Document omG1712XB9ro2QJdpG3EgOLJE

gjggjg- . jfrBjiyyf .s:~Vrt :- '.^-p'r-?!^ " y 'i~. ^5 '--MiW 2U PONT 22 NEMOURS AND COM?ANT 22X2222 2I3ERS DEPARTMENT C-&C Si- PLAINTIFF'S EXHIBIT DUP-54 MANUAL OF ENVIRONMENTAL ANALYTICAL METHODS METHOD N'C . ?5 37 REVISION NO._ '22: ASBESTOS IN AIR-AREA AND PERSONAL MONITTBING APPROVED BY: Signature or Departmental 2AM Coordinator Dare NOTE :5active adoption date Departr.entaliy is the date the method a approved by the Department AM Coordinator. * Originating Oiviaion only V73 OUP 0904296 &M*tali' -iy* r iiL :M. _J_ rechkecal sEeIXch SAM 9137 AS3EST0S EH AIK, .. AREA AKP PEP.SOHAL MCHTTCR3G :. prehceplI asbestos la air is collected and determined by drawing air through a membrane fliter by~meane of a battery powered personal sampling pump. Ehe filter is chan transformed,by chemical treatment, fro* an opaque solid membrane :o a cranaparanc opeicaiiy homogeneous gal. The fibers ara alzad and counbed using a phaaa-concrase mcrcaeops ae 4C0-450X aagnificacions. PRECESECM AHD TTME RZOtrXRgl A. Coefficisnt of variation dacarsinad in raferanca is 16.2, which indue as exparlancad and nen-experianead counbars. 3. Tonal analysis elna required for one sample (does noe include sample collacblon) is 1.2 hours, and for eighb samples is 3.3 hours. EEX. ECCHCKIC5 A. Standard oparator bins co make a single dacaminaclon has not been sat. 3. Cost of materiel for a single determination is SO.90. 77. RErEP-SHCZ CSTH/HIOSH senbesna filter method for evaluating airborne asbestos fibers, 3I7XSXOH_OF TRAIMIHG, u. S. 3EET. 0? HEW, CEHCEHNAII, OHIO (1974). v. soorpjgyr amp material specijIcatioh A. Sampling Equipment 1. HSA portable parsonai vacuum pump or equivalent - Mina Safety Appliance Company, Pittsburg, Pa. Specifications - Able so oparaea up to 3 hours ae a constant flow rata of ae laaat 1.7 Hears par sinuea against a rmaiatanca of If.2 centimeters of water aaaaurad at the pump inlet. 2. Laboratory eublng, plastic or equivalent with 6 niliinatar bora and 90 cantinscere long. 3. Clothing clip spring eo monitor personal, John T. McGuire Company, Pawtucket, SI.I. 4. Three piece filter monitor oaeeacta, Millipor* Corporation; Cat. Ho. PC37A0, praloadad cassettes. 5. Cellulose sealing bead, Minas Safety Applianea Company. DUP 0904037 zz'szt&xt and y-ATSF-i-u. A. Sagillnr vguirmenc (Coned.) (c;nt3.; .S.__p.30u 37ViM plain unite celiuloae ester membrane filter, Hillipore Cerp., ^Cic. No. 3CVP037C0. 3. ?viao Calibration loultaenc 1. Tubing-to-filter aonitar cuh::i adaptor, hillipore Carp. 2. ICCQ-al. bubble burette, Cat. :io. L04130, Lib Gli, lac. 3. ^Stopwatch, graduattd la 0.5 facoads, A. H. Thomas Ccopsny. 4. --SCO--al (lias baaicsr 5.^ Soap solution - 2 al Ivory dishwashing liquid or equivalent ia 400 al. water. C. Cotleal Tculpnent 1. . Bauaca and leas dynoptit aitroscope with binocular iaad or aquivalant. I. 10 3 Euygenian aya piaca* or equivalent. 3.JT3iuaca and Lamb PR-27 ribban-filanant illuminator (preferably built --ia and bavins provisions for adjusting light iatanaity) or equivalent. ^Specifications - Muse obcain Koehler illumination, in Appendix 3. 4. A portoa raticla or aquivalant. 5 Hachanical aeaga. 6. Abba or ZsrndJca condansar fitted with phase ring (or Haine) with a maarical apartusa 01 .A.) equal to or greater than the y. A- of the objective or aquivalent. 7. 40-453 (N.A. 0.65 + 0.75) posltiva phase contrast aehrcmatic abjective. 3. Phase-ring cantering telescope or bertrand leas. 9. Stage mlcrcmecsr with Q.OLhM subdivisions. 0. "liter Mounting iauipment 1. 2.5 x 7.5 s* glass alcroscops slides. 2. #1 1/2 (0.17J21) thickness cover slip. 3. #10 curved blade scalper or equipment. 4. 'Tweezers DUP 0904088  tr o 3 ;cL~n~acr Afro hAiiaiAi specification (cohtd.) 2. 3. -ana ciaaua - 6. Olaaa rod or equivalent '. _Vhaacon 3aliaa Bottle Z. ^eejeaca 1. Disachyi Phchaiaca OUagant Grade) 2. Jlieehyl ozalaea (Reagent Grade) - Heuatisg Solutlca Precaracion Add 5 a! disechyl pfachaiate to 5 si diathyl ozaiaea is a Wheaton Balaaa boctia. Add 0.3 (rasa of ouc up seobrana filter sacarial. the solution is ready for uae after 24 hour*. Stir solution Che fine hour, the cornel aheif lift ia 6 noncha. f. ProTeocora the aicroaoope isage say se furcaer projected :o aid counting, h'uaerouj projaccioa devices are available, however. Old Hicdory uaea a television aeeaod having a criaocular aicrascopc sained with a Miliiporerr MC caiavisioa casera aad soaicor. e unit ia saaufaceured by Hiliipore Corporaeioa. Bedford, nacbuiec:i 01730. DUp 0904089 1A30RAT0RY SEC7IC3 71. Afni^itLITT This nachod has bun successfully applied to ubtstoa la air ualag a 37>M nillipore (0.3 nicron) ;il:r ana t small battery operacad personal sanallag pump a: `lev rata of 1.0 :3 2.2 libera per nlnuce far time periods of If to ISO ainucet ac concentrations of 1 to 20 fibers per cubic cenciaecar. The optimum a amp ling time is reached whan the sample has 1 to 2 fibers per counting field. 7TI. TNUSUAL SAjZTT PRECADTTOHS A. (.'ear rubber glcrves and splash proof goggles while airing dimethyl phthalace and diethyl oxalate. 3. Keep reagents away from neat and open flame. They are flaatable. C. Avoid contact of reagents with the akin. (.'ash akin with soap and water if contact'occurs. SAhPLTS'C TTTg o The optimum sample time is determined from: a. Optimum fiber concentration of 2 to 10 fibers per cm^ or 1-2 fibers ft? field. b. Optimum flow rate of 1 to 2.2 liter per minute. Til. ?aOCSEPB A. niter installation and Semolina 1. Calibrate the portable pereooal vacuum pimp (Appendix A). 2. Separaea the filter cassette and inatall ona filter pad and 0.3 nicron filtar at the baae of the pump inlec side of eaasecte. 3. Aaeemble the caeeette and place a damp calluloea band around tha eaaaatta, insuring that tha two sections era joined without leakage. A. Allow the celluloce band to dry. 2. Connect a charged calibrated pump (change the pump battery for IS hours Ton "High" one day prior to use) to tha filter side of the cassette with tubing. S. Remove the top eection of the eaaaatta to expose the filter. 7. a. For area sampling, connect tha pimp and filtar to a ring icand or buggy. Position tha casaacte so chat the open end is facing down. b. For personal sampling, fasten the pump to Che worker'a belt and fasten the cassette to the lapel or shirt front (aa close to the -- face as practical). Position the eaasecte so that Che open and " la facing down. am -5 - ra:. ??.ocrsu?.g_ (ccjto.) A. 8. S^tart ths pump and record.' a. Start tin* ?? Plow rati c. The workers tana for personal sampling d. Area location a. Type of work being dona f. oilcar number g. Type of sample (asoescoa on air, etc.) 9. Check the pimp periodically during sampling for proper operation and fisw rate. 10. Stop the pimp at the end of the test period and record the stop tine. 11. Replace the caaaetta top and plug. 3. Saaple bounties 1. Clean all zouaclng equipment. 2. Apply a snail drop of nounclng solution, using a glass red, onto the canear of a clean microscope slide. 3. Spread the nounclng mania into a triangular shape, the size of vhion will coincide with the dimensions (.cue-eighth of the sample filter surface) of the filter wedge to be cut from the sample filter. 4. Separate the aiddle and bottom sections of the filter cassette to expose the sample filter. 5. Cut a triangular wedge from the sample filter center to the outer edge with e scelpel. (The else of Che wedge should be 1/8 of the filter surface.) 6. Creep the filter wedge, with tweezers, ec the outer edge portion and place the wedge, seapled side up, upon the mounting medium on the microscope slide. 7. Place e clean cover slip, using tweezers, on che simple filter wedge (once this contact hxe been made, do not reposition the caver slip). 8. The sample wedge will become transperent after If minutes. If cloudy, it may be necessary to prasa gently on the cover slip. 9. Reed the simple within one dey after mounelng. C. Semple Counting end Sizing 1. Calibrate the-microscope (Appendix 3 and C) 2. Place the microscope elide on the mechanical stags and poaitltn the center of the wedge under the 10 X objective lens, focus. DUP 0904091 i 1>ji>*- j'jKfflm - _ :. -6 - ?30C23CB (CONTD.) C- Sample Counting ted Siting .toned.; 3.__ Change co cr.e 4C--15 Z objective and focus. Achieve coaparabie results: T7I. Count randan fitlds from ona and ot the wedge and progress along __ a ranlcal lina co cha ochar and. -__b. __ -s^r Seiset the field of visw without looking through si microscope eyepiece to eliminate unconsciously saiaepiag "Heavy" or "lijhc" araas. Sire only fibers vied a length to width ratio greater than or equal to 3:1. --4. Counc onlv fibers greacar t.-.an 3 nitrometers in length. a. " When an agglcnerata (mass of naterlal) covers a significant portion of the field of view (approx. 1/6 or greater) reject the field and select anocaar (do aoc iaclude it ia the minaar of fields counted). ~f. Counc bundles of fibers as oaa fiber unless bath ends of a fiber -- crossing another can be clearly resolved. "g. 3a fibers that cross either ana or two sides of the counting field, -- the following procedure is used to obtain a representative count, "irst select: ------ ------ the left and bo toon sides and - The upper and lover left corners are used es decision elds. h. then count any fiber greeeer than S nicroaecers in length, but -- only if the fibers - lit enciraly within the counting aces or - Croeeee the left or bottom sides, or - Crosses the upper or lower left corners, or - Crosses both the top and boctoa sides. zl. Hej set and do not counc all othsr fibers. -- - Safer co Flguree 1-6 in Appendix 3. J. Count se aany fields as nacsssary to yiald a total of at least ICO fibers. Excapcion - Count at lease 10 fields even if you count nora than 100 fibers. ^ - Scop sc 100 fialds even if you have not reached ICC fibers. OUP 0904092 tzzz. ?aocm.~as cccstd.) 3 lank Sample k. Virh eech ctv batch (130 par package) of fliters, read 4 unused filters. 12. iALSCLATtOS Airborne aabescca fiber concentration is calculaced from :he formula: C - CS-3) (V) JZ) Vhere: C Airborne fiber concentration in fibers > 5per ca^ : Average fiber count in fibers> 5yn per field 3 Average fiber count of blank in fibers'^?] /um per field V - 855 sa* for 37mm diameter filter A Area of the counting field of a calibrated reticle in mm" per field ?S* total air volume collected through filter expressed in milliliters et standard conditions of temperature and pressure. Where:__ -__ V X ?___ X 298 760 I + 273 and 7 Volume of air sampled in milliters ? Barometric pressure in millimeters mercury ac sample time. T temperature of air sampled, 9C DUP 0904093 appstoix a CALISRATISS C~ ?0aSA3L2 7ACTTH PCX? r?.0C3TC3 A ?unp "snould be calibrated before each use. 1. Charge the puapa' Sectary far 16 hours on "high" prior co calibration. 2. Pour 200-l of soap solution in a 50 al beaker. 3. Vet Che 100 al bubble buracca inside with soap solution and leavevet. 4. Invert the 1C00 al burette and clasp co a ring stead. 5. Resave the plugs fees a prepared (has filter end pad installed) filter cassette, and attach the pump side of cha cassecta to a hose which is connected to the personal prap. 6. Attach The free end of the cassette to the tap of cha inverted burette, vlch cubing Capprox. 4 inches in length). Turn pump cn. 7. Raisa the beaker with ecap aoluclan to touch cha south of cha burette. A bubble should fora ac burette souch and rise coward the top. 3. Determine the clsa repaired for the bubble to rise from zero to one thoueend allllllcirs, using a stopwatch. 9. cor the desired 1.7 liters per sinuts air flow, the bubble will taka 2S.5 seconda to reach cha 1000 al mark. 10. Adjust cha puap sacting until the flow rata la exact. DUP 0904094 wamm A??grort 3 MIC?-CSC3Pg S57V? 1. The portog reticle is a round disc mada of glass and about the sane alae and thlciseea as a disa. Tha reticle haa a pnocegraphieally produced scales acd Is nduncad la the eyepiaea. 2. Koehler aachod of illumination requirements: a. An image of the Light source sust be la focus at the plana of the microscope condenser Iris. b. The Image of the field Iris auat be In focus at the plana of the specimen. c. the field iris opening is slightly greater than the alcraacopc's field of view. 3. Sec up procedure with Sausch and Lenta Synoptic Microscope and P&-Z7 illuminator. (The sana_principles that apply to this particular system will apply to any similar system.) a. The parton radicle must be aounced in eye piece. b. Clip the stage aicroaeter into the eechanlcal stage. c. Turn'on the illuminator to the high position. 4. Place the front of the filter holder seven inches from the mirror fork. 5. Close che field iria.__ 6. Center the band of illumination (che projected image of filament) acroas the mirror fork. 7. Cains the microscope's condenser focus 'snob, nova che condenser upward until it nearly touches che side. 3. Move che lens fully forward using che illuminators condanser focus knob. 9. Position yours so chac you can res the reflection of che bottom of che condenser la che mirror. 10. Close che condenser iris. 11. Sherply focus the image of che filament using either the illuminator condansar focua lamb or tha focus criming knob at the taar bass of the illuminator. 12. Opan che microscope condenser iris full. 13. Open the field iris half way. 11. Selaec che 10X objective. 13. Select the 40-4SX annaelars. DUP 0904095 appscix 3 costd 14 Find comes focus oy loosing cron she side of she nisrssespe while noving sis ooReceive so she coversli? unsil caey seariy souca. 17 leek shlough she eye pieces end widen she so;ecsive-cnverslip ciasaace wish she ccarse-cocua lenoo unsil see image of see aicroceser cones iaso scarp focus. Selees she -tO--C5X objeccive and sharply focus Che image. 19 Clsee she field iria fall-/. :o Ca che field of /lev Caere will be e brlghs spoc of lighs: a. Be aure you are in focus on sae ssage nicrcnecer. b. Focal she spec aaiag sae microscope sosdeaser knob. e. Vhlie looking shcougn c.-.e nieroscepe, open che field iris ansi! ic.;aas clears sae field of vsev. d. ifcar she illuainacion svscao la finished, chare is one nora caiag caas nusc be done oefsre you calibsace che microscope, chia is seactring che case of illasinasion visa cr.a aojeecize's pnese thifcing eleaenc. Here are che aecaaaary scape foe ccsrpiecisn. - lasers eisner she phase selescope (as in she case of Beuach and lac's) or" she Bertrand lens (as in sae case of laics Oialux) lass cat spcicsl syacan. This enables che SLicroacsplss so see bosh rings. Cne is brlghs and coses froa sae condenser, she ocher Is dark and is in che objactive. - hake she rings eoncancris using she ctncerlng knobs on che condenser. - Remove che selescope or 3ersrand lees. (The microscope is now properly see up for pheae-eonersse viewing end can be used for counsing and sizing.) DUP 0904056 cappstcdc CALisaATtcit of ?cf~ch amb pattzpocx oic3e iztzczi lacaiibracioa is required only when a specific objective - eye pixex reticle ccablnacion La changed. 1. Install Cha 1QX eya piece. 2. Put she ICt objective la place. 3. Plxct the stage al::aete: on the aeceaaical stage, Incus, and ceacer Che image 1, Changx ;c the 4C-45X objective and focus. 3. Adjust (linaup) the first seals division of the aicrcnacer to the Itf; boundary of cha reticle. 6. Ccunc ;h nuabar of divisions between toa left and right boundaries of Che long jsorironcal dimension of cha largest rtetaagia, estimating any percon of cha final division. CThis neaauremanc is 200 1,) 7. Decaralna 1 from tha aicrcmecer reading by dividing the saasuresent by 200. S. Calculate cha haighc of tha vertlcla dimension which is 100 L. 9. insert cha calcuiaced L valve into one formula D L (22)11 where ''a" is the circle number and "D" is cha diameter of the circles X 1 through 9. this is the reference to uaa when counting and aiziag fibers. 10. Calculaca cha area of tha counting fiald by multiplying 100 Z times 100 1 to give KM^. This raciela calibration is valid only for a specific objective - eyepiece reticle "combination. /jkj 4/21/77 DUP 090409 -----:.ira* ;:;;Bgfeas siijsi.T: :..:l...l;.s[j.m:Hgaf MH1M3itt-ia-tkiaraaai- f A?PEHDtX 3 VSrHS.'VtCSH Me-rfarnre Fi'.ttr Mj!- -r/ -/ 1/ i "" : ?>o o n' -- T/ iju.-e :. CCVNT. :;r crosHi both and bot ::m tides. . ^ - "Sk , * ~ '"N * ' --# ' J . V- t 'w ^7 ;::: '! . -. ; i i --- , ; --- j j r g 0`,, l1^; ?"e VF'.pire 3. CCVUT. fiber orotsee left / F ^ . | 1 .^ i<* :JL t -- ^ , \ :.'i ! ! igure 2 COUNT it an* fiber. Figure 4. COUNT, fiber croeee* bottom side* , a/-s ;ure 5. COUNT, fiber crosses lower left corner. 'j Figute 6. COUNT, fiber crottes upper !f: corner. DUP 0904096