Document YjQRbMZ0qYYj0kZ38ogGxzX8k

INSTRUCTIONS FOR INSERTION OF "COSMETIC TALC" STANDARD INTO CTFA STANDARDS Attached are: 1. New CTFA Specification for "Cosmetic Talc" 2, Four new Methods (relating to "Cosmetic Talc") The new CTFA Specification for cosmetic grade talc replaces the Specification for "Talc" issued 5-30-71. In your Spe cifications binder, remove the Specification entitled "Talc" (1971 revision) and replace it with the attached Specifica tion entitled "Cosmetic Talc." So that your index will re main accurate, you should be sure to file this new Specifi cation under the "T1s" (rather than the "C's") where the old Specification fell. The four new Methods are additions to Methods already in your Methods binder. They are: E 32-1; J 4-1; J 5-1; and J 6-1. Remove nothing from your Methods binder. Simply insert the four new Methods in the appropriate sections of your Methods binder. Previously issued Methods and the Spectrum are still applicable. Do not remove them from your set of CTFA Standards. CTFA Adopted Name: TALC COSMETIC TALC TALC COSME Issued: 6 Revised: 3- 51-0i DEFINITION: Cosmetic Talc is an essentially white, odorless, fine powder, ground from naturally occurring rock It consists typically of 90% hydrated magnesium silicate, having the ideal formula Mg6[Si8O 20].(O with the remainder consisting of naturally associated minerals such as calcite, chlorite, dolomite, kaolin and rr nesite, and containing no detectable fibrous, asbestos minerals. TEST C o lo r ........................................................................ O d o r ............................................... Identification ................................. Slip ................................................. L u s tre ............................................. Water-Soluble I r o n ....................... Screen T e s t ................................... Water Soluble Substances .......... Acid Soluble Substances.............. Loss of Ignition ............................. Arsenic (as As) ............................. Lead (as Pb) ................................. Fibrous A m p h ib o le ....................... (Asbestiform Tremolite et al) Free Crystalline S ilica................... (Quartz) SPECIFICATION As specified by the buyer and showing no change after heating As specified by the buyer Positive: 1. Close match to CTFA Spectrum-- IR with no indication of foreign materials OR 2. (Alternate) Close match to X-ray Powder Diffraction File No. 19-770, published by ASTM, showing the most intense reflections at d values about 9.35,1.53 and 4.59 As specified by the buyer Do. Passes test 100% through 100 mesh 98% 'minimum through 200 mesh Finer grades: as specified by the buyer 0.1% maximum As specified by the buyer 6.0% maximum 5.0% maximum 3 ppm maximum 20 ppm maximum None detected As specified by the buyer * * it * + METHOD Heat 1 to 2 g at 200C for 5 minutes CTFA G 3-1 ASTM D 934-74 USP XIX, page 487 CTFA C 6-1 USP XIX, page 487 See test for " Reaction an Soluble Substances" CTFA E 32-1 USP XIX, page 487 CTFA F 1-1, Parts l-A an< CTFA F 2-1, Parts l-A an< CTFA J 4-1 CTFA J 5-1 (DTA) Alternate: CTFA J 6-1 (X-i C op yrigh t 1976 The Cosmetic, Toiletry and Fragrance Association, Inc. No portion o f the CTFA Standards, in whole o r in part, may be reprinted without permission from The Cosmetic, Toiletry and Fragrance Association, Inc. CTFA Me ACID SOLUBLE SUBSTANCES IN TALC Principle ' A sample of talc is mixed with diluted hydrochloric acid and the insoluble portion is removed by centrif filtration. The filtrate is sulfated, evaporated to dryness and ignited. The acid soluble matter is determine( cally as the sulfate. , Vr: 'r'; ' Apparatus - -; :V V t-ifj 1. Controlled temperature water bath 2. Beaker, Griffin, 100 ml ..."': ' V; ? ^ 3. Volumetric flask, 50 ml ^ 4. Centrifuge ' ; 5. Centriguge tubes (2), 50 ml - * 6. Graduated Cylinder, 50 ml 7. Sintered glass funnel, ultra fine porosity, 60 ml (0.9 to 1.4 /xm) Corning #36060-UF or equivalent 8. Vacuum flask, 125 ml ; 9. Pipette, 10 ml . ` ; C; . 10. Platinum or Vycor evaporating dish or equivalent . Reagents 1. Hydrochloric Acid, diluted, 10% v/v 2. Sulfuric Acid, diluted, 10% v/v Procedure , " ' ^ . >- : - .'C Weigh 2 g ( 0.001 g) of sample into a 100 ml beaker, add 40 ml diluted hydrochloric acid, and place in v 55 ( 2.5)C, with occasional stirring for 30 minutes. Immediately remove beaker from bath and pour CO' 50 ml centrifuge tube, rinsing beaker and stiring bar with 2 to 3 ml of distilled water. Centrifuge at 5000 minutes (Note 1). Filter supernatant through ultra fine porosity sintered glass funnel into vacuum flask, using 2 to 3 ml of disti rinse the centrifuge tube and funnel, and using care to avoid dislodging the packed talc at the bottom Filtrate must be clear (Note 1). Pour filtrate into 50 ml volumetric flask, rinsing with 3 to 5 ml distilled wat volume with distilled water. * Pipette 25 ml of adjusted filtrate into tared, ignited evaporating dish. Add 2 ml of diluted sulfuric acid and < dryness. Ignite at 800 ( 25C) for 1 hour. Cool and weigh. Calculation % Acid Soluble Substances = Weight of Residue in g x 200 Weight of Sample in g Note 1. Examine the centrifuged sample carefully to assure good clarity before proceeding with filtration. I detected, centrifuge the sample for an additional 15 to 30 minutes as necessary. * * * +* r n c y p T i r m n P T P V A \in ro A r.P A M rp a c c a h a t t o m tnlt ~ 11?? xt u; ASBESTIFORM AMPHiBOLE MINERALS M COSMETIC TAL< Part I: X-ray Diffraction Method Part li: Optical Microscopy and Dispersion-Staining Method lintroductiore - /-. ' '''--u The method which has been adopted for the detection of amphibole minerals in cosmetic talc is t accepted method of x-ray diffraction. Methods which appear in the literature for the detection of fibrou such as, transmission electron microscopy with selected area diffraction1 and electron microprobe been considered since they are capable of a lower level of detection than by x-ray diffraction. Howev< not been adopted since they suffer from the drawbacks, that the amount of material under examim small (less than a microgram) and the time for analysis, expertise required, and expense of equipme them as routine methods. ' V . v, * V ; v; The methodology presented is the most practical available, based on current technology. The use of " Electron Microscopy with Selected Area Electron Diffraction offers greater sensitivity, but is not prest is unsuitable for normal quality control application. ' . , \ Enrichment or concentration techniques using flotation cells have been tried as a means of improving level; however, all efforts so far have been unsuccessful. Pri nci pl e / t The x-ray diffraction method is based upon the principle that when a crystalline material is placet beam, a portion of the x-rays are diffracted by each set of atomic planes within the crystal. The d strike a scintillation counter as the sample is scanned through a prescribed angle with the resulting of peaks corresponding to each interplanar distance (d). A peak with d value in the range of 8.04 tc sample talc is strong evidence for the presence of amphibole in that talc. The level of detection of this method is 0.5% and above. The variability of-detection is caused by such factors as age and ms x-ray diffractometers, sample homogeneity, specific amphibole mineral present, morphology of amph size, preferred orientation, etc. For these reasons the level of detection should be reported for levels since below this level the data has been found to be not reproducible. If a statistically significant pei intensity equal to or greater than that obtained for the 0.5% standard in the d range for amphibole, des then the sample must be put through the following confirming scheme; X-ray Diffractometry (+ ) Optical Microscopy -- ( - ) -> Stop (Ampt (Acid Leach) i and ( - ) Dispersion-Staining Color Stop (Amphibole absent) Fibrous Morphology (+) ( - ) > Stop (Asbestiform Ampi Stop (Asbestiform Amphibole present) 7-A i.rT nv ixm TDArn Awn; ACcnriATTAM fNJr 11 H Fifteenth Street. N.W.. Washinet Should the presence of a small amphibole peak above the background " noise" be in question, it will be necessary to statistically evaluate the scan. A timer/scaler is required on the electronic panel of the x-ray diffractometer. In order for a peak to be Determine the region of the scan in question: in the Figure 1 scan, a peak appears to be present in tf 10.60 26 region. ,, :- of counts.;- f 7 : 4k ' Determine a background count by scanning a region equal to Vi of the 26 region covered by the peak, ir time used for the peak. Count each background region three times. Then average each region and a averages to obtain the background count (N). :/ , - V - V' " COSMETIC, TOILETRY AND FRAGRANCE ASSOCIATION. INC. 1133 Fifteenth Street. N.W.. Washineton. Standard Preparation Optimal instrument conditions must first be determined with the use of tremolite standards: 1.0%, 0.75%, 0.5% tremolite by weight, prepared in a standard talc / ; which is free of interfering peaks inthe 11.0to 1O,O20region. v / Weigh out appropriate amounts of standard talc and tremolite both of which have been ground to pass i sieve. Transfer to a Waring Blendor.* A d dII00 ml of ethanol to the blender and blend at low speed for 5 rr ethanol on a steam bath. , '? y / : . ^ Shake the sample in a plastic vial for 5 minutes on a-Spex Mixer/MilP to remove clumps and caked sam( from the evaporation of ethanol. .^ ^ ^^ ^ /; Determine by microscopy the homogeneity of the prepared standard previous to the x-ray diffraction i Press the homogeneous standard into a 1 ^ " pellet with a backing of boric acid. Transfer 2 ( 0.2) g of the die-holder and evenly distribute on a polished, scratch-free die. Distribute 4 ( 0.2) g of boric acid ei a pressure of 15,000 to 24,000 lb calculated on a 3" ram has been found to produce suitable pellets). T Registered Trademark ^ C M C T ir m n TTDV Awn n ? Ar.RANfF A W nrU T iO N XNC . 1133 Fifteenth Street. N W.. Washineto pellet 90 with respect to its original position In the goniometer and rescan between 11.0 and 10.O20 orientation may affect peak intensity. The presence of a reproducible peak (or peaks) is due to the j amphibole mineral (or minerals); the absence of peaks in this region indicates the absence of amph sample, within the limit of detection of this technique. Report results as "None detected" or as "Detected at approximately X% level," where "X" equals the lev COSMETIC, TOILETRY AND FRAGRANCE ASSOCIATION. INC. 1133 Fifteenth Street. N.W.. Washineton CTFA Weigh out 2 g of the talc into a 100 ml beaker. Add 25 ml of 10% v/v HCI slowly (to prevent excessive evo if carbonates are present) and heat, with occasional stirring on a steam bath for 30 minutes. Filter with vacuum filtration equipment, and wash several times with hot water. Dry the talc. Optical Microscopy and Dispersion-Staining Carefully disperse 0.1 mg of talc in one drop of Cargille HD liquid, = 1.605, and cover with a clean < Examine the sample in the dispersion-staining central stop mode. The substage diaphragm should be * position. . ; - - , \ ` . V * 5o-i ' \ w , \ v v ' -v' Tremolite, actinolite and presumably other amphibole minerals, under these condi tions, will show the following dispersion-staining colors: yellow changing to blue '; with rotation. The variation of the color change is due to the fact that the tremolite Examine the sample for asbestiform fibrous amphibole minerals. In order for an amphibole mineral to be considered asbestiform fibrous it must meet the foliowing OSH (R e fe re n c e 4). V. . 1. Particles must appear to be fibrous rather than as crystals or slivers. 2. The maximum diameter of a fiber to be counted in 3 microns.' ' 3. The maximum length of a fib e rto be counted is 30 microns. % 4. The length to width ratio must be 5 or more to 1, that is, 5 times or more longer than wii 5. The separate or individual fibers must contain fibrils or the " bundle of sticks" effect, unless 1 nondivisible stage. A fibril cannot be subdivided and would be counted, if it meets the other < length to width ratio of 5 or more to 1 is not meant to imply tnat other particles are not h rn c M P T ir tott f t o v a n h cb at.v am pp ACcnriATiriM rw r - m i C f.# m w u/--u:-- ^ .... . CTFAM /' FREE CRYSTALLINE SILICA (QUARTZ) IN TALC ' (DTA Method) Principle Differential thermal analysis (DTA) involves the measurement of thermal reactions which are induced as it is being heated at a constant rate. First-order thermal transitions are denoted as endothermic or depending upon whether the process is accompanied by the absorption or release of energy in the form sample holder includes a reference thermocouple and a differential thermocouple, which detect thermal i continuously monitoring any difference in temperature between the sample material and a thermally ine substance (calcined alumina) contained in another cavity or sample dish of the holder. V : The DTA method permits the unequivocal detection of quartz (free crystalline silica) in talc at a 0 .5 1 minimum detectable level. The method utilizes the thermal transition representing the reversible alpha to inversion of quartz at 573C. On heating, the latent heat of inversion gives rise to an endothermic reaction an exothermic transition is obtained. The talc is first calcined at approximately 800C for the purpose irreversible thermal transitions attributable to mineral impurities. The cooling curve then shows a flat bs improving detectability for quartz. Studies have shown that the intensity of this thermal peak is affected size distribution of the quartz. Therefore, DTA is not recommended for the quantitative determination of c Apparatus . ** 1. Differential Thermal Analyzer, including either a high temperature powder sample holder of nickel s. steel construction with exposed-loop differential thermocouple (such as Platinel II) or sample holde a ring type differential thermocouple with platinum dishes, with equipment to heat to at least 800C 2. Spex Mixer/Mill, or equivalent mechanical mixer with plastic vial and plastic ball y 3. Sieve, 325-mesh 4. Mortar and pestle, or grinding mill Reagents . .. ; f.y.' 1. Standard talc sample, containing no detectable quartz 2. Standard quartz sample, at least 95% pure ? ~ : "l* Procedure Standard Preparation -" Grind standard talc and quartz samples to pass a 325-mesh sieve. This will give a particle size distrib 44>xm. --\- Weigh appropriate amounts of the ground standard talc and quartz into a plastic vial to prepare 1.0% w/v standard. Mix with a plastic ball approximately 10 minutes in Spex Mixer/Mill. f'rtQKs^'TTtr m u c t d v a Mn c?d a r.D a wrr ACCnriATinw rwr - i m c w * wiv -- CTF ;' ^f-. '>i ' ' " - '* .V' ; V . ': ' v; .*> COSMETIC TOT1.FTRV AWr> CD ar o w n r i ri<rtot i CTFAW % ' Principle FREE CRYSTALLINE SILICA (Quartz) IN TALC (X-ray Diffraction Method) y . ' v: vi *.. `.r' ' .J":'.? silica (quartz), in talc. It is necessary that at least the three strongest diffraction lines of quartz be presen pattern to confirm the presence of quartz in the talc: 3.34xl 4.264, 1.822dA. .> ; <, V,-./ - ;r. * l the same talc. Using this pressed pellet technique, it is possible to detect the three strongest quartz minimum level of 2% w/w. ^ M ,j' . ; ' - Apparatus . >- *; ?r-V. , ~ U u .. - - ". ; ' V- v '"V- y y . . ; : 1/>-f <*"V ' ^ _4.,^ ` , *. -r/-' - . . . . \y y : Vy 1. X-ray diffractometer with nickel-filtered CuKa radiation and a suitable 1VS circular sample h< pelletized sample y > '; y .^ a . Ay y : i:',- \ > . . 4' %' 3, VMVpellet press *l 'ft' ,-y - Reagents 1. Boric acid Procedure " ;; . '* .^ : y ' , 4 ' ,Jt 'i :. A1vv --'-C/v ` V- v \ *' Sample Preparation ; : ' .y `; - /. . . . . y- Transfer approximately 2 g of sample talc to the die-holder and distribute evenly on a polished, scratch fi distribute approximately 4 g of boric acid on top of the talc layer. Compress the two layers into a pellet wh< is free of flaws (Note 1). ,, ||p v v ' ' . . '.-44?., ; y -A" - . 'A y ' / t f: ' ' , l . : yy rn C M P T ir TATI ictdv A\m t n A m Axirr AroArTimrAM < ^ ** A CTFA Method J 4-1 Issued: 10-7-76 Page 1 ASBESTIFORM AMPHIBOLE MINERALS IN COSMETIC TALC Part I: X-ray Diffraction Method Part li: Optical Microscopy and Dispersion-Staining Method Introduction The method which has been adopted for the detection of amphibole minerals in cosmetic talc is the generally accepted method of x-ray diffraction. Methods which appear in the literature for the detection of fibrous amphibole, such as, transmission electron microscopy with selected area diffraction1 and electron microprobe,2 have also been considered since they are capable of a lower ievel of detection than by x-ray diffraction. However, they have not been adopted since they suffer from the drawbacks, that the amount of material under examination is quite small (less than a microgram) and the time for analysis, expertise required, and expense of equipment eliminates them as routine methods. The methodology presented is the most practical available, based on current technology. The use of Transmission Electron Microscopy with Selected Area Electron Diffraction offers greater sensitivity, but is not presented since it is unsuitable for normal quality control application. Enrichment or concentration techniques using flotation cells have been tried as a means of improving the detection level; however, all efforts so far have been unsuccessful. Principle The x-ray diffraction method is based upon the principle that when a crystalline material Is placed in an x-ray beam, a portion of the x-rays are diffracted by each set of atomic planes within the crystal. The diffracted rays strike a scintillation counter as the sample is scanned through a prescribed angle with the resulting development of peaks corresponding to each interplanar distance (d). A peak with d value in the range of 8.04 to 8.85A0 for a sample talc is strong evidence for the presence of amphibole in that talc. The level of detection of amphibole by this method is 0.5% and above. The variability of-detection is caused by such factors as age and manufacturer of x-ray diffractometers, sample homogeneity, specific amphibole minera! present, morphology of amphibole, particle size, preferred orientation, etc. For these reasons the level of detection should be reported for levels above 0.5%, since below this level the data has been found to be not reproducible. If a statistically significant peak is found of intensity equal to or greater than that obtained for the 0.5% standard in the d range for amphibole, described above, then the sample must be put through the following confirming scheme: X-ray Diffractometry (-) (+ ----- ^ Optica! Microscopy -- (Acid Leach) and Dispersion-Staining Color (-) Stop (Amphibole absent) Stop (Amphibole absent) ^ ( +) Fibrous Morphology (+) ( - ) ^ Stop (Asbestiform Amphibole absent) Stop (Asbestiform Amphibole present) COSMETIC, TOILETRY AND FRAGRANCE ASSOCIATION, INC. 1133 Fifteenth Street, N.W., Washington, D.C. 20005 CTFA Method J 4-1 Issued: 10-7-76 Page 2 Part I: Amphibole Minerals by X-ray Diffractometry Apparatus 1. X-ray diffractometer, employing nickel-filtered copper .K-alpha radiation, horizontal or vertical goniometer with variable scan speed capability, suitable talc pellet sample holder, variable speed recorder, electronic panel including ratemeter and variable attenuation and time constant settings 2. Hydraulic press, capable of attaining a pressure of 15,000 to 24,000 lb calculated on a 3" ram 3. Mortar and pestle or grinding mill (Note 1) 4. Waring Blendor,* or equivalent blender 5. Spex Mixer/Mill,* or equivalent mechanical mixer 6. Sieve, 325-mesh 7. Optical microscope (Note 2) 8. 11/4" pellet press Reagents 1. Standard talc sample, containing no detectable amphibole minerals 2. Standard tremolite sample, at least 80% pure Sample of tremolite standard may be obtained by ordering from The Cosmetic Toiletry and Fragrance Associa tion, Inc., 1133 Fifteenth Street, N.W., Washington, D.C. 20005. 3. Denatured ethanol 4. Boric acid Procedure The procedure consists of slow-scanning, under previously determined conditions, a compressed pellet of the sample talc in the 11.0 to 10.O20 (8.85 to 8.04) region for the presence of an amphibole peak. There are times when it is difficult to discrimi nate a possible peak for amphibole over the background noise level. ' Registered Trademark COSMETIC, TOILETRY AND FRAGRANCE ASSOCIATION, INC. 1133 Fifteenth Street, N.W., Washington, D.C. 20005 CTFA Method J 4-1 Issued: 10-7-76 Page 3 Should the presence of a small amphibole peak above the background "noise" be in question, it will be necessary to statistically evaluate the scan. A timer/scaler is required on the electronic panel of the x-ray diffractometer. In order for a peak to be statistically significant, the peak intensity must equal or exceed three standard deviations (3cr) above the average background intensity (N): Where: N + 3cr = minimum peak intensity N = average background count cr = V N Figure 1. Determine the region of the scan in question: in the Figure 1 scan, a peak appears to be present in the 10.40 to 10.60 26 region. Slow scan with cumulative pulse counting through the peak region three separate times and average the number of counts. Determine a background count by scanning a region equal to Vz of the 26 region covered by.the peak, immediately before and after the peak. The counting time for each of these background regions will equal Vz the total counting time used for the peak. Count each background region three times. Then average each region and add the two averages to obtain the background count (N). COSMETIC, TOILETRY AND FRAGRANCE ASSOCIATION, INC. 1133 Fifteenth Street, N.W., Washington, D.C. 20005 Example: In Figure 1. Peak ......................... .......... Background Region A ............. .......... Region B ............. .......... Region (2 6) 10.40 to 10.60 10.30 to 10.40 10.60 to 10.70 Time (sec.) 120 - 60 60 Peak 10.40 to 10.60 2 6 time secs. counts 120 120 120 Average 60,332 59,870 60,105 60,102 Background Region A Region B 10.30 to 10.40 2 6 10.60 to 10.70 2 6 time secs, counts time secs, counts 60 28,784 60 28,943 60 28,634 28,787 60 28,506 60 28,368 60 28,204 28,359 CTFA Method J 4-1 Issued: 10-7-76 Page 4 N = 28,787 + 28,359 = 57,146 a = V57.146 = 239 3cr = 717 N + 3cr = 57,146 + 717 = 57,863 The actual number of counts obtained for the integrated peak intensity was 60,102; therefore, the " suspect" peak is statistically present in the scan. COSMETIC, TOILETRY AND FRAGRANCE ASSOCIATION, INC. 1133 Fifteenth Street, N.W., Washington, D.C. 20005 CTFA Method J 4-1 issued: 10-7-76 Page 5 Standard Preparation Optimal instrument conditions must first be determined with the use of tremolite standards: 1.0%, 0.75%, 0.5% tremolite by weight, prepared in a standard talc which is free of interfering peaks in the 11.0 to 10.O20 region. Weigh out appropriate amounts of standard talc and tremolite both of which have been ground to pass a 325-mesh sieve. Transfer to a Waring Blendor.* Add 100 ml of ethanol to the blender and blend at low speed for 5 minutes. Carefully transfer the contents of the blender, with repeated ethanol washings, into a large beaker. Evaporate the ethanol on a steam bath. Shake the sample in a plastic vial for 5 minutes on a Spex Mixer/MilP to remove clumps and caked sample resulting from the evaporation of ethanol. Determine by microscopy the homogeneity of the prepared standard previous to the x-ray diffraction analysis. Press the homogeneous standard into a VA" pellet with a backing of boric acid. Transfer 2 (0.2) g of standard to the die-holder and evenly distribute on a polished, scratch-free die. Distribute 4 (0.2) g of boric acid evenly on the talc layer. Press the mixture into a pellet under conditions suitable for obtaining a smooth planar surface (for example, a pressure of 15,000 to 24,000 lb calculated on a 3" ram has been found to produce suitable pellets). The resulting pellet must have a talc face which is free of flaws; if not, the pellet must be discarded (Note 3). Prepare two acceptable pellets from each standard. 'Registered Trademark COSMETIC, TOILETRY AND FRAGRANCE ASSOCIATION, INC. 1133 Fifteenth Street, N.W., Washington, D.C. 20005 CTFA Method J 4-1 Issued: 10-7-76 Page 6 Sample Preparation Prepare two pellets from each sample in the manner described for the standard pellets. Make a qualitative scan from 4 to 50 26 on one of these pellets to ascertain the presence of amphibole above the 2% level or the presence of mineral impurities having interfering peaks in the 11.0 to 10.0 20 (8.85 to 8.04A) region of the scan. The presence of such interference will eliminate use of the x-ray diffraction method for the sample, and one will have to proceed directly to the microscopical procedure. Instrumentation Instrumental variables are optimized on the 1% standard. Lower standards are then analyzed under the optimum conditions to determine the lower level of detection. Of major importance in obtaining maximum instrument sensitivity are a slow dif fractometer speed combined with compatible recorder speed, and high attenua tion combined with a statistically acceptable time constant on the ratemeter. Under appropriate instrumental conditions the peak obtained for the 0.5% standard should be detectable above background noise as shown in Figure 2. Typical instrumental conditions employed for the Siemens Diffractometer (Mode! No. M386-X-A4), and Counter and Recorder Unit (Type T) are: Radiation: Divergence slit: Goniometer speed: Recorder speed: Attenuation: Time constant: Cu with Kbfilter at 40KV and 24 ma 1 Receiving slit: 0.2 mm 1/io20/minute 300 mm/hour 1 x 103 impulses/second T (s) = 4 Statistical error of 1.1 % under these conditions Rise Time = 0.18 Attenuator = 20 COSMETIC, TOILETRY AND FRAGRANCE ASSOCIATION, INC. . 1133 Fifteenth Street, N.W.. Washington, D.C. 20005 100-- 0.5% Tremolite soso-- 70- 60- 60-- 2 C 40-- 30-- 20-- 10- 0-- I i i i i iifii .6 10.0 10.2 10.4 10.6 10.8 11.0 11.4 *26 Figure 2 CTFA Method J 4-1 Issued: 10-7-76 Page 7 X-Ray Diffraction Scans Place the standard or sample pellet in a suitable holder and slowly scan between 11.0 and 1O.O20. Then rotate the pellet 90 with respect to its original position in the goniometer and rescan between 11.0 and 1O.O20 since pellet orientation may affect peak intensity. The presence of a reproducible peak (or peaks) is due to the presence of amphibole mineral (or minerals); the absence of peaks in this region indicates the absence of amphibole in the sample, within the limit of detection of this technique. Report results as " None detected" or as " Detected at approximately X% level," where "X" equals the level detected. COSMETIC, TOILETRY AND FRAGRANCE ASSOCIATION, INC. 1133 Fifteenth Street, N.W., Washington, D.C. 20005 CTFA Method J 4-1 Issued: 10-7-76 Page 8 ' Part II: Asbestiform Amphibole Minerals by Optical Microscopy and Dispersion-Stainirtg Apparatus 1. Polarizing microscope. Best results will be obtained if the instrument includes the following: a. Individually centering objectives b. Bertrand lens c. High-intensity light source d. Centering condenser/substage 2. Dispersion-staining device (Note 4) 3. Vacuum filtration equipment, including either a porcelain cone with glass fiber filter mat or a porous glass bottom cup Reagents 1. Hydrochloric acid, 10% v/v 2. Cargille immersion liquid Series HD, n f = 1.605 (Note 5) Procedure Acid Treatment Because of the interference caused by some carbonates (e.g. calcite) in the detec tion of asbestiform amphiboles in talc by optical microscopy/dispersion-staining, it is necessary to first remove these carbonates by a simple acid leaching procedure: // COSMETIC, TOILETRY AND FRAGRANCE ASSOCIATION, INC. 1133 Fifteenth Street, N.W., Washington, D.C. 20005 CTFA Method J 4-1 Issued: 10-7-76 Page 9 Weigh out 2 g of the talc into a 100 ml beaker. Add 25 ml of 10% v/v HCI slowly (to prevent excessive evolution of gas if carbonates are present) and heat, with occasional stirring on a steam bath for 30 minutes. Filter with vacuum filtration equipment, and wash several times with hot water. Dry the talc. Optical Microscopy and Dispersion-Staining Carefully disperse 0.1 mg of talc in one drop of Cargille HD liquid, n^5 = 1.605, and cover with a clean cover slip. Examine the sample in the dispersion-staining central stop mode. The substage diaphragm should be almost com pletely closed, the field diaphragm may be partially closed to enhance color contrast, and the polarizer should be in position. Tremolite, actinolite and presumably other amphibole minerals, under these condi tions, will show the following dispersion-staining colors: yellow changing to blue with rotation of the sample relative to the polarizer or yellow changing to orange with rotation. The variation of the color change is due to the fact that the tremolite may lie in one of two positions relative to its principal optical orientation. Examine the sample for asbestiform fibrous amphibole minerals. In order for an amphibole mineral to be considered asbestiform fibrous it must meet the following OSHA definition (Reference 4). 1. Particles must appear to be fibrous rather than as crystals or slivers. 2. The maximum diameter of a fiber to be counted in 3 microns. 3. The maximum length of a fiber to be counted is 30 microns. 4. The length to width ratio must be 5 or more to 1, that is, 5 times or more longer than wide. 5. The separate or individual fibers must contain fibrils or the " bundle of sticks" effect, unless they are at a nondivisible stage. A fibril cannot be subdivided and would be counted, if it meets the other criteria. The length to width ratio of 5 or more to 1 is not meant to imply that other particles are not hazardous. COSMETIC, TOILETRY AND FRAGRANCE ASSOCIATION, INC 1133 Fifteenth Street, N.W., Washington, D.C. 20005 CTFA Method J 4-1 Issued: 10-7-76 Page 10 Report results as " Asbestiform Amphibole Present" or as ``Asbestiform Amphibole Absent." It is imperative that both dispersion-staining color and fibrous morphology criteria be satisfied before identifying a particle as asbestiform amphibole, since other sub stances may show colors similar to those described. Notes 1. Talcs to be analyzed and the tremolite used to prepare standard samples must be finer than 325 mesh (maxi mum particle size of 44 microns). The Tekmar Analytical Mill (Model A-10) is recommended. It is available from: Tekmar Company P.O. Box 37202 Cincinnati, Ohio 45222 2. It is important that the homogeneity of the prepared talc-tremolite standard samples be verified by optical microscopy. 3. This requirement is critical since excessive surface scatter will cause abnormally high background counts. 4. The only commercially available dispersion-staining device is sold by: Walter C. McCrone Associates, Inc. 2820 South Michigan Avenue Chicago, Illinois 60616 5. Available from: -- or from laboratory suppliers. R. P. Cargille Laboratories, Inc. Cedar Grove, New Jersey 07009 References 1. Rohl, A. N., Langer, A. M., Environmental Health Perspectives 9, 95 (1974) 2. Rubin, I. B., Maggiore, C. J., Environmental Health Perspectives 9,81 (1974) 3. L. S. Birks, X-Ray Spectrochemical Analysis, pages 54-55, Interscience Publishers (1959) 4. "Tremolite and Talc." U.S. Department of Labor, Occupational Safety and Health Administration, Field Informa tion Memorandum #74-92, November 21,1974. COSMETIC, TOILETRY AND FRAGRANCE ASSOCIATION, INC. 1133 Fifteenth Street, N.W., Washington, D.C. 20005