Document QJVnzvyQB3GbR2Va59bnzozmL

FILE NAME: Johnson & Johnson (JAJ) DATE: 1995 Aug 21 DOC#: JAJ068 DOCUMENT DESCRIPTION: J&J Consumer Companies Worldwide Specification (Strictly Confidential) Analysis of Powdered Talc for Asbestiform Minerals by Transmission Electron Microscopy J J&J Consumer Companies Worldwide Specification Issued Strictly Confidential A N A LYSIS OF POW DERED TA LC FO R ASBESTIFO RM M INERALS BY TRANSM ISSION ELECTRO N M ICROSCOPY Name TM7024 Type Test Method Content Nam T N 7024.d o c Reference Documents Name TM 7024-Revl Protected Document-Subject to Protective Order Form at generic Description Strictly Confidential ---------------,-------------------------- Pile S h e 35640 I e x h ib it 1 Page: 1 of 9 JNJNL61_000006032 Related Specifications IName I User Defined Attributes No Objects Found Additional Attributes No Objects Found No Objects Found IType No Objects Found TM 7024-R ev1 Protected Document-Subject to Protective Order Strictly Confidential Page: 2 of9 JNJNL61_000008033 C om pany: PersonalProducts Worldwide Personal Products Company Desblens ProductsInc. D ocum ent No.: T M 7024 Test Method F ra n c h ise ; Johnson <kJohnson ProductsInc. Odonto Corporation Ltd. X Johnson A Johnson Consumer Products Co. Location: ROYSTON, FLUID, KOLMAR D ocum ent Type: Permanent E xpiration D ate: None Subject: ANALYSIS OF POWDERED TALC FOR ASBESTEFORM MINERALS BY TRANSMISSION ELECTRON MICROSCOPY___________________________________________________________ R E V ISIO N 03/08/89 03/21/95 08/21/95 AUTKQ&KATIQM____ DESCRIPTION OF CHANOE BCR0113S2 New Test method. CR020127 Location revised. (Spec. D ept) CR020688 Issue Date: August21,1995 TM 7024-Rev1 P ro tected D o cu m en t-S u b ject to P rotective O rder Strictly Confidential Page 1 o f6 Page: 3 of9 JNJNLS1_OOOOOSOS4 C om pany. Personal Products Worldwide PersonalProducts Company D eviens Products Inc. Test Method Johnson 4 Johnson ProductsInc. Odonto Corporation Ltd. X Johnson A Johnson ConsumerProducts Co. D ocum ent No.: T M 7024 F ra n c h ise : Location: ROYSTON, FLUID, KOLMAR D ocum ent Type: Permanent E xpiration D ate: None Subject: ANALYSES OF POWDERED TALC FOR ASBESTTFORM MINERALS BY TRANSMISSION ELECTRON M ICROSCOPY__________________ __________________ 1-0 SCQES&HIBPQSE Ib is method is applicable to the identification and quantitation of small (typically 1-20 micrometer) asbestifonn minerals in powdered talc. Samples may be previously screened w ith light microscopy or x-ray diffraction techniques. 2.0 The combined techniques o f transmission electron (SAED) and energy dispersive x-ray analysis (ED! on morphological characteristics, followed by a area electron diffraction o f aribeitifonn minerals based identification o f each fiber. 3.0 INTERFERENCES >are caused by fibrous adbestos, and by large particles or particle nafrg& estos fibers include rolled taktffljfron additives such as peritonea may ciy MMIF#-F products. In the absence o f positivi from positively identifiable rosy obscure fibers. Positively identified silica fibers and iron oxide fibers. Organic 1 or needle-shaped crystals in finished cosmetic l, all otherfibers m ustbe classified as unidentifiable. 4.0 The talc soedm en of 20.000X and 5.00X. TEM at an accelerating voltage of 120 kv and at magnification 5.0 SB N SrnvITY This method is capable o f detectings single fiber aa small as lm icrcaneter(m m )km gby 0.075 mm wide in ti entire T E M fidd, which results in a theoretical detection lim it of 10-5w eight percent Such fibers usually canbe identified readily by SAED and EDXRA. The mass of a fiber w ith the above dimensions is 1.1 x 10`u g firr chrysolile and 1.5 x 10*14g for amphibole. 6.0 LIMIT OF QUANTIFIABLE DETBCTEQN The detection o f five or mote asbestifonn o f one variety in an analysis constitute a quantifiable level of detection. W hen no asbestifonn minerals are detected, a representative fiber size is used to calculate a detection lim it A representative fiber size is 3 ram longby 0.2 mm wide by 0.06 m m thick, which is considerably larger than tte sm allest fiber that esatbe detected (see section 5, SENSITIVnY). b u t is more lypical o f small asbestos fibers that are detected in talc analyses. The mass o f five such fibers is calculated as follows: 3 mm x 02 mm x 0.06 mm 0.036mm5per fiber x 3.3E-12 g / mm* 1.2 B-13 g p er fiber Issue Date: August 21,1995 TM 7024-Rev1 P ro tected D o cum ent-S ubject to P rotective O rder Strictly Confidential Page 2 of 6 Page: 4 of9 JNJNL61_OOOMSOM Test Method C om pany: Personal Products Worldwide Personal Products Company Desbiens Products Ina Johnson A Johnson Products Ina Odonto Corporation Ltd. Johnson & Johnson Consumer Products Co. D ocum ent No.: T M 7024 F ra n c h ise : Location: ROYSTON, FLUID, KOLMAR ' D ocum ent Type: Permanent Expiration D ate: None Subject: ANALYSE OF POWDERED TALC FOR ASBESTIFORM MINERALS BY TRANSMISSION ELECTRON MICROSCOPY_____________________________________________________________________________ x 5 fibers - 6E-13 grains per 5 fibers. The lim it o f quantifiable detection for most talc analyses is approximately 6 x 10"4weightpercent H u theoretical and quantifiable detection lim its assume homogeneity o f the material being sampled. 7.0 QUALITY ASSURANCE Blank suspensions are routinely prepared and tested in order, from the samplejars. Blank carbon-coated grids are greater th an 4 fibers per grid are present, the jais aro respective o f the test potential residual contamination rnitor the ambient fiber count. If or ne'aibon-coated grids are prepared, 8.0 BACKGROUNDCORRECTION As o f the tim e o f this writing, background cor aftvtrfns hag h m tn qignifiwiTrt j . The amount ofbackground the levels of asbestos found in contaminated samples. 9.0 PfffiP M A M ANPANALYSIS Preparation tim e per sample (incl per sample is a maximum o f >no frelated materials) is one hour. Analysis search time 10.0 APPARATUS 10.1 Analytical balraB^W th <0 g am sensitivity 10.2 W eighing bhonattes V 10.3 Narrow spatula 10.4 Wide month polyethylenejars (125 ml) 10.5 M ild ultrasonic bath, minimum 50 watts 10.6 M icropipettor (5-10 m l range) w ith disposable tq s 10.7 Standard 3 mm diameter, 200 mesh, copper TEM grids, covered w ith a carbon-coated fbrmvar film . 10.8 Transmission electron microscope (IBM ) w ih an 80-120 kv accelerating voltage and energy dispersive x-ray analyzer. Issue Date: August 21,1995 TM 7024-Rev1 P ro tected D o cum ent-S ubject to P rotective O rder Strictly C onfidential P ag e3 o f6 Page: 5 of 9 JN JNL81JM M 0M 38 Test Method Personal Products Worldwide Personal Products Company Desbiens Products Inc Johnson & Johnson Producs Inc. Odonto Corporation Ltd. X Johnson & Johnson Consumer Products Co. D ocum ent No.: T M 7024 F ra n c h ile : Location: ROYSTON, FLUID, KOLMAR D ocum ent Type: Permanent E xpiration D ate: None Subject: ANALYSIS OF POWDERED TALC FOR ASBBSTXFORM MINERALS BY TRANSMISSION ELECTRON M I C R O S C O P Y _______________________________________________________ 11.0 BRAGENTS 11.1 M ethyl cellulose, powder, USP 4000 cps - Fisher Certified Reagent #M~352 or equivalent 11.2 Water: deionized, particle free (+0.2 mm filtered) 11.3 M etfyl cellulose solution- 0.002% (w tfti) (20 j 5 00m lof deionized particle free w ater to make t working solution. 20 % 0.5 m g o f methyl cellulose in solution. D ilate 1:1 to make a NOTE: M ethyl cellulose a d s as a sample dries, by greatly reducing the 12.0 SAMPLEJ^ARAUQN 12.1 Transfer 30 to 50 mg o f talc uniform particle distribution as die ;5 m l polyethylenejar. 12.2 Add 80 m l of 20 ppm nut cap and shake vigorously for one m inute 12.3 After staking, Then shake again fo r 10 minutes in order to disperse the finer particles. 12.4 immediately a ftst^ u rid fiL m a p and remove 92 microlitars with a micropipette. 12.5 Transfer a 9 ml d i^ ^ x a u b o n film covered TEM grid. (Grid was first lightly anchored by 2 parallel strips o f d o u b le* b k tape mounted 3 mm apart on a clean glass microscope slide.) Repeat to make two sample grids per talc sample. NOTE: Do not expel tte remaining 0.2 m l ssqK oaian from fee micmpipette tip. it tends to sputter and frequently destroys the stability o ffee sample drop. 12.6 Transfer slide w ith grids to a desiccator. (Drying time is 2-3 hours.) Do not leave the grids on the slide fo r more than one day as the double-stick tape may adhere too tightly. NOTE: The talcrwater ratio may reed to be varied fcr some samples. Preparation o f talc samples w ith a significantly finer or co a rw particle size results in large differences in particle coverage on the TEM grid. Issue Date: August 21,1993 TM7024-RSV1 P ro tected D o cu m en t-S u b ject to P rotective O rder Strictly Confidential F ag e4 o f6 Page: 6 of 9 JN JN L 81 _OOQ0O8O37 C om pany: __PersonalProducts Worldwide __Personal Products Company Desblsns Products Inc. Test Method Johnson <kJohnson ProductsInc. Odonto Corporation Ltd. X Johnson Si Johnson ConsumerProducts Co. D ocum ent No.; T M 7024 F ra n c h ise : Location: ROYSTON, FLUID, KOLMAR D ocum ent Type: Permanent E xpiration D ate: None S u b ject ANALYSIS OF POWDERED TALC FOR ASBESTIFORM MINERALS BY TRANSMISSION ELECTRON MICROSCOPY____________________________________________________________________ 13.0 TEM ANALYSIS 13.1 Definition o f fiber: An elongated particle w ith parallel sides and an aspect ratio 3:1. The ay vary w ith the needs o f the client 13.2 Scan sample at 120-150X magnification to check for < dispersion o f particles and to locate grid squares w ith optimum particle density. (Optimum j is particle coverage over 15-35% of the field of view.) 13.3 Scan three grid squares on each grid at 20,0 5,OOOXforasbestifbrmminerals. E ach: tremolile, anthophyffite, etc.), structure ( and seven grid squares on each grid at recorded as to type (chiysotfie, and dimensions (length x width). 13.4 Questionable fibers are examined f ia t Amphfijole SAED chrysotile SAED pattern is unique and >utusually characteristic. Additional analysis done if warranted. 13.5 Ten percent o f d ay sotile patterai not clearly examined by ED! EDXRA for further confirm atioa If the SAED consistent w ith an amphibole SAED pattem , dim it is ition o r to identify the type o f amphibole. 14.0 CALCULATION OF RES! 14.1 M assofchry MCE) - 3.14159 r =*fiber radins 1 = fiber length d = density o f chrysotile - 2.55 x lO^1 g/mms 14.2 "asbestifonn amphibole particles: M(4) M ta l-lx w x th x d 1" length w-= width th - thickness g 0.3 width (approximation) 14.3 Mass o f talc deposited on each TEM grid: M(s) M (s)T x(V /fI) T " amount o f talc sampled (step 12.1) V volume o f aliquot transferred to 1EM grid (step 12.5) Issue Date: August 21,1995 TM7024-ROV1 P ro tected D o cu m en t-S u b ject to P ro tectiv e O rder Strictly C onfidential Page 5 o f6 Page: 7 of 9 JNJNU1_0000M0M Test Method C om pany; Personal Products Worldwide Personal Products Company Desbiens Products Inc. D ocum ent No.: T M 7024 F ra n c h ise : Johnson <t Johnson Products Inc Odonto Corporation L td 2 Johnson &. Johnson Consumer Products Co. Location: ROYSTON, FLUID, KOLMAR Document Type: Permanent E xpiration D ate: None Subject: ANALYSIS OF POWDERED TALC FOR ASBESTTFQRM MINERALS BY TRANSMISSION ELECTRON MICROSCOPY_____________________________________________________________________________ H - volume of methyl cellulose solution (step 12.2) 14.4 Tbtal estimated talc mass examined: M (t) M (t)= M (i) x (N x A(s)VMg) N = number o f grid squares examined A(s) - area o f a single TEM grid square Issue Date: A ugnst21,1995 TM 7024-Rsv1 P ro tected D ocum ent-S ubject to P rotecflve O rder Strictly C onfidential P ag e6 o f6 Page: 8 of 9 JNJNLS1 000005039 This document is generated by an electronic system. END O F DOCUM ENT TM 7024-R ev1 Protected Document-Subject to Protective Order Strictly Confidential Page: 9 of 9 JNJNLS1JDOOOOS040