Document 5DQQ46OjMnNe4yYaVvm4ZqxN8
FILE NAME: RT Vanderbilt (RTV)
DATE: 1976 Oct
DOC#: RTV126
DOCUMENT DESCRIPTION: Govt Inspection Report - Industrial Hygiene Study of the Gouverneur Talc Cov Number One Mine & Mill
' t G o io c sn
FINAL REPORT^
INDUSTRIAL HYGIENE SIUDY OF THE GOUVERNEUR
TALC COMPANY, NUMBER ONE MINE AND MILL J B a lra a t, New York
Volume I I
Talc Bulk Sample Analyses By NIOSH, w.c. McCrone and Mt. S in a i S chool o f M edicine
Department of Health , Education, and Welfare Center for Disease Control
National I n s t i t u t e or Occupational Safety and Health :ion. o f S u r v e i l l a n c e , Hazard E v a lu a tio n s and F i e l d S tu d i e s
C in c in n a ti, Ohio
A m - C o/r> rr)~ 3 | }2.
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VV. ' wV
- vt;\ E l e c t r o n M icroscopic A nalyses o f R.T.
V anderbilt Talcs C ollected from Talc Suppliers
Analyaca Performed By John H. Dement Ralph D. Zumwalde
Date October , 2976
Department o f H e a lth , E d u c a tio n , and 'Welfare Center for Disease Control
National In s titu te for Occupational Safety and Health Division of S urveillance, Hazard Evaluations and F ield Studies
C in cin n ati, Ohio
IN T R O D U C T IO N
As a p a r t o f ongoing re s e a rc h by th e N a tio n a l I n s t i t u t e for Occupational
S afe ty and H e a lth (NIOSH) concerning h e a l t h e f f e c t s o f o c c u p a tio n a l exposures to t a l c and as requested by the Occupational S afety and Health A dm inistration,'-
seven b ulk t a l c s produced by th e R.T. V a n d e r b ilt were an alyzed f o r a s b e s to s
content. These ta lc s were obtained from independent ta lc su p p lie rs and have
been " c e rtifie d " by V anderbilt not to contain asbestos.
*
for asbestos content by an aly tical electro n microscopy.
Samples were analysed The fol.lov nq p a ra
graphs describe sample preparation! and a n a ly tic a l methods employed along with
results.
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METHODS
Given in Table 1 are d e sc rip tiv e d ata f o r the 7 ta lc s obtained and analyzed in c lu d in g source and NIOSH sample number assigned.
Samples fo r transm ission e le c tro n m icroscopic analyses were prepared by d i s
p ersin g the powder samples in e th y l a c e ta te by u ltra s o n e r a tio n . Approximately
10 ng o f each powder was p l a c e d i n 10-20 ml. of e t h y l a c e t a t e follow ed by
vigorous u ltraso n e ra tio n f o r 10-15 minutes using a c e l l d is ru p te r. Samples were prepared using a micro c a p illa ry tube to place a drop of the solu tio n
o n to 200 mesh Formvar/carbon s u b s t r a t e copper e l e c t r o n m icroscope g r i d s . The
e t h y l a c e t a t e was allowed t o e v a p o ra te i n a l a b o r a t o r y c l e a n hood, j f n e c e s s a r y , an a d d itio n a l drop o f th e s o l u t i o n was used to in s u r e s u f f i c i e n t m a t e r i a l
for e f f ic ie n t analysis by e le c tro n microscopy. same manner as the samples.
Blank g rid s were prepared in the
Samples were an a ly z ed by f i r s t s c a n n in g th e e n t i r e g r i d a t low m a g n i f i c a t i o n to a s c e r t a i n th e s u i t a b i l i t y o f th e p re p a r a tio n f o r a n a ly s i s . At a m ag n ifica tio n o f approxim ately 17,00OX, a l l p a r t i c l e s w ith an a s p e c t r a t i o (le n g th to d iam eter) o f 3 to 1 o r g r e a t e r were i d e n t i f i e d u s i*n g b o th s e l e c t e d are a e le c tro n d iffr a c tio n and energy d isp e rsiv e microchemical a n a ly s is fo r f i b e r i d e n t i f i c a t i o n . A t o t a l o f 25 t o 50 i n d i v i d u a l f i b e r s were so analyzed f o r each sample, a JEOL, JEM 100B t r a n s m i s s i o n /s c a n n i n g e l e c t r o n microscope equipped w ith an EDAX energy d i s p e r s i v e x - r a y a n a ly z e r was used f o r a l l a n a l y s e s . Electron micrographs of typical fib ers along with th e ir d iffra c tio n patt- rns and x -ra y spectrum were re c o rd e d ' f o r each sample.
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Table i
Sources o.f R.T. V a n d e r b i l t T a lc s Produced a t t h e Gouvemeur T alc Company, Number One Mine
and M ill and obtained from Suppliers
Nytal 300 N ytal 400
5x 325 X pi 3x
1 Crone Chemical P.O. Box 14042
' Houston TexaB 77021
P a u l c r a z i e r Company 1115 S ilv e r 5 t. Houston Texas 77067
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001 002
003 004 oos 006 007
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RESULTS AND DISCUSSION
R e s u lts o f a l l a n a ly s e s $re shown i n Table 2 and t y p i c a l micrographs o f . fib ers in these samples along with elec tro n d iffra c tio n p a tte rn s and x-ray s p e c tra are shown i n t h e Appendix. Based on t h e i r s e le c te d a rea e le c tro n d iffractio n patterns, fib ers vera c la ssifie d as p o sitive amphiboles, positive c h ry so tile , non-asbestos o r "ambiguous" meaning th a t the p a tte rn was n o t s u f f i c i e n t l y c l e a r f o r p o s i t i v e i d e n t i f i c a t i o n . The energy d i s persive x-ray sp ectra were used to c la s s ify the amphiboles as to type and for fu rth e r confirm ation of ch ry so tile id e n tific a tio n by e le c tro n diffraction.
As shown i n Table 2, r e s u l t s o f t h e s e a n a ly s e s show a l l t a l c s a n a ly z e d t o be o f e s s e n t i a l l y t h e samte f i b e r co m position. The major f i b e r component i s a sb e stifo rm a n th o p h y l l it e , ranging from 67 to 084 o f the f i b e r s p r e s e n t in add itio n to fibrous trem cilite (4 to 12%). Aspect r a ti o s fo r these f i b e r s ranged up t c 1000 to l , w l t h th e lo n g e r , t h in n e r f ib e r s b eing a n t h o p h y l l it e . Trace q u a n t i t ie s of c h r y s o tile were found i n two o f the samples. C h ry so tile f i b e r s observed were s m a ll i n d ia m e te r (< 0 .1 uml and s h o r t i.n l e n g t h (most < 1.0 urn).
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Table 2
Summary o f NIOSI! E lectron M icroscopic Analyses of Talc Produced at the Gouverneur Talc Company Number One Mine and Mi l l
Samples Obtained Frcm T alc S u p p li e r s
Talc Sample
Range of Fiber. Aspect ` Ratios
Fiber Id entification (Percent)
P o s itiv e Amphiboles Tremolite Anthophyllite
Positive C h ry so tlle
Nytal 400
3/1 to 1000/1
8
88
N.D.
Nyt a l 300
3/1 to 100/1
12
72
N.D.
5x
5/1 to 100/1
11
80
Trace
X
8/1 to 80/1
0
80
H.D..
3x
5/1 to 100/1
12
67
N.D.
FT
3/1 to 50/1
16
72
N.D.
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325
3 /1 to 50/1.
4
88
Trace
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* Selected area diffraction patterns not su ffic ie n t for positive Iden tificatio n
HD - None Detected
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CONCLUSIONS
Using present " s ta te -o f-th e r t" techniques fo r asbestos f io e r analyses a ll 7 talcs analyzed demonstrated large quantities of asbestifosm'-tremolite and a n th o p h y llite to presen t. Only tra c e q u a n titie s o f c h ry s o tile wera detected in 2 of the 7 ta lc s . Based on these analyses, a l l ta lc s analyzed should be la b e le d w ith th e osha a s b e s to s w arning l a b e l.
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APPENDIX i Electron Micrographs, Electron D iffractio n Pat'terns and X-Kay S pecta f o r T y p ic a l F ib e r s i a R.T. V a n d e r b i l t T a l c s .
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Dtpartntrtlef Community?H,tlkirv
A p r i i 29 M976
Mr , John Dement N10SH Room 527 Post Office Building F if t h and Wslnut S tr e e t C in c in n a ti, Ohio 45202
Dear Mr. Dement :
T h is re p o rt covers t h e r e s u l t s of a n a ly s e s of seven NYTAL sam ples; .400, 3 5 , X, E'T, 300 . 325 and 5X.
The seven samples were analyzed q u a n t i t a t i v e l p f o r t h r e e v a r i e t i e s o f asb e sto s m in e ra ls - c h r y s o t i l e , a n t h o p h y l l i t e and t r e m o l i t e and a l s o f o r q u a r tz . Ana ly tic a l techniques included polarized o p tical microscopy, x-ray d iffra c tio n , tran sm issio n e l e c tr o n microscopy and scanning e le c tr o n microscopy w ith energy dispersive a n a ly tic a l systems.
Q u a n tita tiv e d e term in a tio n s by x - r a y d i f f r a c t i o n o f th e fo u r m in e ra ls in ques t i o n were made by comparison w ith d i l u t i o n s t a n d a r d s o f t h e s e m in e ra ls . A uniform method o f back mounting in which t h e sample i s remounted and r e - r u n fo u r times at id e n tic a l instrum ental s e ttin g s over d iag n o stic r e f le c tio n s has been shown t o be r e p r o d u c i b l e and a c c u r a te . Q u a n t i t a t i o n o f t h e s e m i n e r a ls was a ls o done by x - r a y d i f f r a c t i o n in t h e s t e p - s c a n , f i x e d count mode.
In teg rated i n t e n s i t i e s fo r d ia g n o stic x -ray r e f le c tio n s were measured using both t h e back-mounting and s t e p - s c a n te c h n iq u e s . When r e f e r r e d t o c a l i b r a t i o n curves prepared by each te c h n iq u e , t h e NYTAL unknowns showed egreem ent, av e ra g in g about 10% stan d ard e r r o r . The r e s n l t s a r e 2s fo llo w s ;
NYTAL 400 ft 3x
SERPENTINE PHASE % 14-18
31-35
TREMOLITE
% 24 32
.ANTHOPHYLLITE
2-3 not detected
QUARTZ
% 7-10 7-8
It
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ft
FT
26-30 26-30
50-60 * 17
not determined not detected
9-10
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not detected
300
14-18
18 .
4-5
9 -io/tC ''-AY i \
n 325
19-23
24
5--7
3 -4 1.
M 5x Because of the
14-18
27
targe amounts of tre m o lite
7-9 (50-605) p re sen t
8-9 _ X '
in sample X unthophyl-. s X / '
l i t e could not be q u a n t i t a t i v e ly d eterm in e d by x - r a y d i f f r a c t i o n . Hcwevr;^ni?rc5 > > ^
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.y s i s of f i b e r s on t h e SEM shdws t h a t a n t h o p h y l l i t e i s p r e s e n t. X -ray
.ndicated the'presence of serpentine phases in a l l samples, but the
r a l s p e c ie s o f t h i s group which' in c lu d e # c h r y a o t i l e , antlgorifc e and,
>uld not be p o s i t i v e l y i d e n t i f i e d although t h e l a t t e r m o s t c l o s e l y
-ray p a t t e r n s . Examination by TEJt and iEM w ith energy d i s p e r s i v e
em confirmed t h s t v i r t u a l l y a l l o f t h e s p e r p e n tin e phase c o n s i s t s
C h ry s o tile was d etec ted by e le c tro n microscopy in the samples, .
:ylng photomicrographs)/
._
eri prepared f o r a n a ly s is by tra n s m is s io n e le c tr o n microscopy by
chnique which did not a l t e r t h e s i z e d i s t r i b u t i o n o f p a r t i c l e s . Two
t h r e e Brf g r i d s were scanned at. 25,000; m a g n if ic a tio n on a H ita c h i
cope. F ib ro u s p a r t i c l e s were abundant in a l l seven samples". , Morpbol-
ystal cleavage c h a rc c te ris tits indicated the presence 'of amphibvles.
fied-by observing a typical layer-type selected area .electron d iffra c -
on the f i b r o u s p a r t i c l e s . The l a y e r l i n e distaftfee normal t o th e
:is was c o p s is t/jn tly observed t o be 5.3X, which i s c h a r a c t e r i s t i c of
:peat of amphiboies.. These p a r t i c l e s were" d efin e d as amphibole and
^ on a g r i d f a c s i m i l e re c o rd e d . The specimens were t r a n s f e r r e d t o
e c tro n microscope (CVflRSCAN) equipped w ith an energy d i s p e r s i v e x - r a y
The amphibole .p articles w e re analyzed by point count and were found
two g e n e ra l m orph o lo g ical-ch em ical ty p e s o f p o p u la tio n s which p e rm its
fined as d iffe re n t m ineral species, The'long, th in fib e rs (aspect
more) showed Si/Mg in r a t i o s c o n s i s t e n t w ith a n t h o p h y l l i t e composi-
f ib e r s contained l i t t l e or no iron. Short p rism atic f i b e r s with
. from about 3/1 to S /i^ c o n ta in e d Sl/Ca/Mg p roportions c o n s is te n t
e . No iro n was found i o t T e e v a l i t e .
,,,, .
A r t h u r S. Rob! , ph.D. Environmental Sciences Laboratory
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