 

27 
TABLE 14.-Instnonental neutron activation determinations of elements in IPT-42 by the Nuclear Radiation 

Center, Washington State University 

(In parts per million. Two sample portions were counted by two spectroscopy systems. x, mean; sd, standard deviation; -, no data) 

s2ectrosco~l Slstem S~ectrosco~l Slstea 

1 2 r sd 1 2 x sd 

Fe 6,999 6,985 6,864 184 Sb 0.990 0.751 0.80 0.13 

6,601 6,872 .782 .696 

Na 216.8 213.8 216.6 18.2 Ta 1.422 1.188 1.25 .12 

240.1 195.8 1.154 1.235 

K 4,560 4,471 4,244 408 Th 14.01 13.98 13.49 .79 

4,291 3,656 12.33 13.64 

As 1.827 1.944 1.67 .26 u 4.192 4.105 3.27 1.07 

1.562 1.376 2.006 2.760 

Ba 256.9 268.9 234 41 Zr 287.9 290.1 266.2 34 

232.8 177.3 271.6 215.4 

Co 2.420 2.471 2.43 .14 Sc 18.08 17.74 17.26 .81 

2.235 2.583 16.26 16.97 

Cr 72.13 69.32 68.18 3.28 La 70.27 71.16 69.12 3.08 

64.52 66.74 70.02 64.56 

Cs 1.453 1.464 1.48 .083 f Ce 98.57 101.5 96.2 5.54 

1.409 1.601 88.57 96.37 

Sa 33.76 36.48 33.46 2.54 Nd 49.46 47.10 49.74 4.99 

33.35 30.27 45.58 56.81 

Hf 5.786 5.509 5.53 .18 Sa 10.80 9.094 9.56 1.48 

5.388 5.422 10.67 7.668 

Ni 32.09 (30 32.09 Eu 2.564 2.554 2.47 .11 

(30 (30 2.338 2.433 

Rb 27.31 25.57 24.76 2.99 Tb 1.121 1.179 1.090 .076 

20.44 25.72 1.005 1.053 

Sr 142.4 136.4 128.3 13.0 Vb 3.731 3.937 3.66 .22 

117.1 117.3 3.460 3.522 

Lu .994 .734 .82 .13 

.ass .715 

28 
TABLE 15.-lnstrwnental neutron activation detenninations of elements in NBS-97a by the 

U.S. Geological Swvey, 1976 and 1985 

[In parts per million, except Fe and Na in peroent. x, mean; sd, standard deviatiou; -,no data) 

1995 1976 

812UI1 

Dtterainatians i sd l 2 I sd 

Fl 0.319 0.318 0.320 0.002 0.31 0.30 0.298 0.012 

.322 .30 .28 

Ill .040 .038 .039 

<.1 

Ba 500 540 527 23 1150 670 667.5 12.6 

540 680 670 

Co 4.3~ 4.41 4.39 .04 4.3 4.1 4.08 .21 

4.42 4.1 3.8 

Cr 215 216 217 2.1 180 180 182.5 s.o 

219 190 lBO 

Cs 1.56 1.56 1.59 .06 1.6 1.4 1.58 .13 

1.&& 1.7 1.6 

Hf 12.57 12.50 12.66 .21 12.0 11.9 11.52 .95 

12.90 12.1 10.1 

Rb u.s 15.0 12.2 3.7 

13.5 

Sb .97 .87 .91 .05 .9 .7 .78 .10 

.90 .a .7 

Ta 3.01 2.9f 3.01 .02 3.16 3.16 3.21 .063 

3.02 3.23 3.29 

Th 34.1 34.2 34.2 .1 31.7 31.1 31.3 .09 

34.3 32.2 30.2 

u 6.8 6.8 6.9 .2 

7.1 

Zn 44.0 45.5 45.2 1.0 

46.0 

Zr 530 430 507 68 550 580 582.5 28.7 

560 ~20 580 

Sc 31.7 32.1 32.0 .3 32.3 31.2 31.35 1.21 

32.3 32.2 29.7 

La 91.7 94.3 93.7 1.8 102 100 102.8 3.0 

95.1 102 107 

Ct 190 192 190 2.5 207 200 205.8 3.9 

187 209 207 

Nd 76 88 83 6.4 86 84 88.2 4.3 

86 n 89 

s. 18.8 18.7 18.8 .I 21.4 20.4 21.45 1.24 

18.9 23.2 20.9 

Eu 3.67 3.67 3.69 .04 3.85 3.77 3.82 .037 

3.74 3.80 3.84 

6d 18.1 18.0 JB.O .1 

17.9 

Tb 2.72 2.77 2.78 .07 2.81 2.&8 2.77 .10 

2.86 2.fi0 2.69 

T1 .95 .99 1.00 .OS 

1.05 

Yb 6.89 7.00 6.93 .ott 7.8 7.:5 7.7 .39 

•• 90 8.2 7.3 

Lu 1.001 .973 .986 .014 .98 .93 .995 .052 

.984 1.05 1.02 

29 
TABLE 16.-Instrumental neutron activation detenninations of elements in NBS-98a by 

the U.S. Geological Survey, 1976 and 1985 

(In parts per million. except Fe and Na in percent. x, mean; ad, standard deviation; -, no data) 

1985 un 

&11UI1 

DttlninatiDDI 1 5d 1 2 i lid 

Ft 0.940 0.935 0.940 O.OOit 0.89 0.90 0.188 0.010 

.946 .sa .88 

Na .057 <.1 .057 

(,2 

81 470 460 467 5.8 530 460 492 29 

470 490 490 

Co 12.20 11.95 12.04 .34 1l.4 11.7 U,6 .18 

12.21a 11.8 u.s 

Cr 254 252 253 1.2 214 214 2U 3.6 

254 209 207 

Cs 6.19 6.06 6.16 .09 6.2 6.3 6.28 .06 

6.23 6.3 6.3 

Hf 8.10 7.98 8.06 .07 7.2 7.6 7.42 .17 

8.10 7.5 7.4 

Rb 37.8 38.0 35.7 3.8 37 36 34.2 2.6 

31.4 32 32 

Sb 2.68 2.63 2.64 .03 2.5 2.3 2.35 .13 

2.62 2.4 2.2 

Ta 2.42 2.36 2.40 .03 2.43 2.53 2.48 .04 

2.42 2.47 2.49 

Th 26.3 26.0 26.2 .17 23.7 23.9 23.1 .129 

26.3 24.0 23.8 

u 46 4lt 46.3 .6 

47 

Za 42.9 50.2 46.7 3.6 

47.0 

lr '362 1265 321 50 690 790 738 50 1336 770 700 

Sc 35.1 34.5 34.9 .35 34.8 35.2 34.85 .25 

35.1 34.8 34.6 

La 109 110 109 1.2 uo 167 162.5 3.7 

110 159 164 

Ce 189 200 196 5.8 219 222 219.5 1.73 

198 218 219 

Nd 104 19 94 9,0 99 103 98.8 5.4 

88 102 91 

Sa 16.6 15.9 16.4 .44 12 13 14.0 3.4 

16.7 19 12 

Eu 3.13 3.10 3.13 ,04 3.11 3.18 J.lB .06 

3.17 3.20 3.25 

Sd 15.6 14.4 15.4 .92 

16.2 

Tb 2.19 2.92 2.91 .02 2.9lt 2.83 2.91 .06 

2.91 2.92 2.93 

Ta 1.21 1.23 1.24 ,04 

1.28 

Vb 8.1 8.2 8.4 .38 9.6 9.1 9.25 ,37 

8.8 8.8 9.5 

Lu 1.25 1.23 1.25 .02 1.13 1.11 1.12 .04 

1128 1.16. 1.08 

1 CoiTeCtion for fission product interference exceeds 20 percent of the reported value. 

30 
TABLE 11.-Determinations of lithium in clay reference samples by inductively coupled plasma spectroscopy (/CPS) and flame atomic 

absorption spectroscopy (F AAS) by the U.S. Geological Survey 

(In parts per million. x, mean; sd, standard deviation; -, no data) 

Deterainations by ICPS Deter•inations by FAAS 

2 3 4 X sd 1 2 3 4 X sd Avaragt 

NBS ... 97 990 960 960 960 968 15 860 850 870 880 865 12.9 916 

NBS·97b 500 500 480 480 490 11.5 450 440 450 450 448 s 469 

NBS·97a 520 soo 51() 510 SlO 8.2 450 460 470 460 460 8.2 485 

NBS-98 100 100 106 100 100 84 84 91 90 87.2 3.8 93.6 

HBS-9Bb 180 190 190 190 1BS 5 150 160 160 160 ISS 5 173 

NBS-9Ba 320 320 320 320 320 300 290 300 300 298 5 309 

NBS-679 61 60 63 62 61.5 1.3 51 54 53 52 52.5 1.3 57 

IPT-28 <S <S 6.7 6.4 6.6 (5 (5 (5 <5 (5 (5 6.6 

IPT-32 46 47 47 47 46.8 .5 41 41 40 42 40.8 .5 43.8 

IPT-42 <5 <5 7.4 7.6 7.5 (5 <5 6.6 6.6 6.6 7.0 

31 
Fe203 

NaaD 

K2D 

As 

Ba 

Co 

Cr 

Cs 

Sa 

Hf 

Hi 

Rb 

Sb 

Sr 

Ta 

Th 

u 

Zn 

Zt 

Sr: 

La 

Ct 

Nd 

Sa 

Eu 

Gd 

Tb 

T1 

Yb 

Lu 

TABlE 18.-Averages of laboratory means for NBS-97 and NBS-97b 

[Oxides in percent. Trace elements in parts per million. SS, spectroscopy ~m; -, no data) 

NBS-97 

USGS 

1976 

. 0.941 

258 

3.32 

576 

2.40 

38.7 

24.5 

1.40 

4.18 

36.9 

101.5 

1,368 

20.8 

33.2 

57.0 

119.3 

5.8 

1.24 

1.26 

6.72 

.95 

USGS 

1985 

0.949 

.077 

205 

3.34 

664 

2.24 

40.4 

23.0 

1.46 

4.34 

38.0 

7.22 

79.8 

1,788 

19.7 

27.9 

50.0 

1 19.7 

5.10 

1.26 

1.16 

.so 

&.20 

.91 

Three data in the laboratory mean. 8 Two data in the laboratory mean. 

wsu 

0.955 

.078 

.558 

4.S8 

281 

3.40 

624 

2.46 

54.9 

43.6 

34.3 

24.8 

1.63 

121 

3.84 

40.2 

8.73 

1,256 

20.1 

30.3 

56.6 

28.9 

5.44 

1,36 

1.07 

6.95 

1.38 

Average 

0.948 

.078 

.sse 

4.88 

248 

3.35 

621 

2.37 

55 

40.9 

34 

24.l 

1.50 

121 

4.12 

38.4 

7.98 

90.6 

1,470 

20.2 

30.5 

54.5 

23.3 

5.45 

1.29 

1.16 

.s 

6.59 

1.10 

usss 

1.245 

.085 

224 

3.62 

231 

3.34 

12.6 

32.3 

2.13 

3.97 

36.4 

7.4 

78.9 

500 

23.2 

24.8 

43.2 

2 26 

3.3G 

.742 

5.7 

.so 

.67 

4.58 

.754 

32 

wsu 

SS-1 

1.1~0 

.069 

.596 

10.8 

279 

3.56 

217 

3.56 

52.1 

13.4 

34.5 

31.8 

2.16 

LOS 

3.64 

36.3 

11.3 

429 

22.7 

22.7 

46.1 

17.1 

·3.09 

• 79 

.81 

~.58 

4.12 

NBS-97b 

wsu 

SS-2 

1.330 

.070 

.575 

8.34-

275 

3.50 

212 

3.50 

56.9 

13.5 

22.0 

29.7 

2.06 

127 

3.20 

36.7 

10.3 

329 

22.4 

23.6 

46.3 

20.2 

3.12 

.79 

.92 

4.55 

.859 

TDU Average 

1.165 1.225 

.075 

.SB6 

9.57 

259 

3.54 3.56 

231 223 

3.37 3.44 

54.5 

13.0 13.1 

28 

32.5 31.6 

2.12 

116 

3.68 3.62 

36.6 36.5 

9.4 9.6 

79 

420 

23.4 22.9 

23.4 23.6 

47.4 45.8 

16.8 19.2 

3.18 3.17 

.815 .784 

5.7 

I B:S ,84 

.72 .10 

4.92 4.66 

.82B .890 
TABlE 19.-Avemges of laboratory means for NBS-98 and NBS-98b 

(Oxides in percent. Trace elements in parts per million. SS, spectroscopy ~; -, no data) 

NBS-98 NBS-9Bb 

usss usss wsu Average uses wsu wsu lOlL Average 

1976 1985 SS·l SS-2 

Fe2o~ 2.~04 2.137 1.911 2.017 1.739 1.660 1.721 1.652 1.693 

Na20 .275 .261 .268 .204 .165 .179 .183 

K2D 3.019 3.019 2.741 2.868 2.804 

As 4.78 4.78 6.33 6.92 6.62 

Ba 655 653 731 680 652 709 773 710 

Co 13.8 14.6 13.4 13.9 15.6 15.0 14.6 15.1 15.1 

Cr 112 136 124 124 119 114 107 123 115.8 

Cs 10.8 10.6 10.5 10.6 15,6 16.0 15.7 16.3 15.9 

Sa 33.9 34 25.1 29.6 27.4 

Hf 7.1 7.6 7.67 7.46 6.53 6.85 6.78 6.93 6.77 

Ni 44.4 44 57.6 46.1 51.8 

Rb 153 157 151 154 170 169 133 178 162 

Sb 1.22 1. 70 1.59 1.50 1.60 1.63 1.79 1.67 

Sr 263 263 208 205 206 

Ta 2.22 2.22 2.00 2.15 1.98 1.87 1.63 1.98 1.86 

Th 19.4 21.2 20.8 20.5 20.1 20.2 20.1 21.0 20.4 

u 5.02 7.06 6.0 3.5 8.58 8.19 4.80 6.3 

ln 124 104 114 95 95 

Zr 335 1335 262 320 288 243 193 240 

Sc 22.8 23.1 21.8 22.6 22.1 21.7 21.1 23.0 22.0 

La 78.5 73.3 71.5 74.4 67.6 55.6 60.5 64.6 62.1 

Ce 135 130 130 132 104.9 109.4 105.2 117.2 109.2 

Nd 48.0 51.5 57.0 52.2 39.5 33.5 39.3 38.5 37.7 

Sa 9.98 9.89 8.81 9.56 6.34 4.97 4.61 6.64 5.6 

Eu 1. 73 1.78 1.81 1. 77 1.12 1.16 1.15 1.25 1.17 

Bd 9.08 9.1 s.s 5.8 

Tb 1.33 1.31 1.15 1.26 .85 ,8() .89 .92 .86 

Ta .63 .63 .475 .575 .52 

Yb 4.88 4.51 4.37 4.59 3.33 4.07 3.41 3.86 3.67 

lu .645 .70 .90 .75 .554 .99 .71 .64 ,72 

1 Three data in the laboratory mean. 

33 
TABLE 20.-Averages of laboratory means for NBS-679 and /PT-28 

(Oxides in percent. Trace elements in parts per million. SS, spectroscopy system; n, number of determinations;-, no data] 

NBS-679 IPT-28 

wsu wsu USGS TDU Averagt TDU wsu uses Average 

SS-1 SS-2 n=2 n=4 n=4 

Fe2o~ 11.93 12.06 13.37 12.89 12.56 0.76 0.750 0.785 0.766 

Na20 .169 .173 .193 .178 .025 .2 .025 

K2D 2.63 2.64 2.64 .044 .044 

As 9.37 9.98 . 9.18 1.99 1.99 

Ba 480 506 464 483 358 276 320 

Co 23.15 23.15 25.25 2S.OB 24.16 .52 .522 .41 .48 

Cr 94.5 92.9 103.2 110.5 100.3 140 129 132 132 

Cs 9.27 9.17 9.33 9.86 9.41 .3 .2 .2 

Sa 36.5 39.8 37.7 44.8 45 

Hf 4.09 4.21 4.18 4.53 4.25 31.6 31.3 29.8 30.8 

Ni 48.6 52.3 50.4 '30 30 

Rb 195 1~4 184 196 192 24.3 {16 4.3 

Sb .82 .eo .81 .81 .942 1.04 .99 

Sr 3 102 :}99 100 271 271 

Ta 1.30 1.18 1.34 1.36 1.30 4.10 3.76 4.19 4.0 

Th 13.4 13.54 13.85 14.75 13.89 50.2 48.5 48.1 48.7 

u 4.88 5.19 2.17 2.9~ 3.8 4.2 7.14 3.42 S.l 

Zn 113 113 3 14.1 14 

Zr lBl 139 184 168 837 1,258 1,050 

Sc 21.06 21.07 22.4 23.6 22.0 18.0 16.63 17.15 17 .l 

La 4B.l4 50.85 50.~ 50.22 50.0 181 197.8 182 188 

Ce 95.5 98,1 94.5 111.8 100 378 339.8 327 342 

Nd 40.5 46.9 43.9 49.0 45.0 129 11B.B 111 118 

Sa B.16 7.34 8.91 9.59 8.5 17.4 15.0 16.4 16.0 

Eu 1.67 t. 73 1.66 l. 91 1.74 2.80 2.58 2.48 2.58 

Sd 7.3 7.3 9.85 9.8 

Tb 1.04 1.15 1.18 1.27 1.16 l. 21 1.03 1.06 1.09 

Ho 2 1 .. 75 1. 75 

T1 :s.49 .61 ,56 .70 .59 .63 

Yb 5.43 3.32 3.35 3.96 4.02 5.22 4.72 4.45 4.71 

Lu 4 1.21 .60 .54 .64 .59 .90 .94 .75 .86 

1 One datum in the laboratoey mean. 

8 Two data in the laboratoey mean. 8 1bree data in the laboratoey mean. 4 Not included in the average. 

34 
TABLE 21.-Averages of laboratory means for /PT-32 and /PT-42 

[Oxides in pereent. Trace elements in parts per million. n, numer of determinations; -, no data) 

IPT-32 IPT-42 

TOU wsu USGS Average TDU wsu usss Average 

n=2 n=4 n=4 n=2 n=4 n=4 

FezD~ 3.42 3.30 3.50 3.40 1.12 0.98 1.02 1.02 

NazO .18 .17 .18 .03 .03 

K20 .79 .79 :st .51 

As 7.48 7.49 1.67 1.67 

Ba 480 366 420 234 226 230 

Co 4.59 4.36 4.42 4.43 2.77 2.43 2.39 2.48 

Cr 62 ~9.2 56.1 56.5 80 68.2 68.5 70.7 

Cs 3.06 3.06 2.89 2.99 1.56 1.48 1.32 1.43 

Sa 39.5 40 33.5 34 

Hf 18.6 17.8 16.6 17.5 5.76 5.53 5.11 5.41 

Ni 1 25.6 26 32.1 100 32 

Rb 39 37.4 34.4 36.5 26 24.8 22.2 24.0 

Sb .60 .46 .53 .so 2 .57 .70 

Sr lOB 108 128.3 (300 128 

Ta 3.80 3.42 3.74 3.62 1.40 1.25 1.34 1.32 

Th 35.0 33.4 32.6 33.4 14.6 13.5 12.8 13.4 

u 7.8 8.21 5.45 7.0 1.8 3.27 1.34 2.2 

Zn 58.0 58 24.6 2~ 

Zr 503 685 590 266 230 248 

St 16.8 15.46 15.62 15.8 19.5 17.3 17.1 17.7 

La 106 110.9 104.3 107.3 64.6 69.1 59.7 64.4 

Ca 160 146.6 140 146.6 110 96.2 90.3 96.6 

Nd 66.4 58.4 59.8 60.6 56.8 49.7 48.1 50.5 

Sa 10.8 9.23 9.86 9.80 10.9 9.56 9.95 9.98 

Eu 1.74 1.~9 1.51 1.59 2.78 2.47 2.27 2.45 

Sd 7.65 7.6 LS.2 8 

Tb 1.06 .sa I 97 .95 1.33 1.09 1.13 1.15 

Ta .38 2 .40 .39 .66 1 .48 ,57 

Yb 3.09 3.36 2.80 3.08 4.07 3.66 3.68 3.75 

Lu .49 .63 .43 .52 .66 .82 .52 .67 

11\vo data in the Jaboratoty mean. 1 Three data in the laboratory mean. 

35 
TABLE 22.-Provisional averages for the 10 clay reference samples 

(Oxides in percent. Trace elements in parts per million. -, no data; lREE, summation of average rare earth element contents) 

Flint Plastic Miscellaneous 

NBS-97 NBS-97b NBS-97a NBS-98 NBS-98b NBS-98a IPT-32 NBS-679 IPT-28 IPT-42 

FezD:s 0.95 1.22 0.44 2.02 1.69 1.3 3.40 12.56 0.77 1.02 

NazO .OB .08 .OS .27 .18 .08 .18 .18 .02 .03 

KzO .56 .59 3.02 2.80 .79 2.64 .04 .51 

As 4,89 9.57 4.79 6.62 7.48 9.18 1.99 1.67 

Ba 248 259 607 680 710 481 420 483 320 230 

Co 3.35 3.56 4.21 13.9 15.1 11.8 4.43 24.16 .48 2.48 

Cr 621 223 197 124 116 229 58.5 100 132 70.7 

Cs 2.37 3.44 l.SB 10.6 15.9 6.23 2.99 9.41 .2 1.43 

Sa 55 54.5 34 27 40 37.7 45 34 

Hf 40.9 13.1 12.0 7.46 6.77 7.69 17.5 4.25 30.8 5.41 

Li 9.16 4,69 4.85 93.6 173 309 43.8 57 6.6 7.0 

Ni 34 28 44 52 26 50 30 32 

Rb 24.1 31.6 12.2 154 162 34.9 36,5 192 4.3 24 

Sb 1.50 2.12 .84 1.50 1.67 2.47 .53 .81 .99 .70 

Sr 121 116 263 206 108 100 271 128 

Ta 4.12 3.62 3.12 2.15 1.86 2.45 3.62 1.30 4.0 1.32 

Th 38.4 36.5 32.5 20.5 20.4 24.8 33.4 13.88 48.7 13.4 

u 7.98 9.6 6.9 6.0 6.3 46 7.0 3.8 5.1 2.2 

Zn 90.6 79 45 114 95 47 58 113 14 25 

Zr 1,470 420 550 320 240 320 590 169 1,050 248 

St 20.2 22.9 31.6 22.6 22.0 34.9 15.8 22.0 17.1 17.7 

La 30.5 23.6 98.9 74.4 62.1 140 107.3 50.0 ISS 64.4 

Ce 54.5 45.8 199 132 109.2 209 146.6 100 342 96.6 

Nd 23.3 19.2 86 52.2 37.7 96.7 60.6 45.0 118 50.5 

Sa 5.45 3.17 20.3 9.56 5.6 15.0 9.80 s.s 16.0 9.98 

Eu 1.29 .78 3.76 1.77 1.17 3.16 1.59 1.74 2.58 2.45 

Sd 5.7 18 9.1 5.8 15.4 7.6 7.3 9.8 B 

Tb 1.16 .84 2.77 1.26 .86 2.91 .95 1.16 1.08 1.15 

Ho 1.8 

T1 .8 .70 1. 0 ,63 .52 1.24 .39 .56 .63 .57 

Yb 6.59 4.66 7.37 4.59 3.67 8.9 3.08 4.02 4.71 3.75 

Lu 1.10 .89 .99 .75 .72 1.18 .52 .59 .86 .67 

rREE 124.69 105.34 483.09 286.26 227.34 493.49 338.43 218.87 683.66 238.07 

36 
TABLE 23.-Elemental ratios for averages for the 10 clay reference samples 

(Trace elements in parts per million. Fe. K, and Mg in percent used for ratio. -, no data) 

Flint Plastic Miscellaneous 

NBS·97 NBS-97b NBS-97a NBS-98 NBS-9Bb NBS-98a lPT-32 NBS-679 IPT-29 JPT-42 

Largt cations 

K/Rb 1 1.91 1.55 3.44 1.63 1.43 2.47 1.81 1.14 0.77 1.75 

K/Ci .20 .14 .26 .24 .15 .14 .22 .23 .16 .30 

K/Ba2 l.BB 1.89 .69 3.69 3.27 1. 79 1.57 4.53 .10 1.84 

Rb/Cs 10.17 9.19 7.72 14.53 10.19 5.58 12.21 2D.40 21.5 16.79 

Rb/Sr _.20 .27 .59 .79 .34 1.92 .02 .19 

High·valtnte eleaents 

Zr/Hf 35.8 32.1 45.1 42.1 35.4 41.6 33.7 39.5 34.1 45.7 

Th/U 4.91 3.80 4.71 3.42 3.24 .54 4.77 3.65 9.55 6.09 

Th/Ta 9.32 10.08 10.42 9.53 10.97 10.12 9.23 10.68 12.18 10.15 

Hf/Ta 9.93 3.62 3.85 3.47 3.64 3.14 4.83 3.27 7.70 4.U 

Ferroaagnesian eleaents 

Co/Fe 5.08 4.19 13.58 9.79 12.80 12.97 1.86 2.75 .89 3,49 

Co/ttg 21.3 46.8 32.0 5.06 18.8 20.0 207 

Ni/Ca 10.15 7.86 3.16 3.44 5.87 2.07 62.5 12.90 

Ni/Kg 216 101 111 1,250 2,667 

Li/Mg:s 58.3 53.9 2.16 12.2 1.86 2.75 5.83 

1 Xlol. 

It X101• 

1 Xlo-11. 

37 
TABLE 24.-Provisional means for samples normalized to the grand mean for an element 

[IREE, summation of average rare earth element contents; -, no data] 

Flint Plastic Miscellaneous 

NBS-97 NBS-97b NBS-97i NBS-98 NBS-9Bb NBS-9Sa IPT-32 NBS-679 IPT-28 IPT-42 

Ba 0.56 0.58 1.37 1.53 1.60 1.08 0.95 1.09 0.72 0.52 

·Co .40 .43 .so 1.66 1.81 1.41 .53 2.89 .06 .30 

Cr 1

3.32 1.19 1.05 .SB .62 1.22 .31 .53 • 71 .38 

Cs .44 .63 .29 1.96 2.93 1.15 .55 1.74 ,04 .26 

Hf 1

4.41 1.41 1.29 .so .73 .83 1.89 .46 '3.32 .sa 

Li 1

5.00 2.56 2.65 .51 .94 1.69 .24 .31 .04 .04 

Rb .36 .47 .18 2.28 2.40 .51 .54 2.84 .06 .36 

Sb 1.14 1.62 .69 1.14 1.27 1.88 .40 .62 .76 .53 

Sr .74 .71 1.60 1.26 .66 .61 1.65 • 78 

Ta 1.35 1.18 1.02 .70 .61 .so 1.!8 .42 1.31 .43 

Th 1.36 1.29 1.15 .73 .72 .88 1.18 .49 1.73 .48 

u 1.31 1.57 1.13 .98 1.03 17.54 1.15 .62 .84 .36 

Zn 1.33 1.16 .66 1.67 1.40 .69 .85 1.6& .21 .37 

Zr 14.12 1.19 1.54 .88 .67 .90 1.66 .47 12.95 .70 

IREE .40 .33 1.39 .91 .72 1.57 1.07 .69 2.17 .76 

1 Provisional mean for this element not included in the grand mean. 

TABI.E 25.-Certified values of the major and minor oxide contents from Certificates of Analysis for four NBS and three IPT 

clay reference samples 

[In percent. Samples dried for 2 hours at 140 "C. LOI, loss on ignition at 1,000 oc. n.d., not determined] 

NBS-97 NBS-97a NBS-98 NBS-98a IPT-28 IPT-32 IPT-42 

SiD2 42.87 43.67 ~9.11 48.94 45.1 51.8 51.9 

AlzD~ 38.77 39.79 25.54 33.19 37.& 2B.S 32.2 

Ft20:s .99 .45 2.05 1.34 .83 3.46 1.09 

MgO .21a .15 .72 .42 .04 .39 .19 

CaD .10 .11 .21 .31 .09 .17 .05 

Na2D .07 .037 .2b .082 .02 .16 .02 

K~o .54 .50 3.17 1.04 .01 .SCl .47 

TiOz 2.'38 1.90 1.43 l.hl 2.04 1.~9 .9o 

P2Ds .08 .3b .08 .11 .15 .13 .07 

HnO • 0~2 n.d. .oos n.d • n.d. n.d. n.d, 

LOI 13.35 13.32 7.28 12.44 13.9 12.6 12.9 

38 ~u.S. G.P.O. 1987-181-407:60027