Document X7RVryYEZ43KXD0BroLRDkvRK
A
S e p te m b e r 16, 1975
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The Cosmetic, Toiletry and Fragrance Association, Inc.
1133 16th STREET. N.W.; WASHINGTON. D, 20Q5 -`202/331-1770 TELEX 69-2673
Jp.mcr H M'jriul
Prrc.d-.-.'if Norman F, E^trin. Oh.D.
Wee Pj-c -- St-fvict-
M a r c h 15th, 1976
Mr.. Heins; J. Eiermanri
_
F o o d -a n d D r u g A d m i n i s t r a t i o n
200 C Street, S.W. *. .
Washington, D,C. 20204
On M a r c h 11th, 1976, Mr, Eierniann
-- the CTFA Talc Subcommittee-mot to discuss the current sta tus of talc It was recognized'that a need exists o o r r i n g t o your a t t ^ t L n a -profile of the analyses f o r asbestos form materials in talc used in the U.S. production of c o s m i c . , and toiletry products.
the freeaem item eont^inatit, by
asbestos form materials of cosmetic talc products.
I n d i v i d u a l c o m p a n i e s a r e .more, t han w i l l i n g t o d i s c u s s the detailed data with you at your convenience-
N o r m a n F, Estrin, Ph.D. Vice President - Science
N F E :j j "
Attachments
FORMERLY THE TORET GOODS ASSOCIATION, INC
FOR IMMEDIATE RELEASE M a r c h 8, 1976.
F O R F U R T H E R I N F O R M A T I O N CONTACT ; N o r m a n F. Estrin, Ph.D. Anita Curry
...202/33 - 17-7Q
ASBESTOS IN t a l c
The C T F A has an expert. Talc Subcommittee, which has'been working for the
p a s t t w o years, o n the d e t e c t i o n of a s b e s t o s in talc.. -, T h i s S u b c o m m i t t e e
has. d e v e l o p e d r e p r o d u c i b l e research, m e t h o d s for the d e t e c c i n of f i b r o u s
'minerals in cosmetic talc- CTFA has performed-.repeated analyses on the
talcs r e p r e s e n t i n g m o r e t h a n 85% of' the v o l u m e of c o s m e t i c t a l c sold- in .
the U n i t e d tatos. C h r ysotile Asbe s t o s has not been found in any of
these talcs.
V
.
CTFA has also developed a specification for cosmetic crade talc and has
m a d e i t s s p e c i f i c a t i o n s a n d t est m e t h o d s a v a i l a b l e to. the F D A and t h e -,
a p p r o p r i a t e OTC. p a n e l s .
'.
A l t h o u g h C T F A h a s n o t h a d the- o p p o r t u n i t y to r e v i e w the Mt. S i nai d a t a .
fr methodology,, we believe the results of the analysis on asbestos fiber
c a n b e m i s i n t e r p r e t e d because: (1) t h e d a t e s of the sam p l e s are u n k n o w n
and. d o n ' t r e p r e s e n t c u r r e n t l y m a n u f a c t u r e d products,
other raw
materials represented in the formulation can confuse the test.results,
(3) p r e v i o u s Mt. S i n a i t e s t r e s u l t s on some U n i t e d K i n g d o m f o r m u l a t e d
t a l c p r o d u c t s h a v e b e e n d i s p u t e d by well r e c o g n i z e d e x p e r t s in this field
For t hese r e a sons the C T F A crit.ioally questions, the validity ox the
Mt. Sinai conclusions on the alleged presence of asbestos like particles.
On the issue of nickel detected in talc, one Of our member companies has e x t e n s i v e l y s t u d i e d t h e i r talc. T h e y h a v e r e p o r t e d that, the n i c k e l is p e r m a n e n t l y b o u n d ..within t h e m o l e c u l a r l a t t i c e of t h e t a l c a n d t h e r e f o r e cannot be extracted.to react with body tissues.
16?^ bYC$TPtrET
WOti oft1
2- -
T h e work by Dr. Wagner on the occurence of fibrosis in rats was only o n e of s e v e r a l studies on t h e safety, of c o s m e t i c .talcs r e v a a l e d last S e p t e m b e r , A lif e t i m e i n h a l a t i o n .study in hamsters, e x p o s e d to. talc. . .. reported no fibrosis. An epidemiological study on'talc workers showed no evidence of increased cancer despite high occupational exposure,over a 3o-year period. All of1this information has been presented at world- . wide scientific meetings, published in the proceedings and forwarded
to the FD.
T h e C T F A .d o e s n o t f e e l t h a t c o n s u m e r t a i n p r o d u c t s r e p r e s e n t any h a z a r d
to the c o n s u m e r .
'
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( 'S ) / " ) The Cosmetic,Toiletry and Fragrance Association, Inc.
Vit/'
1133 15th STREET N.W., WASHINGTON, O.C.2005 202/331-1770 TELEX 89-2673
vrames H.Merritt
Pr*3lil*at
Norman F. Estrin, Pfi.O,
Viet Prtinttat- Sconce
minute s
OTTA TALC TASK FORCE
A meeting of the CTFA Talc Task Force was held on March 11th, 1976
I a t the C T F A o f f i c e s iri W a s h i n g t o n , D.C. T o s e xn a t t e n d a n c e were: i
G e o r g e Sandland, Bristol-Myers C o m p a n y (Chairman)
J o h n E, Clements, Pf i zer, Inc.
Ray K r a m m e f , W h i t t a k e r , Clark- & Daniels
r n m n a i ,v
George Lee, Johnson & Johnson Baby Products company
M o n r o e M e s s i n g e r , C h e s e b r o u g h - P o n d 's Inc.
Roderick A . M u n d y , Sterling Drug Inc. . L o uis D. Murino, C y p r u s industrial Mine r a l s Company
D.R. Fetterson, Johnson & Johnson Baby Products Company
Fred Roe sch, Whit taker, Clark & Daniels Robert Rolle, Johnson & Johnson B a b y Products Company
J o h n P. Beheiz, J o h n s o n & J ohnson B a b y Products C o m p a n y
M a u r i c e Siegel, Fabefge, Inc.
.
j;C. Simko, jr,, Colgate-Palmolive company
Harold Stanley, Pfizer, Inc,
Ian Stewart, W a l t e r C. McCrone A s s o c i a t e s
Robert Suffis, The Mennen Company ,
S. T h o m p s o n , R^T, V a n d e r b i l t & C o m p a n y
John J Travers, Avon Products, Inc..
W i l l i a m e, Waggoner, Johnson.& Johnson .Baby Products Company
N o r m a n F, Estrin, C T F A
Mr. Sandland opened the meeting and proceeded with th agenda.
1. S t a t u s Review. ;
A. Talc Standards,, and Methods
1
Copies of the proposed specification and methods, plus c o p i e s of a l e t t e r to. Dr. S c h a f f n e r w ere d i s t r i b u t e d to task force members.
B. A -status r e p o r t .(dated'. M a r c h tftn, .1976'i, pre p a r e d b y . Dr, Patterson, on cosmetic talc status was distributed to those present,. * a copy of an article by
; '
CONTINUED ON NEXT PAGE
Dr, Rahl a n d Dr. Arthur M. Langer on " I d e n t i f i c a t i o n
a n d Q u a n t i t a t i o n of A s b e s t o s in -Tal" w a s d i s t r i b u t e d
a s it appp3i<; -in E n v i r o n m e n t a l H e a l t h P e r s p e c t i v e s ,
_
V o l u m e 9, 197 4 > pp- .95-109. Also, a c o p y of the c o r r e c t i o n
t o t h e M a r c h 8, 1 9 7 6 W a s h i n g t o n Post a r t i c l e o n talc
'
and the summary of the.draft Talk Paper anticipated from
the FDA was distributed to those present.
C . Lewin Samples
Mr ; Sandland summarized the contents of the November, 1975 letter from Hehry D a v i s (FDA) r e q u e s t i n g C T F A . apply its methodology to several of Dr. Lewin samples provided on a coded basis.- The results of the analyses w e r e described bv Dr. Roll.
2 ; Mt. Sinai Analyses on Old Production Samles
Dr. F e t t e r son g a v e d e t a i l e d b a c k g r o u n d -ri. Dr- L a n g e r 's work. H e s t a t e d t h e o b j e c t i v e of th- t a s k f o r c e s h o u l d b e to deY 0lop a n d c o l l a t e d a t a t h a t w o u l d l ead to a p r e s e n t a c i n before the'Miscellaneous External* Panel, in order to attempt to h ave talc placed in Category-I. The r e s u l t s of Dr, Pooley s analyses,, sponsored by Johnson & Johnson, were summarized. .
It w a s .r e p o r t e d t h a t .D r . L a n g e r -performed h i s a n a y l s e s o n sara p i e s - p u r c h a s e d in 197 3. Mr. S i m k o d e s c r i b e d a m e e t i n g .between
h i mself and.Dr, Langer on Tuesday. He estimated^ the sample ; o f " C a s h m e r e B o u o u e t " t e s t e d was- p r o b a b l y p r e - 1 `17 0 sample. Mr. M U n d v (Sterling) r e p o r t e d o n his 'contact's w i t h r. Lang e r , and stated the Sample. Dr, L a n g e r tested w a s from 1970 production.
-3 , R e c e n t P r o d u c t i o n D a t a
It w a s agreed' by the t a s k 'force that it w o u l d be extremely beneficial if induvidual companies, could provide data to the F D A o n r e c e n t p r o d u c t i o n . -.Most c o m p a n i e s p r e s e n t i n d i c a t e d that they possess such data and would be willing to provide t h e - d a t a . Mr. M e s s i h g e r ( C h e s e b r o u g h - P o n d 's) sta t e d he w o u l d h a v e .'tb c o n f i r m this w i l l i n g n e s s w i t h his m a n a g e m e n t . It w a s suggested, each; c o m p a n y p r e p a r e a letter,, a d d r e s s e d to Dr. Estrin,-with.a summary of the data on recent production for their products and a commitment to set-up a subsequent
meeting-'with F D A ' t o d i s c u s s t h i s data, in d e t a i l , if FDA so
d e s i r e s . This- l e t t e r s h o u l d b e d e l i v e r e d to Dr. E s t r i n b y Monday,' March I5th. Subsequently, a-meeting was set-up for that. M o n d a y , M a r c h 15th-, at- the- C T F A of f i c e s , w i t h a m e e t i n g at F D A to.be held in the afternoon.
4 . .C T F .Study on Current-production -
A d v a n t a g e s .and d i s a d v a n t a g e s - o f having. C T F A c o n t r a c t an i n d e p e n d e n t .laboratory'.to do .t e s t s on c u r r e n t production, sampies was discussed. It was noted that such data would no doubt be useful, not only in discussions with FDA, but also as part of a presentation to the Miscellaneous External Panel and, perhaps, to other panels as well; it was suggested the CTFA methodology be utilized for such a task, but that TEM be used on those samples that have been shown to be positive
CONTINUED ON NEXT "PAGE
DCST # .IEUIR # PRODUCT
1338 .
72
1339
-77
1340
96
1341
97
1342
101
1343
' 1024
1344
143
1345
144B
1.346
151
1347
154
1348
15 7A
1349
160
1350
163
1351
75
1352
' 173A
Lady E s te r Face Powder, Rachel Touch, and Glow Face Powder B la n c h a rd 's D usting Powder Born W ild D usting Powder, Del Labs T ai Winds Sp ra y T a lc , Avon Tosca D usting Powder Piri-Zow T a lq u e , P e r f . B e a u ty P ro d ; O v e rto n ' s "H igh B ro w n ". Face Powder E a r ly Am erican Old S p ic e Talcum Powder B is m o lin e M edic a ted Powder M a vis. Im p o rted ' Ta 1cum Avon Beau ty Dust R e f i l l - Charism a P tn a u d Clubman T a lc OH 1 de London T a 1 c , Y a r d l e y Corsage D usting Powder
TREMOLI TE
LE riIN . DGST X-RAY 1 : (OM) ____
chrysotile"
LEtflN
DOST
X-RAY
ND
2,800 f/mg. ND
ND
3 5,600 ND ?
8 13,000 10 -
12 60,000 15 ND
15 8,900 ND ND
IO .1,800
7 ND
5 400 10
5 ND ? ND
ND 2,000 2 9,000 6 ND
ND -
ND t
8 ND
ND 9,000
trace " ND
IO ?
10 -
ND -
ND ?
ND ND 1 ?
b y C T F A m e t h o d o l o g y a n d a l s o ^ b e p e r f o r m e d .on. .3 r a n d o m b a s i s on Other samples. Company representatives were polled at this m e e t i n g and previously by Mr. George Lee to determine whether t h e y w o u l d b e w i l l i n g to p a r t i c i p a t e in such a s t udy by ass.:?-- i n g t h a t c u r r e n t p r o d u c t i o n s a m p l e s w o u l d b e p r o v i d e d and t h a t f i n a n c i a l s u p p o r t w o u l d b e given. T h e results would be m a d e k n o w n - t o the F D A arid.probably p u b l i s h e d in some form. The f o l l o w i n g companies i ndicated they would be willincr to p a r t i cipate.*
Avon Products, Inc.
Bristol-Myers Company
Colgate-Palmolive Company C o t y , Inc.
Faberge, Inc.
jphnson & Johnson
Menneh
Sterling
'
in addition, C h e s e b r o u g h - P o n d 1s , Mem, and Yardley would probably be interested.
The task force agreed to await the results of the meetings ,
with CTFA before deciding on whether a study cn current produc
tion should be initiated.
/
"
The m e e t i n g a d j o u r n e d in o r d e r f o r a .small g r oup to m e e t with F D A at 2; 00 p.m. t o d i s c u s s t h e r e s u l t s of C T F A a n a l y s e s of Dr. L e w i n 's samples,
forman F. Est r i n , P h .D , Vice President - Science NFE jj March 12th, 1976
pi*
jt
A v o n p r o d u c t s , in c .
$ U F f F R N * V F W Y O R K lui .0 l
March 12, 1976
Dr* Norman E s tr in
CTFA 1133 15th S t r e e t , Washington, D.C.
N.W, 20005
Dear Norm:
This i s to confirm our in d icatio n yesterday of our w illingness to disclose to you and/or the Food and Drug Adm inistration the re s u lts o f our analyses of, al 1 lo ts o f t a l c we have used in our products during the past three years
During 1973-a l l o f our-tale re c e ip ts were sampled, and aliq u o ts were sent to McCrone Associates fo r X-ray d iff r a c t io n analyses with the s p e c ific . request fo r confirm ation of the prsence or absence of c h ry s o tile . We did not sp ecify other amphiboles a t th at time because our e a r lie r data indicated that they-.were present only ra re ly in the ta lc s we examined. A to ta l o f 1/v. samples o f t a lc s used in our products were examined by McCrone during tnat
year. The X-ray d iffr a c tio n patterns are on f i l e . . a t McCrone and can be -
reviewed by authorized people.' .The results.'were negative.' / .
Since February, 1974, we have analyzed about. 250 samples o f t a lc re ce ip ts -:
in-house by D1A fo r c h ry s o tile and IR fo r tre m o lite . As mentioned above, ,
we f e l t th a t R fo r trem olite. was adequate fo r screening purposes, because
o f the rareness o f Other amphiboles. The data from these analyses can be
made a v a ila b le , a ls o , i f needed.. The re s u lts were negative.
-
Please l e t us know i f th e re .is anything e lse we can do to hejp re so lve the question o f asbestos: in cosmetic t a lc .
Yours t r u ly ,
.fULS ^ohn J . Travers
JOT :mc
..
cc: C. S, Rowland
G, A. S p ro tt
R. C. Reardon
Central F ile
Chesebrough Aotids Inc.
RESEARCH LABORATORIES
T R U M B U L L I N D U S T R I A L P A R K . T R U M B U L L . C O N N E C T I C U T 06(511
PHONE: 377-T1DQ
March 12, 1576
Drc Norman Estriri ,
. .'
Cosmetic,. Toiletry & Fragrance Association
1133 _ 1 5th Street., N.W.
Washington, D,C. 20005
Dear Norman:
For some-years, Chesebrough-Porid's Inc. has been concerncu
about reports that some talcs-might contain ssoestoc. a.
naturalise spurring contaminant. As "Ou Know, >'rc have, wiih CTEA,- and through -0T?A with .the FDA in developing suiracle
and practical methodology.: to resolve _the very coupie.. c-m
difficult task of identifying asbestiiorm fxoers in
--
have also worked, closely with resuonsxole. talc .upp o
identify high quality sources of talc.
By the beginning'of 1973, W^ -f-e-.-l-t t-h--at -*practica.l me,thouol.oiv the. purpose- was applicable, i-.Since then, we na\e aull.^eo techniques described in'the attachment tc_ mc.;u, or^
talcs of three types that wc liavd been'using. -nese u
from three different geographical areas. .
:metic .
I have reviewed the results- of. these analyses on the Iredmlng-lc-ti of these talcs used in recent production of ^saetn. ,;vnd . v a -.., products'in the United States. -The last 84 .reports, cuvtrin--, a ?h?ee-5ear period, are, .without.exception, negative for ohrysotlle-
and negative for fibrous amph-ibol.es..
If It can be useful, we wouid.be pleased to discuss these data with
scientists a t .the Food and Drug-Administration.
-
MB/bm end.
Sincerely, V,
l' V jL ^
n.y
lS~\
Murray Berdick .
.
Director:of Regulatory Affairs-
COLGATE-PALMOLIVE COMPANY 909 River Road
Piscataway, N.J. 08854
M a r c h 15, 1976
Norman F . Estrin, Ph.D.
Vice President .
.
The Cosmetic, Toiletry and
F r a g r a n c e Association,' Inc..
1 1 3 3 - 1 5 t h S t r e e t , N. W.
Washington, D.C. . 20005
Dear Dr. Estrin:
A t t a c h e d p l e a s e find a s u m m a r y of A n a l y t i c a l D a t a on 42 T a l c ..
S a m p l e s ( r e p r e s e n t i n g 20 r a w m a t e r i a l s apd 17 finished products)
covering the period 971 to present and examined by various tech
niques by the Colgate-Palmolive Research and Development Analytical
Department and McCrone Associates. - . '
Asbestos minerals were not detected in any of these s a m p l e s , with the'exception of insignificant trace amounts found by micro scopic m e t h o d s in three samples from 1971-1972, which is believed due to laboratory contamination. Other methodologies indicate the absence of any asbestos. The results of these analyses indicate to us that talc products produced by the Colgate-Palmolive Connany since 1972 are free of asbestos minerals when subjected to the. most sophisticated methodology available.
: We have ascertained by inspection of the package and analyses
o f t h e p r o d u c t t h a t the s a m p l e o f C o l g a t e - P a l m o l i v e 's C a s h m e r e
Bouquet examined by D r . Langer of M t . Sinai-Hospital was
m a n u f a c t u r e d p r i o r to 1970. T h e B a u e r and. B l a c k T a l c r e p o r t e d
b y D r . Langer, has not b e e n m a n u f a c t u r e d .since the end of World
War II. This company was acquired by Colgate-Palmolive approximately
three years ago.
. , .:
:
Very truly yours,
t* X' ! t
fa
C h r i stopher H. Costello, Ph.D. Administrator Regulatory. Affairs
C H C :m p Attachments
March Id, 1976
To: Dr. C. H. C o s t e l l o
From:
J. P. Simko, Jr.
Subject: Analytical Data on Talc Samples 1972-Present
S i n c e late 1972 w h e n - t h e p o s s i b i l i t y of a s b e s t o s in talc -was first raised, RfD Analytical has been engaged in re-analysing U.S. talc raw material and-finished products for asbestos minerals by the most sophisticated methodology,available at that time. A n a l y s e s w e r e m a d e on a spot *c h e c k b a s i s : T e c h n i q u e s u s e d m house are x-ray .diffraction followed by o p t i c a l a n d scanning e l e c t r o n m i c r o s c o p y , if n e c e s s a r y . X-ray is the b a s i c screc-iu.no tool a n d e x a m i n a t i o n by m i c r o s c o p y is m a d e w h e n p o s i t i v e v - s p o n s e s occur. A d d i t i o n a l tests on r a n d o m samples w e r e m a d e by trailsm i s s i o n e l e c t r o n m i c r o s c o p y and s e l e c t e d a rea e l e c t r o n di ti.raction by an outside consulting firm.
F o r t y - t w o sam p l e s (from dO r a w m a t e r i a l s a n d f r o m 1/ f i nished p r o d u c t s ] , c o v e r i n g the p e r i o d 1971 to the present., h ave b e e n examined b^ these various techniques.. Asbestos minerals wcre_not d e t e c t e d in any of these w i t h . t h e ' e x c e p t i o n o f . t r ace amounts -in 3 samnles- f rom 19''!-:. T h e s e lev e l s are c o n s i d e r e d yeneu,ll>_ - n l u the normal background levels encountered wnen this microscopic m e t h o d o l o g y is' employed, It is b e l i e v e d that t h ese trace a m o u n t s are d u e to' l a b o r a t o r y c o n t a m i n a t i o n . A 'detailed tabula t i o n is
attached.
JPS/ed tt
Ko. of Samples Examined for Asbestos Minerals 1972-76
Method, TEM-SAED ;.
Sample dates (yrs.)
Raw Talc *5 `
.
1971-72
Cashmere Bououet
**7
1972-76
X-ray plus microscopy (optical - SEMj-
Sample dates (yrs.)
12
1971-76
11
1972-76
DTA Sample dates (yrs.J
6
1972
1
1972
sample 19 71 raw talc contained 10-100 ppm. chrysotile *1 sample 19 73 raw talc contained 1-10 rpm, chrysotile
T h e s e level.,, A p re se n t po^sib
background von
tan.nation
**1 sample 197? Cashmere Bouquet taic contained < 5 ppm. chrysctiih
No araphlbole detected in. any of these.
JPS/ed 3-12-76
*
1133
STREET, N.W., WASHINGTON, D C. 2005 202/331-1770 TELEX 69-2673
M EM R A N DM
James H. MeritU
PrrsHer1
Monrian F. Estrin, Ph.O
VrCP Ycsrtferti--S^/fertce
TO: FROM: DATE:
N o r m a n F, E strin, Ph. A n i t a S. C u r r y March 12th, 1976
J i m J e n k i n s c a l l e d r e g a r d i n g t h e .l e t t e r y o u h a v e a s k e d for o n c u r
r e n t t a l c a n a lyses, - H e w i s h e s to i n f o r m y o u . a s t o 'w h a t t h e y h a v e
been doing:
1. Mr. C l e m e n t s c o n t a c t e d p r . Langer w h o gave n i m ' t h e c o d e on t h C o t y A i r spun t h a t w a s tested.. . It turns out'that this was a July, 1?69 produc tion item. .
2 In 1970 Coty changed to a completely different * taic; s i n c e t h a t t i m e t h e s u p p l i e r (WC&D) ha.s s u p p l i e d l e t t e r s to t h e e f f e c t 't h a t t h e y d c continuous monitoring- of production/ even . t h o u g h i n d i v i d u a l .b a t c h e s sold to. C o t y m a y n o t be individually tested.
3, C o t y has h a d tests- r u n o n i n t e r m i t t e n t batches^ T at the Pfizer Laboratory in Easton,- Pennsylt a m a . These were done by X-ray diffraction and TEM. The results were all negative. Also, in the last week they have tested 1974 and 1975 lots. These too were negative.
S C :j j
CTFA v sm
WL VSH TLXAl4fc
VAF139 C1427)C.l-0)B216AS72)PD 03/12/76 1424
twx cn-nao L3A
Lgjg L-A
RiS THE COSMETIC. TOILETRY AND FRAGARNCE ASSOCIATION. IN.
1123''f i f t e e n t h s THEFT, n. V.
WASHINGTON. D. C. 0005
MARCH IS.' 1976
DR. MCRMa N ESTJUN
'
VICE PRESIDENT - SCIENCE
DE/R DR. ESTF-INs
AS A RESULT. OF DISCUSS IDOS I HAVE HAD WITH LOUIS MJRIMC COKCE^MIMG THE MARCH It. 1973 CTFA TALC SUB-COMM ITT it. .
-I WOULD LIKE TO STATU' TH-H-T VS HAV^. A CONTINUING PROGRAM 1 EXIST CUTS TO TEST OUR MONTANA GRADES OF TALCS THAT ARE LEINS OFFERED'TO THE.COSMETIC INDUSTRY-
PRIOR COF.RESPOT'DE'-ICE BETWEEN 0UR3LLVE5 AMD 'H*_ _GEORGE V. 'SAMDLriUiL CHAIRMAN OF THE TALC SUS-CCHUITT-- . KAC ESTABLISHED THAT v s LAVI- TESTED 2. B39 Si^iPL^S F*ROM OUT; OCRS DRILLING PROGRAM AtID ST M-HAY DIFFRACT!JD PATTERNS HAVE HO SEEN AMT DETECTABLE .LEVEL.. OF. CH3YSvT.IL,F AMD TFF^CLITE- CUR X-RAY DIFFRACTION TZCHHX.aULS. i.E::L IM a c c c f d a h c s uir; t h e c t f a j -a - i m e t h o d o c t l u u d FCR USE UFFEH CTFi. SPECIFIC:.TJ ON5 FOR COSMETIC TnLC
SINCE OUR OR I INAL IWESTlGATICN AMD SUEUIS5I0N (i.UGj'ST A. 1975) . 'IF HAV EVALUATEDh H ADDITIONAL FIFTY ' CNm TAN ,
PRODUCT!ON SAMPLES WITH-THE SAME 'OCCELLENT RESULTS. 'ME CONTINUE TO USE M-Ra Y DIFFRACTION TECHNIQUES AS OUTLINED 3i CTFA J-4-l. '
'JS SHALL BE HAPPTY -TO CONTINUE TO COOPERATE WITH CTFA IN
OUR testing program.
VERY TRULY YOURS.
CYPRUS INDUSTRIAL MINERALS COMPANY
555 SOUTH FLOWED STREET
. '
LOS ANGELES... CALIFORNIA 900 7 1
TELEPHONE' C213) 459-3700
END '
iNN ''
H. T. MULRYAN PRESIDENT
323PEST '
.CTFA WSH
Ort"
it i
L --:-i! ;.-r .-.r.fi
talc investigations
Our investigations of talc dates back to.November 1972, whan the following samples were analyzed by McCrone Associates and round to be tree of any
asbestos content:
.
Music Talc Aphrodisia Women's Talc Aphrodisia Men's Talc Flambeau Talc Woodhue Man's Talc Straw Hat Talc Tigress Talc Brut Talc Kiku Talc Woodhue Women's Talc Xanadu. T3l.c Zizanie Talc ,
9-26-72 d-r-26-72 9-26-72 9-26-72 9-26-72 9-26-72 9-26-72 9*26-7-2 9-26-72 9-26-72 9-26-72 9-26-72
In.November ,1.975, the following samples were and found to be free of any .asbestos content:
ural
hr' cAo-'h-1 bauaciates
Brut Talc Brut Talc. Kiku Talc Kiku Taic Kiku Talc Xanadu Talc
3.4.75
20.6.75
11.11.75 24.4.75
3.7.75 20.6.75
__
On of
March 9, 1976, McCrone Assoc, purchased Brut Talc, Lot #2585, which was produced
in on
a Chicago September
store, one L5, 19/
4 oz. container This sample
was also found to be free of any asbestos content.
FBtRG DIVISION -r- r a-;.s
.-a
BABY PRODUCTS COMPANY
^ofiHVon^ijcfttncii N E W BRUNSWICK. N J 0SS03.
M a r c h 15, 1976
Dr. N o r m a n F. E s t r i n Vice President - Science C o s m e t i c , Toiletries',;and
Fragrance Association 1133. 15th Street, N.W. Washington, D.C. 20005
-
Re: Examination for Asbestos In Talc
Dear Dr. Estrin:
T h e t a l c w h i c h is u s e d b y J o h n s o n & J o h n s o n _is solely d o r i y e d from
its own mine in Vermont, where the ore ys/mined selectively and then-beneficiated by the.process of flotation.
S h i p m e n t s of t h i s hig h l y p u r i f i e d talc a r e . ^ o h t i n e l y e x ^ i n o r t by
o u r o w n l a b o r a t o r y to v e r i f y the a b s e n c e of asb e s t o s mineral. ..
H i s t o r i c a l l y , J o h n s o n &, J o h n s o n has a l w a y s b e e n c o n c e r n e d a b o u t the
M t a S i c a i integrity
i t s t , l c s a,,d e y , a i t s ^ a r l ^ s s p e c i f
f i r a t i o n s h a v e r e q u i r e d the .examination for a c i c u l a r part n...u. i . . m e n w a s r o n e o u s l y reported in 1971 that our powder contained a s b L t L L sponsored a scientific seminar of mineralcgical and a n a l l t w i l e a ? M ? s for the FDA to prove that our laid la not eon+ fl+ edi w i t h a s b e s t o s . At t h a t t i m e n u m e r o u s sam p l e s we., e a n a l y z e d by e x p e r i e n c e d C o n s u l t a n t s s u c h ias- M c C r o n e A s s o c i a t e s ,
C o l l l l t o s c h o o l o f Mines, P r o l e s s o r F. f 1 . ^ y < o : ^
iion 1^ l ? i e Cr a (olfM ):i
hi! irao-
analysis! d W f e r e n t i a l thermal analysis, and transmissron electron
microscopy.
,
.
.
During.-the p e r i o d D e c e m b e r .1972 to O c t o b e r 1 9 7 3 93 J `B
p ^ 0c*
S d: S L r S ^ r a ? l : eXr S h S o ^ r L dsiipentine minerals .ere
detected in any sample.
Dr- N. F, E s t f i n C.T.F..
-2- M a P c h 15, 1976
Beginning in October 1973, differential.thermal analysis was added to our specified requirement. Both, differential thermal analysis a n d X - r a y d i f f r a C t o m e t r y w e r e i n s t i t u t e d for the r o u t i n e e x a m i n e tid'd o f s e q u e n t i a l lots... A f u r t h e r 100 lots h a v e since b e e n examine d , a p p l y i n g b o t h m e t h o d s to. e a c h sample. Again, no a m p h i b o l e r-r s e r pentine minerals have been.detected,
I w o u l d l i k e t o a d v i s e that w e are. c o n t i n u i n g to e m p l o y dit "eren.tial t h e r m a l a n a l y s i s arid X - r a y diffraetoiiietry in the e x a m i n a t i o n of sequential lots for the detection of amphibole and serpentine min
erals.
'
It should be pointed out that we also maintain a worldwide-monitoring of- t a l c s u s e d b y o u r J o h n s o n & J o h n s o n a ffiliates, e m p l o y i n g th o s e
same techniques.
Finally', let .riie a d d that p e r i o d i c a l l y , we. a l s o submit s u b - s a m p l e s for Transmission Electron Microscope examination and these have always v e r i f i e d the absence oi asbestiform m i n e r a l s .
It is our understanding that you would wish to submit this information to the FDA, P l e a s e r e g a r d t h i s l e t t e r as. lion-confidential.,
Sincerely yours, /
George Lee
^
D i r e c t o r of A p p l i e d H e s e c r c h
GL/mm
V.,
BABY PRODUCTS COMPANY
(jfcrflilVCIKtijoh11cu
N E W BRUNSWICK- N -1 OB9u3 March 14, 1976
A total of 3S samples Department ol
M t , Sinai HosptU t'_ s ^ au effort U , oubetanttn.e r*~ -
" p u t r i i t," staff of the 'It. S i uai H o s p i t a l -
AmericonJ^Gffi^^i^ ' .-
, ,,Ain-r
fn
19
American
. ptc-nn
C.il6-
A total of 20 W 10 wre sunjeotwi to
^ " S S ' b y X-'rav rSrodu0TS
and electron icr-cohtalaeo severa'
K. 1.1;Kproo
u
t
,
K -
This, is
. tn thP-'Mt. S i n a i report tiiat 't' and that another five o
contained 8 to * - 1 .^bestowcontainocl less than u.o ashcstos.
of the pV' >d`.icts ;r dllCIS
British Talcin^T^cKlU-cll;-
Poole;
1,^ f'i t'4< d. one
S i m i l a r l y , IS p r o d u c t s w e r e ^ i n i n e d b ^ h ,; c t h o r hand -.....
produc-t. as c o n t a i n i n g n lltnop y - tromo M ts in three p r o d u c t s ^ and___
microscope Han r o u t e d t
It s h o u l d he e m p h n a i t e d that t h ese
in 1 971 and arc not nc,.essai i1) l
talcum p r o d uction.
. . ... rc ,.m p icJ
current American
waiter c. me crone associates, Inc,
CONSULTING: ULTRAMICROANALYSIS MICHOSCOPY SMALL PASTiOLe Pr.OB'-K-VS O U D .JY A 't C
12 M a r c h 1976
U p , N o r m a n Estriii
_
Cosmetics Toiletries and Fragrances Association
1133 15th Street, N.VV. Washington, D.C. 20005
Dear T>r. Estrtn:
This letter will amplify our recent conversation on-talc analyses for asbestos.
Since'1971, Walter C. McCrone Associates, The., has worked With several producers and users of talc, the majority of them involved with cosmetic grades of talc. During this period w o have analyzed several nundmt talc _ samples for the presence of asbes.tifo r m minerals. 1 he mctnodologies Uscu have been principally X-ray diffraction and light microscopy using dispersion staining, although extensive transmission electron .microscopy examinations have been carried out for some companies. Subject to the approval ox our clients, w o ate prepared to m ake available to the F D A .through CfFA.tm. results of these analyses. W e also have available retained samples lor m o m
of the analyses.
Verbal agreement to release this data has been already given by clients accounting for probably 80-90ch of the samples; the others have not yet been approached. It would,, however, be improper for us to comment on specific samples until such time as written approval is received from our clmn-s, together with identification of those materials used in cosmetic production. T he latter point is stressed because several of our ana lyses represent the results of raw material assessments which some companies initiated a m might include talc ore bodies which are unacceptable.for cosmetic applica
tions.
;
I do not think, however, that I would be violating any company confidences if I were to com m e n t on the asbestos in talc situation as wo saw it over the last 5 years. 1 think our view can be summarized quite briefly as follows.
2320 SOUTH hVCtl'dAN AVENUE <CHICAGO, ILL'NGI EOT,16 -SiT/bV'mc. C.'iSLE C iA V iC riONE
12 M a rch 1976
Bh * N o r m a n Estrin Cosmetics Toiletries and Fragrances Association Page Two
S o m e cosmetic talcs prior to about mid-1972 to early 1973 were found to contain amphiboles -- principally-of th Tromolite-Anthcphyllite type at levels, determined by X-ray diffraction, of the order of 5-15% by"weight.
Microscopical examination of these talcs, however, indicated that the bulle of this amphibole content (>99%) was non-fibrous, even applying the 3:1 aspect ratio criterion for a fiber, and hence not asbestos.
N o ehrysotile asbestos was found in thse talcs.
Since 1973 none of the talcs which w e have examined and winch have been
identified to us as production materials have shown any detectable level:;
of either ehrysotile or asbestjform amphibole.
"
Yours sincerely,
P-
In M. Stewart Manager, Electron Optics Group
Companies contacted and granting verbal approval to release, inrbrmctiar
include :
~
Avon Products, Inc. Bristol-Myers .Products Chesebrough-Ponds, IncColgate-Palmolive, Inc. Fabrge, Inc. Johnson & Johnson Windsor Mrnerals, Inc. Whittaker, Clark' & Daniels,
Inc.
.
lmh
0 - D ' I i ' U G 1 VI* riJ
S O - P R K A V E N U E . MTW \ O R K . M / 10016
EXECUTIVE 0FTICE5
M a r c h 12, 1976
Corporate Director of Quality
* - - j'. ; it
* *N .
Dr< Norman Estrin. f>resident " Science
1133 ? i f t e e h t h T StrJetyN \ FragranCe A s s o c i a tion, ln c . W a s h i n g t o n , D . c . 2000s'
Dear Norman:
Of the taiinL e d U?71IZBT1B ^ i ap ^ dg J n tir]a N o v e m b e r 1 3 7 1
a s b e s t i f o r m m i n e r a l s . S i n S ^ h S tfme " ? " ** of
b y x^ray diffraction a n a l ? " s a b ju t S S e t, T 5 * * tasted
received* In all instances--thwas no detectable as'bestifnrm^i
^ Qf the lozs '1 R d l G ated t h ere
s a m p l e s . W e a lso h a v e hsrl a
n e r a l s p r e s e n t in these'
Whittaker,. Clark & Daniels monitor the shipments of t4lc
Ur suPPl i e r r ^ l 0 * ti3ielir
a m o a n t J ? tifrm rainerals and have found no d e L c t L l ^ ^ TM ^
to teatinatare
Powder" tested b^thlTMount
Qj ',zflf Baby
and W a s produced in June 1970. tie are^df t?rou p ." as c o d e d
!971 does not contain asbesliform L e r a S " Sincerely,
S1"Ce l9ts
RAM:mm
R o d e r i c k A. Mundy
The Cosmetic, toiletry and Fragrance Association, Inc.
1133 15th STREET, N,W , WASHINGTON. O.C. 20005 202/33M 770 TELEX 89-2673
.
H Mar.,in ii
Norm;-T F. Ecfin. Pn.D,
MINUTES. TALC. M E E T I N G AT FDA
A meeting was held oh March 11th/ 1976 in the Commissioner"a C o n
f e r e n c e .R o om, P o o d and D r u g A d m i n i s t r a t i o n , 200 O Street, g.w. /
'Washington, D.C., to. d i s c u s s r e s u l t s of the, C T F A a n a l y s e s of c o d e d
s a m p l e s s e l e c t e d b y F D A a n d t h o s e u s e d by. Dr. Lew,in f o r his a n
alyses. T hose in atte n d a n c e were;
'
G e o r g e Saiidland,- B r i s t o l - M y e r s C o m p a n y (Chairman)
Henry M..Davis, FDA
'
'
George Lee, Johnson & Johnson Baby Products Company
Robert Rolle, Johnson & Johnson Baby Products Company
John P. Schelz, J o h n s o n & J o h n s o n B a h y P r o d u c t s C o m p a n y
R o n a l d L. Yates, FDA.
'
N o r m a n F. Estrin, C T F A
Dr. Estrin opened the meeting by introducing the Chairman of th~
C T F A T a l c T a s k Force,- Mr. George. S a n d land,-' a n d b y n o t i n n to V i m ~
D a v i s t h a t C T F A is p l a n n i n g a m e e t i n g o n Monday, March. 1.3ch to d i s
cuss other data collected on talc. "
'
" *`
Mr.. Sandland, n o t e d t h e N o v e m b e r l e t t e r from. M r . D a v r . s and the fact
that the anal y s e s b y Dr. Rolle have now been completed. Dr. Roily's
letter of December 29th, 1175 and the results of"the analyses ware submitted to Mr. Davis and to ethers present. Mr. Davis than c r i
tically c o m p a r e d the resu l t s with those of FDA and Dr. Lewi.n. S u b
s t a n t i a l a g r e e m e n t w a s f o u n d w i t h F D A a n a lyses. r.f w a s noted tha
m e t h o d u s e d w a s d e v e l o p e d for r a w m a t e r i a l s and n o t fihishf-E p r o d u c t s . -A copy' of the. C T F A m e t h o d w a s d i s t r i b u t e d to those p ras nt Dr. E s t r i n e m p h a s i z e d the work done o h these old p r o d u c t i o n nr plu is v a l u a b l e f r o m the m e t h o d o l o g i c a l p o i n t of.view, but is not v a l u
able if.one's goal is to ascertain the present quality of cosmetic talcs.
D u r i n g the meeting,. Mr,. D a v i s n o t e d an, a r t i c l e b v G o r d o n E v e r e t t ent i t l e d , -" A n a l y s e s for A s b e s t o s in E n v i r o n m e n t a Samples" ( F n v i r m m e n t a l H e a l t h P e r s p e c t i v e s , V o l u m e 9, 1974, pp. 1 8 1 - 1 8 2 ) . "
There
further- business, the meeting ndiournod --------------- .
N o r m a n F. 'Estrin, Ph.D. Vice President - Science
N F E :jj M a r c h 12th, 19 7 6 Attachment
BABY PRODUCTS COMPANY;
For CTPA Tale Meeting M a r c h 11/ 1976
March 8/ 1976
mhMKTTC TALC STATUS'
T h safety of.coneUmer talcum products has-been under continued attack, primarily led by the Mt. -Sinai group,-. b e c a u s e of three alleged concerns. Those allegations, a. ~ a*
follows :
- ' . ....
`
.
1. C ommercial talcs often contain asbestos as naturally
Occurring contaminants.
... .
..
2. T a l c c o n t a i n s other- impurities.; m i n e r a l s and m e t a l s Which may have potential biological s i g n m e a n c s .
3. Ta l c as a m i n e r a l itself m a y be hazardous.
X. F A C T S Qrt T A L C '
. '.
A. Asbestos and Cosmetic Talcs
- c h r y s o t i l e a s b e s t o s has n e v e r been, d e t e c t e d i n cosmetic talcs or finished' talcum p roducts.
- amphibole asbestos, e.g. tremolite and anthophvllite, h a s b e e n f o u n d i n a .'few tJ. S. c o n s u m e r t a l c u m p r o - ducts (by Mt. Sinai and confirmed b y a very reliable
expert consultant).
.V b
- disagreement existed between Sinai scientist and an expert consultant, in recent analyses for'asbestos
: in B r i t i s h O T C t a l c u m p r o d u c t s . T h i s r e s u l t e d -in
withdrawal of h i g h l y c o n t r o v e r s i a l a l l e g a t i o n s oi ,.
a s b e s t o s in B r i t i s h t a l c u m p r o d u c t s m t e n d e - for. ;
p r e s e n t a t i o n at the 4th International S y m p o s i u m on
inhaled Particles & Vapours.
- Mt. S i n a i d i s c l o s e d s t a t e m e n t s in F e b r u a r y '7 6 d u r i n g private interview.with the Canadian. Broadcasting
Corporation, t h a t t h e i r a n a l y s t s of U. S . p r o d u c t s
:.
has found asbestos.
,
March .8, 1976.
B* Biological testing of Cosmetic Talcs
- e x t e n s i v e animal tasting data' is only available for Windsor 66 talc and Italian 00000 talc.
'
_ nattelle h a m s t e r i n h a l a t i o n t e s t i n g oh W i n d s o r G
talc with- c h r o n i c exposures u p to 185 times, m e d i a n baby dosage has demonsorated no exposure-related .
pathology-.
... : . '
: ' , : - ..: -
M R C (British M e d i c a l R e s e a r c h Council), t e s t i n g w i t h
" S a l i a r o o O O talc -indicated no tumours resulted zrom
intrapleural inoculation or ingestion.
.- . .
M R C t e s t i n g W i t h Italian t a l c ' s h o w e d fibrosis at h i g h v a r y i S a g ' w W r t ( W t o 1000 tim e s m ed ien b a b y
dosage) . . - - -
''
'
C- Human Medical Studies
'
.
Pnhino Mortality Study indicated no excess -deaths d u e ' ? f c " n c e ? a m e n g e t t a l e mi n i s a n d m i l i a r s e n a o s e d to-
I t a l i a n c o s m e t i c talc. ..../
'- .
- Green p r o s p e c t i v e P u l m o n a r y S t u d y w i t h W i r ^ o r -talc . miners .and m i l l e r s have, shown, n o - r e spiratory d _ s e , s e -
- K l e i n f e l d h a s 'published t h a t d e a t h s w e r e d u e t o c u n c e r o f :lung and p l e u r a a m o n g s t t a l c w o r k e r s r e c a n ing hi,). to industrial talcs mixed with appreciable amounts of tremolite, anthophyllite and small amount
of silica.
D1 Conclusions
%.
o f b e t t e r t h a n 9.0%, a n d no a s b e s t o s .c o n t e n t . . .. -.
l w r i S e n to preclude s o n * which aro marginal as to potential contaminants.
-3March 3, 197
FDA/OTC PANEL REVIEWS OF TALC
F D A - L E W I N PRODUCT ANALYSES ... .
.
- p r o f e s s o r L e w i n `s m i s - i d e n t i f i c a t i o n of c h r y s o t i l e in store shelf talcum products highlighted to FDA the need to develop analytical methodology for talc. ;
;
O T C C O N T R A C E P T I V E S fi V A G I N A L P R O D U C T S P A N E L ;
- After a brief look at the safety of talc, the September 1S19 , 1975 meeting decided to defer definitive action on
talc to the OTC Antiperspirant Panel.
OTC SEDATIVE PRODUCTS PANEL
'
- This panel originally proposed that talc, a non-essential inqredient be banned from OTC products that are meant to b e ingested. B e c a u s e o f a J & J ,response, t h i s P a n e l
. a l t e r e d its p o s i t i o n t o u r g e t h a t t a l c c o n t a i n i n g a s b e g t o s^ not be permitted to ba formulated in OTC products meant .
to be ingested. : . ' '
,
;-
OTC a n t i p e p s p i r a n t PRODUCTS PANEL .
.
-.Talc, w a s c l e a r e d for u s e in' ant i p e r s p i r a n t s o n l y o n the basis of the low exposure in use. This panel has stated that it has not cleared talc for other uses.
OTC MISCELLANEOUS EXTERNAL DROP PRODUCTS PANEL
- B e c a u s e a l l t h r e e of t h e above.. Panels h a v e n o t i s s u e d
an u n e q u i v o c a l conclusion in the safety of talc, thio.
f o u r t h P a n e l w i l l b e r e q u i r e d to p r o v i d e a n u l t i m a t e . .. :a n d d e f i n i t i v e s a f e t y r e v i e w o n talc. , Wjt tb. t h e p r e v x o u s
history of attacks in:the public media and the erosion of consumer conf idence, all means should t e taken to . . . .
obtain a Category I for cosmetic grade talc. Tre^publj.cxty
of category XII would do irreparable, h a r m to talc s
. a l r e a d y t a r n i s h e d image. - - .. .
;
P R ESENT P R O B L E M F O R CTF A H IIDU5TRY
..
- Present allegations f r o m .Sinai, that they have .anaLysed
n-2 found asbestos- in a substantial number o r 1. ^
talcum, produces is particularly damaging to CTcA s 'anal :
presentation testimony .that'-means-are present/ bexng . .
. t a k e n b y i n d u s t r y to .self-- regulate. ,.
-4March 3, 1976
U n l e s s this S i n a i d a t a is refuted, it w i l l adversely influence th M i s c e l l a n e o u s External Panel s fo-.tncpm.ing safety review for talc arid.undermine the tenet that sa-e cosmetic grade tiles are now being responsibly utilized
y t h e i n d ustry-
III.
r e c o m m e n d a t i o n s '.I1 R c t f a a c t i o n - .
-- CTFA should immediately provide refuting data by o r g a n i z i n g a. t e s t b f c u r r e n t t a l c u m p r o d u c t s and conduct examination-for asbestos by the best method t h r o u g h i n d e p e n d e n t experts-. T h e s e same p r o d u c t samp l e s should be offered to the FDA and the Mt. Sinai Laboratory, for v e r i f i c a t i o n f analyses-. .
to support an effective and persuasive presentation, to the OTC Miscellaneous External Panel, CTFA should-issue a s t r i c t r e v i s e d t a l c -s t a n d a r d -which .would v e r y c l e a r l y distinguish cosmetic from industrial grades of talc. . Such a specification will be credible to the consumerist advocates o n l y if it fulfills the following.requirements:
1 It must, s p e c i f y the absence o f a sbestos c o n s t i t u e n t s
' by the most sensitive method. :
2. It m u s t a d h e r e t o a talc p u r i t y l e v e l w h i c h _is ' closely-similar to that.already used xn toxi cological studies; namely, at least 90% talc. .
- C T F A s h o u l d identify c o n f o r m i n g s o u r c e s o f t alc as C T F A
Cosmetic Grade Talcs and encourage manufacturers using this grade-to label their finished products witn tins
designation.
*
C*BLE~SL!rlNAot
' ^0,, 5f-ioo
I ri,,,
1 T33 F ifi-tTdi:jUarters
W a s h ir,9tonen^
N. w .
. , U *C - 20005
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9
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^ould be thr S ' 7t deterrf V de ta,Cs that to Pa,"'y r insure
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is '
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oubjeoteci
have also Useo '' '
- b o r a t c i e s . . ., ,,P r j d U c t s w a3-sS
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^pn'of;.
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chtinuec/ .'
. :
-
CDeoluBmelbl.iaSi SRciciehnatridfisconI,n dEunsftireileds,, CAounsntienc,ticTuetxa's'
W e a re w illin g to sub m it th is inform ation to the com m ittee in d e tail to
help substantiate th e ir c la im s.
'
V ery tr u ly y o u r s, ' ",' / ; .
WH ITTAKER, CLAR^K & DANIE L S, INC.
. J > ... Frederick F. Roesch ' Executive V ice President
^
F F R /d m
The Cosmetic,Toiletry and Fragrance Association, Inc.
,1133 15th STREET, U .W ., WASHINGTON, D.C. 20005 202/331-177D TELEX' 89-2073 '-
-'
''
,
* ,
'
MEM'O RAN'D UM
. Janins H. Merritt * Pnsstd&fii
Norman E. Eatrin, F'h.D, Wc Pirsklon!-- Soirncc
E. Edward Kavanangli Vina /'ipsMeuf->
Cofty/'osiiofutf Ri'ilions
Margaret W. Smith Lxccutivc Secfiflaiy
TO: The CTFA Talc Subcommittee
FROM:
F o r m a n F. E s t r i n , Ph.D,
DATE:
November 2nd, 1976
SUBJECT; CTFA Talc Methodology
McCrone has performed a very useful service by comparing and' e v a l u a t i n g C T F A m e t h o d o l o g y .
Their suggestions with regard to methodology and their other suggestions should be discussed at the November 10th Talc Subcommittee meeting.
NFE:jj Attachment cc: W a l t e r C. M c C r o n e
IVv^-j waiter c. m e crone associates, ine.
i\ CONSyLTi? ,:, UuTnAMiCrtaANAlTCIS * MICROSCOPY SH UL RAnT.CLL PROaLtl.lS - SOlOD-STATE ChfMlfiTRY
'3 September X9"jS
Dr. dorsali F. Estrin
1133 15th St., Washington, DC 2005
Dear Dr. Estrint
As you know, ve, at McCrone Asroclateg, have done CLCsiderablo work on talc and especially or. various Binerai imturitios in talc, As a result vs have accumulated data, procedures (and prL^udicfcs) concerning these analyses. .
I have recently had occasion to look at the proporsi OTTA procedures for astescifans minerals; in talc and can't .Ip feeling that our routine procedures aro, 1 regret to say, considerably rare sophisticated. Since 1 vos about to commit our -.ethods to a paper cor another publication '(unfortunately* for the FDA) 1 felt that, as an intellectual esercire, 1 would recast Che e .no tr-ateriul as a CTFA method. I as enclosing this horrendous document for your perusal and sympathise if ycu choose to quickly burn it at the stake. Note first, however, that 1 have retained sene of the features of your method `that I liked.
Still, in cur hands, the methods ve prepose work very well, lo addition, they are rapid and reasonably inexpensive* Ve are interested in inproving the competence of nitroanalyats generally a*.d, as you. may lcr.ow, teach about .;0 courses a year in these procedures both hare and abroad. As n ratter of fact,'I leave this veihend where 1 will be teaching 3 back-to-baek courses in the idebcificstioft of asbestifora minerals by the nethoda covered in the infamous enclosure.
Seriously, I don't propse you adopt these cathode in the detail I've ^Uggjsstcd but X do suggest that you urgrt each CIFa member to take steps nov t:.aEf 'vili Iced to chair ability to mtke such analyses. The more each company knows about the products it makes anu the raw materials it uses the better a M vili that company be co ^tey out of trouble end represent Its best iatfcrastn if trouble arises, 'ie can help here chrough .our teaching arm, I seggane we offer a course either directly through the CTFA.or simply to t h e member ccmpnnics. This course would train one or more Qualified ticroanalysts in each company in the use of che proposed x-ray diffraction and dispersion staining methods for the study of cosmetic talc and possible contaminating substances.
Ve would further aid each company in setting up (purchasing, if necessary) the equipment, supplies and mineral standards required for aiich studios. The imeire package voulJ include a or-s-week intensive course in dhicago, evaluation of* the company laboratory and equipment, furnishing sets of
$70SOUTH liiCHIGA N AVcJiUE . CHICAGO. ILLINOIS t^fiA . S U fiJ2-71u5 C ABLE; CHEMICrOWc
Or, l!orran IT Estrin Pwt two .
standard saf^/les and test rnterial and .a follow-up aver a severni-aonth piiti'oc of progress in each company by r.^cx.-s of a series of round-robin sanple analyses. We will sign off each ccnp^ay when vc. are satisfied thair personnel and ofluipnent can do a professional job of analysing talc spies. The cost of this package would be $1500 per company,
I look. fcTvard to your response and hope 1 haven't scared yoc away*
Yours Sincerely,
tfoi:cdh Enclosure
Walter C. XcCrone
COSMETIC TALC
eefIMirra;;:
Coar.etlc Tnlc is a white, esaenti-il'Jy odorless, fine powder, "round iron naturally occurring rock ore consisting nainly of hydrated ragnesiuTa silicate having the ideal fori-.ul
tig-CSi^,.] (OH ).uith lesser aaoutit* of naturally us^ociutcd rdnera.r'such at calcite, chlorite, dolonite, kaolin- and ^agnesite, and containing no asbestos minerals detectable by x-ray diffraction
,
TEST
SPECIHCATIOK
. METHOD
Color.... .. Odor..;....
buy*r and shoving ho change after heating
buyer
at 20C*C for 5 sinuses
Identification.......... ..
- -,
' `
Tositive: 1, 'Close Batch to CTFA
Spectrin with no in
di c a t i o n of. foreign enteritis
CTFA C 3-1
Ok
2. (Alternate) Close natch ASTM D 934-76 Powder Diffraction Pile Ko. 19-770 published by ASTM, showing the coat insemie reflections at d valves about 9-35, 1-53 end 6,59 A
S l i p.... ...... L u s tre........
tiater-Soluble Iron...... Screen est...
-
Tusses rest
UST XIX, page 487
511 ir.ininuc through 200 mesh Finer grades: ns .specified by
fthe buyer `
Voter Soluble Substances...
*
0. 1 majtiu.un
UST XIX, page 487
See tost for "Reaction and Soluble Substances'*
Acid Soluble Substances.,,
Loss oi I g n i t i o n . * ,.., Arsenic'(as As).......,,..
Ae specified by the buyer6,OX naxirun .5.01 oaxljitua
3 ppm raxicum
Lead .(as PL) .. ............ ,..
20 ppm maxitma
/unphibole.-,. . . . . . . . . . . . . . ,,
Nona steered by XD
(Asocstiiorn Trcanllte ec al)
Free Crystalline Silica..,.. (Quarts)
As specifltd by the buyer
CTFA E 33-1
E S P J.U, paZ t ',S7 CTFA F 1-1, Farts 1-A and 11
CTFA F 3-1, Fart* 1-A and 11
CTFA J i-1
C TFA J 5-1 (ETA) Altercatei CTFA J 6*1 (X-ray)
A C I D SOLUBLE S U B STANCES Ili TALC
Principle A supple of talc is ir.ixud vith diluted hydrochloric acid *ad the
insoluble portion, is removed by 'centrifugation and filtration. The filtrate Ijs sulfntcd, evaporated to dryness and ignited* The acid soluble natter ia decofciintd gravimutrically as the sulfate*
Apparatus
1* Controlled temperature water bach
102/ Beaker, Griffin, Q m l
3* Volumetric fla&k, 50 nl4. Centrifuge / 5. Centrifuge tubes {2), 50 ml' 6 . Graduated Cylinder, 5Q ml 7. Sintered glai.s funnel, ultra- fine porosity, 60 nl (0.9 to 1.4 tm)
Corning flfrOSQ-UF or equivalent 3. Vac u u m flask, 125 ml
S* Pipette, 10 ml '
10- Platinum or Vycor evaporating dish or equivalent
Reagent's
1- Hydrochloric Acid, diluted, 101 v/v
2 . Sulfuric Acid, diluted, 101 v/v
Procedure
2Weigh
e (0.001 g) of sample into' a 100 ml beaker, add iO tel
rdiluted hydrochloric acid, and place in water bath at *55* (2r5*C), with
occasional stirring for 30 rlnutes. , Inmcaiately remove beaker from bath-and,
pour contents into a 50 ml centrifuge tube* riniiins beaker and stitTing bar
with 2 to 3 tal of distilled cater. Centrifuge at 5000 EPK for 30 citmtcs
(Kate 1).
Filter supernatant through ultrafine porosity sintxred glass funnel
into vacuum flask, using 2 to 3 ml of distilled water to rinse the centrifuge
tube and funnel, and using care to avoid dislodging the packed talc at the
bottom of the tube- Filtrate mast be clear (Note 1), Pour filtrate into 50
ml volumetric flask, rinsing with 3 to 5 isl distilled watervolume vith distilled water.
Adjust to
Pipette 25 ml of adjusted filtrate into rated, ignited evaporating
dish* Add 2 d of diluted sulfuric acid and evaporate to dryness.
Ignite at 600* C25*C) for 1 hour. Cool and veigh.
Calculation
Z A c i d S o l u b l e S ub s t a n c e s h e i g h t o Fetiiiu* in g x 200 . Weight of Sample in s
Kote 1. Examine the centrifuged socplc carefully to assure good clarity be
fore proceedins vith filtration. If haziness is detected, centrifuge the sample for an additional 15 to 30 minutes is necessary.
ASEZSTIFORM MIKEKALS IK COSMETIC TALC The presence of asbestifora minerals in talc is dererciaad by x*"ray diffraction with a -sensitivity of about 0.52 by weight- The mineral identi fication | la confirmed and the dsbcsrlforn habit is determined by polarized light nicroscopy vith the added help furnished by dispersion staining.
If >0.52 of. -asbfcscifom mineral is present the sample is rejected. If the non-asibcatifora habits are present. e,p.. Ilzardite, antigorlte. gruneritCp cinar.ingtonite and reibeckite . the saaale passes., jf <0.5Z of the aabeetifor hab.it* ate present the sample passes. (Kota? The polarizing micro scope with dispersion staining will detect C.C1Z of any mineral with not more than 30 minutes scanning time and l the particles' are,, at least 0-2 r 3
P.>
PAST I -- ASBESTIFOSK HIKERALS 3Y X-KAV DIFFRACTION
Principle
The ix-ray diffraction' m ethod is based up o n che principle th.it when a crystalline m a t e r i a l is pl a c e d in an x-ray bean* a por t i o n ef Che x-rays are diffracted b y ea c h set of atomic planes wi t h i n tht crystal* Th e dif f r a c ted rays strike a s c i n t i l l a t i o n counter .as the sample is scanned through a prescribed an g l e y i c h . t h e res u l t i n g dev e l o p m e n t of p e a k s c orresponding to each Interplan-ar di stance ( d ) .' A p e a k w i t h a d value in the range of .8,04 to 6.65 A for a talc sample is strong evidence for . the presence' of a m p h l b o l e . The licit of detection of assphibole by careful application of this DJthod Is 0.5a .
Apparatus 1. X-ray diffractometer employing nickel-filtcrcd copper K-alpha radi
ation, horlscntal or vertical gonio^tar with variable scan speed capability, suitable talc pellet sample holder* variable speed recorder, electronic panel including fa-teceter variable attenuation and cine constant settings
2. Hydraulic press, capable of attaining a pressure of 15,000 to 24,000 lb applied to a 3" raa
3. Jiortar and pestle or grinding mill (Note 1) 4 Waring Blonder, or equivalent blender
5. Spex ilixer/hiillr o r equivalent m e c h a n i c a l u i x e r 6. Sieve, 325-nesh
7. Optical microscope (Note 2) B. l-L/4*1pellet press
Kfrap.ents' ' ,
1 Standard calc sample, containing no detectable azphlbole idncrals
2, Standard tronollxa sar:.,lfr (at; Xecrt 55* pure.), rray be obtained by ordering frott The Ccsrictne Toiletry and Fragrance Association,
Inc., 1133 Fifteenth Strict,
Washington, U.C. 20S05
3, Denatured ethanol
' A. Boric'acid
Procedure The procedure consists of scanning il'/nin) under otherwise high
civic/ conditions, a compressed pellet of the sazple Calc over the 2 range frore V to 34* ('about 20 A to 2,fi A) with Cu Ka radiation- Check, the recorded trace for the peaks tabulated in Table 1.
" TA3LE 1
?
Possible Characteristic Strong Peaks in the X-Ray Spectrun of Talc
7.6, decrees
6.31 9.45 9.66 10.5! 10.5! 10.55
10.61 12.01 12 404 12*20 12.51 18.50 19,32 19.45 19.48 20.49 20.83
dr A
14.0 9.35 9.15 8.40 5.40 8.38
8.33 7.36 7,34 7.25 7.07 ' 4.C74.59 4.56 4.53 4.33 4.26
I
so 100
20 100 100 100
100 100 100 ICO
8 a 45 25 12 6 35
Klnercl
chlorite talc cutaingtonite (azosite) crocidoiite hornblende trev-dite act indite,
nnthophyllica cuwringtonite chrystile lizardlcc antigorite talc talc tele talc tale talc quat tz
23.02 24.30 24.50 24.57 25.25 25.ES 2.64 27.26 27.33 27.53 2S..59 2S.60 23.60 28.63 25.77 23,16 29.55 30.96 31,60 31.76 . 31.32 32.19 32.46 32.63 32.83 32.90 33, C9 33.15 33.19 35.60 35.85 36.04 ! 36.56 33.43 39.40 41.40
3.66 3.66
12 100 ' .
3,63 3.52
60 60
3.541
60
- 40
3.343 3.26B
100 75
3.2b
30
3.23
50
3,'121
100
3.12
40'
3.12 3.11 3.10
55 100
70
3.05
100
3.02
100
' 2.BS
100
2.629
20
2.314 2.SI
100 ' 100
2.773
60
- 2.756
70
2.742 2.725 2.720.
100 40 60
2.705
90
2.70
30
2.697
20-
2.52 2.503 2,49 2.455.
30 18 100 ' 80
2.337
2
2.255 . 13
2,192;
30
calcite ebryeotile lijardite antistite Chlorite epatite quart*; trendite hentblends anthophyllite traudite talc croeidolite accinolic-e hornblende. Txthopuyilite amoslte calcita dolomite chlorite apatite calcite patite sbasite magnesite trocxdolite apatite trillalit e actinolltD hornblende antisorite magnesite liaardite chtyeotile tale calcite docile
41.58 41.59 45.08 45.81 46.05 48.65 50.16 50.55 51.10 51,25 53.88 59.26 '60.24 SO.41 60.50 61. SO
2.15 2.102 2.095 1.94 1.BS2 1.870 1.817 1.804 1.786 1.781 1.700 1.558 1.535 1.531 1.529 1.500
60 45 18 12 50
4 17 20
30
35 2
60 70 55 60
llzardltc magnesite calcite ctrgnesice tremolite talc quart* dolomite
doXoalte
magnesite tale eUtysotile lirardite talc li^ardite
Soiae ciincrals, ag. > carbonates, quart, -hornblende ate. have been listed here not because of any known harmful effects but because they cay be ob served in talc staples.
Under ideal conditions 0.5-1.OX of all of the above minerals should be indicated by a possible peak in the 4*-34* range. Appropriate peak re gions for the indicated mineral should then be scanned at 0,1'/min as Indi cated below.
Should the pres e n c e of a small p e a k abpva t h e background *fn c i s e M b e In question, It will be necessary to s t a t i stically e valuate the scan ca d e at 0.1 V a i n In the suspected peak rcgion(s). A timer/scaler la required on the electronic panel of the x-ray diffractometer. In order for a peak to be statisticfilly significant, the peak intensity must equal or exceed three stand ard deviations (3<? ) above the a v e r a g e b a c k g r o u n d i n tensity (20*
K + 3d - minimum peak intensity,
N - average background count J W i T
"ia-ik"
10.0
10.2
-Tigure 1
"A" 10.4
10.6
10.3
10.8
10.7
11.0
*20
Exac?1c:
In Figure 1.
PBeaackkRRgreeoggwiiooidnn AB.v ./.n.,i
R10e.g4i0onto(' 1200).60 ' 1100..7400 '
Tine120(se c .) 6600
1ti0n.4e0sPteoetask1. 0.60c*o2u5nt
A v e111r222a000g e
-6560900.,.,B13103075220
*
Background
1ti0n.3e0Re:tegociosn1. 0A.40c*o2u6nt * 1ti0n,6e0Rseteoegsio1. 0n .7B0-c*o2u6nts
666000 22228383,,,1779688457434
666000 22228S38,,,,233506504896
S'- 28,737 + 28,359 - 57,146
.* - 57,14 6 - 239
34 - 717
N + 34 V 5 7 . 1 4 S + 717 = 57.B63
The actual number of counts obtained for the Integrated peak Inten
60 102sity u as
, ; therefore, the "suspect" peak Is statistically present In
the scan.'"'
Standard Preparation ** Opcijnal ins t r u m e n t conditions itust first b e determined w i t h the use
of stsndaT.ds c o n t a i n i n g 1.0?,"' 0.752, 0.5* b y w e i g h t of the suspected contactc a s t prepared in a s tandard talc vhich-*is free of i n t e rfering peaks.
Vc i & h out a p p r opriate amounts of the standard talo a n d the fcineral of incot both of w h i c h ha v e been ground ' to pass a 325-neah slave. Transfer ta a W ari n g iilcmdot. Add 100 Til of ethanol to the blen d e r and blend at low spaed for 5 Kimices.
Carefully transfer, with repeated ethanol vachlngs, the- contents of the blender Into .a large beaker. Eva p o r a t e the ethanol on a steaa bath.
Shake the sample in a p lastic v i a l for ` 5 m i n u t e s on e. Spox H i x er/Kill to remove clumps and caked sample r e s u l t i n g f r o a t h e evaporation of ethanol.
Determine b y microscopy tie homogeneity of the prepared standard previous to eho x - r a y d i f f r a c t i o n analysis.
- Tress the h o m o g e n e o u s standard into a 11 /4Tl pellet wi t h a b acking of bqrie acid. Transfer 2 (-0*2) gran of standard to the die-holder end. evenly distribute an a polished, scratch-free die. Distribute 4 (0,2) grams of boric acid evenly on the talc layer. Press the mixture into a pellet un der conditions suitable for o b t a i n i n g a sm o o c h planai* surface (for example. a pressure of 15,000 to 24,000 lb c a l culated on a 3U ra m h as be e n found to pro d u c e suitable pellets). T h e resulting pellet mu s t h a v e a ta l c faee w h i c h is
3free of flaws; if not the pellet must be d i s carded (lot* ).
Sample Preparation Prepare two pellets from each sample In the manner described for
the standard pellets. Make a cualitativa scan fron 4 to 34*26 on one of these pellets to a s c e r t a i n the pre s e n c e of non - t a l c m i n e r a l s h a v i n g int e r f e r ing peaks.
Ir>crumen ration
Instrumental variables ^re optimised on the 1* standard. Lever
standards are then analysed under the'optimum conditions to deter
mine the lover level of detection. Of-major importance in obtain
ing maximum instrument sensitivity are o slov diffractometer speed
combined with compatible recorder speed, and high attenuation com*
bitted w i t h a statistically a c c eptable time constant o n the raccme-
, ^Jnder a p p r opriate instrumental conditions the peak obtained f o r the 0 ,5X standard should be d e tectable'above background no i s e as sbevn in Figure 2 tor trcmolite.
Typieal instrumental conditions employed for the Siemens Diffrac
tometer (Model No. MISS-X'-M), and C o u n t e r and R e corder U n i t (Type T) are:
Radiation: Cu with Kct filter at 40KV and 24 mA. Divergence slit: lp Receiving Slit: 0.2 rm`(,007M) Goniometer speed; l/10*2e/rvinute
Recorder speed: ICO mm/hour
Attenuttion: 1 x 103 impulses/second Time constant: T (e) 4
Statistical e r r o r of l.`l l u n d e r these conditions
Rise Tine * O.lS Attenuator "20
P A R T I I ; A S i E S T I F O R M AKPlilbOLii M U S K A L S BY P O L A R I Z E D L I G H T MICROSCOPY Ai:C D I S P E R S I O N STAIKJi.'C
Apparatus
Polarisiliig, rcucroscopc* Best results vill be obtained if the Instru ment includes the following:
a. Individually 'centering objectives at centerable stage
b. Bertrand .lens c. Kigh^intanclty light source d. Centering condenetir/sulctage 2, Disp e r s i o n staining device (licte 4) 3. V a c u u m filtra t i o n equipment^ in c l u d i n g either a. p o r celain cc n a v i t h glass fiber filter M t or a po r o u s gl ^ s s bettor, c u p
-Reagents
2. Cargill* iianorsion liquids* nj: 1.550 (tD series!; {Kote 5)
n " * 1.605 (lib " ) '
Op5 - 1,660 (Its " )
n*5 - 1.710 (M " )
Optical microscopy and Dispersion Staining
Carefully adjust the dispersion staining objective for optimum viewing of central stop colors. Tie microscope is first'arranged for Kohler illumination! lamp iris (field, .dlaphraa) in focus in the field of viev; lacn filament in focus In objective ba c k focal plane.- The leap, if movable, should b e placed' clo s e to the n i r r o r so that, the inage of the lamp filament is as snail as possible in the objective back focal plane. Thie along vith o y ervolting the l&ap b y 15-202 and retovinfi Che da y l i t c V l u d filter v i l l .ensure bright central stop colors and d e t e c t i o n of subn i c r o d o t c r p a r ticles.
T h e s u i t should ne x t b e eeaterr.-d and the contrai scop should be 'precisely centered vich respect to the iitace oi the s u b e t c e iris (aperture diephrea) in the objective back focal plane. The substage .iris is then closed just behind the central stop an d th B e r t r a n d ,Ions (otf e q u ivalent vi e w i n g syptesi) Is removed. h T h e preparation 1b sciumed for Xg colora in the visible; critical study of n a r e a or of a given particle is carried out with the field d i a p h r a n n ea r l y closed around 'the center por.tlon of the field of view.
Aor.tlflatlor. of tton~talfc_feindrais by dispersiCr. stcinin.
Kount a r e p r e s entative s a m p l e (about 0.3, tog) in Che following Car- fiillc refractive in d e x l iquids and exa m i n e carefully for nor.-talc aube tances. The particles a r e laourvced in the drop of C argille liquid bet w e e n slide and coverslip. The particles are best dispersed by eliding the covcrslip with a rotary ic^tion of a pencil* er a s e r "gr i p p i n g 1' t h e c o v c r e l i p .. T h e final pi-cp should' h e thin and the cbvcrsllp should b e p arallel to the slide (this avoids a Vprisa" shaped prep that will decenter the image of the substagt iris relfctivc to the cen t r a l stop). The slide and covcrtlip imst be carefully cleaned before, u s e and the pencil eraser tnust be- `dipped in diluted rubber cement and dried before use co avoid transfer of particles to the top of the coverslip* The minerals to b e checked fer include;
Chrysotils
Lizidite
Antirite
Chlorite Quarts
Calcite
Doloiaire
K&gndsltfe
ttorrtblehe
Forsterite
Talc
CAn tlioJih.y11 i <
Trenolice
Act i n d i t e Aasostc
f Curminaconitt [ Crun^rite
Ctocidclice
f Claucophanc { Ricbctfcice
a cr t
Refractiva ndices S t or e
1.3 1.3 1.564 1.600 1.544 1.658 1.679 1.700 1.655 1.640 1.540 . 1.525 I.59S
.2S
1.646
_
E l . 566 1.603
1.665 1.656 1.509 1.635 1.612 1.640 1. 653
1.556 1.556 1.570 1.610 1.553 1.466 1.500 1.509 1.672 1.674 , 1.595 1.650 1.622 1.650 1.674
1.660 1.630
1.70 1.640
1.715 1.645
1.695
1.704
1.710
Minerals * especially silicates' t u t also the isorr.ofphous series of
carbonates (calcitci dolo-Ita* riagnesita etc.) vary. , in r e f r active index.
Figure 2 a. and b. s h o v ave r a g e indices for the m inerals v h i c h n i g h t he found
in talc. Generally, the d i s persion s t aining curves for these liberals r a v e
parallel to themselves as the c o m p osition c h a n t s , th e bir e f r i n g e n c e values
Cv-** 3-a and c-v) vill generally remain nearly constant for a given mineral
although the indices themselves nay very considerably* , T h e combi n a t i o n of crystal morphology, 'and optica is else a great
help' in m ak i n g sur e of the i dentity of a g i v e n m ineral* O n e should loch for
different vietra of a given mineral an d / o r va r y the v i e w on a single crystal
by tapping gently on. the top- of th e cov e r s l i p v i t h '& cecils. I n this way
fiberlike talc plates os edye can be tipped into the plate view and quartz
Can b e m a d e to shov c as v e i l as u.
1*
Sot h morphology end optics are noted 'in order to identify the
asbestiforcnincrals. To be asbestiiora requires that they be fibers* not
slivers* s o u r i n g < 3 pm,in diameter, < 3 0 nm in length and ho v e a length to %*
v i d t h ratio ot at least 5:1.
Examine the Semple for nsbestifotr^ or fibrous japhlhola minerals
I n orde r for a n ocphifcolc T en o r a l to be considered asbestiforra. or
fibrous it ff.vet m e e t the folloving QSItA def i n i t i o n (Reference 4),
1. .Particles must, appear to b e fibrous r a t h e r then as crystals or sli vers*
2* T h e martimta diar'ieter of a fiber to be counted is 3 Tricromctcro. 3* `The m a x i m u m le n g t h of a fi b e r to be counted 30 micrometers. h. T h e length to v i d th-tatio r w s t be 5 or more to 1, chat is* 5 tines
6r more'lonse* than vide.
5. The separate or individual fibers =u s r c ontain fibrils or the "'bun dle .of eticka'".effier, unless they ere at a nori-divisible stage, A. fibril ejnnot b e subdivided ana would oc counted* if it meets Che other criteria. T h e length to width ratio of 5 or aorc to 1 is net meant to imply th.it other particles are tot hazardous.
The analysis proceeds by pouncing the sample in successive Cargills
liquids w ith identification of each mineral shoving visible 1q colors in each
liquid. The first liquid is n D - 1. 5 5 0
C a m i l l e hith disirrersion licieid
" 1.550:
-- :-- "
- 1
---- -lr---- *----
A representative ssrple, tbout 0.1 eg co u n t e d in this li q u i d vill
sh o w characte r i s t i c Xq colors for any^ of th e following: talc, quartz, c hryso-
tile, iizerdite, ant i g o t i t e and na n y fibers (paper* silk, v iscose raycr..and
human hair e t e O , The crystallographic data in Figure 2 should ensure iden
tification of most of these substances or allov the conclusion that any other
substance shoving colors it this liquid is net o n e of th o s e listed (Figure
3). Characterizatio n of this extraneous substance v i l l often. b e p ossible b y
referring to the Farticlt Atlas,
Carftille hitih difl?prsion liquid rfj^ - 1.6~>5i Chrysotilc and all other substances giving. dis p e r s i o n s taining col
ors in liquid 1.550 will bo w h i t e or pal e ' b l u e In 1,605 (Figure t ) , Ta l c is the on l y s u b stance in this gr o u p that shovs a Xq close to the v i s i b l e (ca 7G0 n n ) . All talc plates sh o w b oth n ' > (fc & *y) close tD 1*605 in the red hor.ee the central scop shows a pale blue in all directions lying in the talc plate and w h i t e correspond i n g to the e direction. Ocher m inerals s hoving colors in Ojj * 1,605 include trc~.olite, c h lorite a n d actiriolite (Figure 5}.
Carftllle Liould
*= J.660 Cf.F s^ries^
Hon-talc minerals shoving dispersion staining colors in
1.660
include actlnolite, fersterite, hornblende, calcite, eusaingtonice and dolo^
m i t e (Figure 6).
tttl'HA'J IIVt- it'JULA Uf OMUiilt_LU LIWUIU
X o WAVELENGTH C n m
Fisura la. Dispersion staining curvea
Anclioiibyllitc Chlori.Le (y)
Chiarite (cO
Trcrr-llte (a)
T.-C (y )
t)
ftO c
-rae -
Ant f,ori te (y)
AnUCf^iCc (o)
I.irnrt te ('') Chrysotilc (y )
LimriSUu. (a)
(Juarir '(t) Chrysatilc (ti) Qunrtz (u) T a l e (a)
foGnesite (c)
Dolomite fe)
C a l c i t e (c)
31.710 Cf
UJ1.700_J = IODO
<P ce
g.680
HIJL 1.670
rUJ1.600"
Q v
ISSO
>UJ rir
t-- lo^O--- Oi < T~ - 1530
J rLU
ce1520
L6I0
tsoa
oa
Fleure 2b. Disperslot etolnlnfi curves
Tatt:
vlyLte-yclltv (<4C0) -Srycllow (<4Q0)
Quartr;
j
coiichoidal flakes, ail.&hov X^ ca 630 na corresponding to u on.rocation o ihfi'scaco; 90* fsron the u orienta-
tior. iitber e ti JSO n-n) or any c' {5S0 cl0 <SQ), U
--+-- white yellow vhitc-blue (>7G0)
'Chrvso,.,tr-'i-l-c:
a ,blue (660)
Y r
rc<i TT`J':nca (520)
f
r- 1
T
0-
- red's'-inta
(52)
Paper fiberst
irregular rounded fibers
yellow-white X X T v ^ F v 'S S fpalc VIpc
tisarltci
Aggregates of very fin plates,
r.'s .slight > chryootile* 0 i y in
plane of platen Ju^ m (blue
magenta).
Antifloritc;
jG (ca 41Q) 0 pole yellow
L pale a , ft ^ pale ___ Ij" 'll yellow 4.d golden yellow (470) (ca 400)
Figure 0. Central step dispersion staining colots In 1.550 (IIS)
Cartill! Liquid
Tilc:
1 .G5 ;
Treniolte?
vhltc
7Cp>
Actrnolite;
Ficure 4 General stop dl.persiGn'stanlng colors in Carglll* liquid tip ^ 1 * 6 0 5 (O serles)*
AccpoIIc;
Calcite:
r'^I~ |v.'pale blue (>>700),, TV*,jlue-trr-fm (ca -GO) -- L_______ Lj
r
l, Tcrrtericei
3 pale Mue (>700) . ------h-lei1 (ca 700)
. ra --
r1 j
ycllow (4$G)
A?^
*-1
jJTil1
bv.lejcv'-cfltorcijrjrIiuc(-f-i(C>.)7L`0*0)
"t
Kari-M^rtdc::
Ci'~-'::'.~vanire;
aj Mui'-srfctn (660)
~rZ7~
j
yelicu o^yo)
/patite:
Wt bluO'*recn (700) p/iie Lluc-fcrccti (>700)
-- l blue (560)
r`- + f.alflfrn T
(510)
uc-n.rccn (700) b l ue-grecu (70)
ligure 5, Central acop diap^Tsion. scainitig colera in CarciUe liquid nD l^i&u (R? aerles)*
wj i;
Cufriir.gtiafii a * vhitc (7G0)
Ct`un<Ti tt:
, Y\
v ple blu e (>700}
V. pal* blue (*700}
v p&lc blue (>7Q0)
ay T>ii)e M u4 (70S)
Figure 6* Central stop dispersion staining colors in Cargille liquxd tip * 1.700 (!i series).
Caraille 11 raid n t Q 3 , 7 6 0 (K series) Minerals to look for in r.^ 1.700 Include cunningtonitcv grunc-
rita, crocidolite and lr-aghesite..
] cKurort rp ..iritis a ^sbcsc-f fotra AneMholt Present" or aft *V,shfchtifQrtB A m o M -
bo Ab:.atii.u `It is imperative that both diapersion-staining color ar.d fibrous
morphology criteria be satisfied before identifying a particle as asbestiform asphibole, since other substances nay show colors `similar to those described.
jtetes
1. Talcs to be analyzed and the'-itandard minerals used zo prepare standard samples raist be -325 raeah (maximum particle else of 44 mi crometers). Te'-osar Analytical Will {Model A-lQj is recocnaended.
It.is available from:
371C2Tekmar Company
F. 0. Sox Cincinnati! 0*A 45222
>
2. It is important tint the hero^Bncity of the prepared ralc-cremelito standard socples.be verified by optical microscopy.
3* This requirement is critical since excessive surface scatter will .cause abnormally high background counts.
4. The only CDrcxrcidlly available dispcrcion staining device is sold
by;
Valter C. McCrone Associates, Inc.1 2S20 South Michigan Avenue Chicago , XL 6061-4
5. Available from:
P, ?> C a rgill* laboratories, Ittc.. Cedar Grove. KJ 07009
or from laboratory suppliers
References
. l k Rohl, A. N t A, H. Longer, EnvIronTrentaJ H e _ I t h fer s - e c n i v e r 9 9^ (1 ? 7 -----------------------------------------------------------------------
2* Rubir, I* 2. X. J. itaftfilorc. EnvifonnenCiil Health Perspectives 5.
.81 (1974).
--------------------------
3. L. S. Birhs, X-P.ny Spcctroetiralc.il Analysis, pages 5455, later^ science Publishers (1959),
4. "Trenolite and Tale.11U.S. Department of labor, Occupational Safety and Health Administration, Held Infornacion Kenorandun J74-92,' Sover.ber 21, 1974.
5. IfcCrone, H. C. and J. D. Dally, P a r t i c l e A t l a s . 2nd Edition, A n n Ar b o r Science P u b l ishers, Inc. (1973).