Document p8nkYejQaQEnrVQ6bM5NoRdw

.sterufficc Alenioniiiiluiii Z (Mm* *no Location) _______ *Mr. M. R. StenzeT'- Dallas ~',M |NTI< ana Location) Mr. F. S. Ramey_____________ i July 14, 1980 I REFERENCE NO. I ESR-396-80 ANALYTICAL METHOD FOR ASBESTOS FOR FIELD USE Attached is an analytical method for screening unidentified insulation or other building materials for the presence of Asbestos (a small pea size sample must be pulverized). The method is suitable for use in the field and is simple and inexpensive. Presence of Iron (Fe+^) and/or magnesium (Mg+^) develops identifiable colors for a positive test. The absence of Fe and Mg in a test sample indicates the absence of asbestos. False positive results can be obtained due to other Fe+2 and Mg+^ containing material which is not asbestos since this simple test is not specific for asbestos. The method, recently developed by NIOSH, is Coloimetric. It was described in the June 1980 issue of National Safety News, page 20, as "an inexpensive and simple method for quickly determining whether asbestos is present in building materials. " Kits using the above analytical scheme are now marketed by Sipin and SKC with availability unknown. Home made kits are easily made for much less than the asking price of Sipin and SKC. Mr. Cody Milburn of Suntide Refinery (Corpus Christi) demonstrated his home made kit (cost about S50. 00 including fishing tackle box) at an informal meeting of local Safety and Health people which was sponsored by the local Vallen people. Mr. Cody has his laboratory technician using this test method in the field with an estimated analysis time of 30 minutes or less. I obtained a copy of the method from. Mr. Cody. Included in the method is a list of reagents required. If our people use this method, they should be properly informed of the hazard ous chemicals present and the safe handling of the more dangerous reagents such as 50% Hydrofluoric Acid, 10N Sodium Hydroxide, and concentrated Phosphoric and Sulforic Acids. If I can be of further help, let me know. ejv 000041 ESR-396-80 Page 2 SO r. R. F. Stubbeman (without attachment) r. P. J. Volpe r. Grover Vos - Dallas " 11 Mr. C. D. Barrett " " " July 14, 1980 Uniterms Asbestos Analysis Colorimetric Analysis Workplace Screen NIOSH Method 1980 563 000042 TEST FOR SCREENING ASBESTOS Sfz 5/P'a/ 7?t&5 O/v TbtE /)7'^-i. toc/h. Sv^j-rsoe (SSE^> .,<?- Momt ft& oe: kit' u/'/^c^ 7 U S f^O/Z. /a/ TJJ-& {=., ^_> c Walter S, Kim James W. Carter, II Richard E. Kupel U.S. DEPARTMENT OF HEALTH,' EDUCATION, AMD WELFARE'-' Public Health Service- Center for Disease Control ' National Institute for Occupational Safety and Health Division of Physical Sciences and Engineering Cincinnati, Ohio 45226 r% r.* *( ?jrni.tctv**j October 1979 n an. ljc; 0000*3 rrrirr ' r;* - *--y- TEST FOR SCREENING ASSESiOS I. SCOPE AND API'T.ICAT CON This colorimetric test is applicable to the detection of magnesium (II) and iron (II). from asbestos in bulk samples. These samples include sprayed on asbestos ns wall as ceiling tiles. The test is. simple and can be readily used in the field to screen for the presence or absence of asbestos. The amount of the sample needed for the test is only about the size of a large pea. II. PRINCIPLE The teslj is based upon the formation of ij^lor complexes with Mg+2 and Fe released from asbestos.- The Mg chrysotile is conplexo-i with p-nitrophenylazo-a-naphthol. The Fe from crocidolitc and amositc is complexed with 1, 10-phenanthroline.+2^ positive+cst is indicated by the formation of colored complex for Mg and/or Fe , and it indicates possible presence of asbestos-. III. INTERFERENCES T' he test is a colorimetric spot test +2 for Mg and +2 Fe , and is not specific for asbestos. A bulk sample may contain Mg and Fe compounds other than asbestos. Without treating the sample as in the Procedure, a few drops of color forming reagents are added directly-to the sample. If either color forms, an interferring substance is present and the sample must be cleaned before the test is conducted to eliminate the interference. In this cleaning process, plaster, mineral wool, fiberglass, and soluble Mg and Fe compounds are removed before the screening test, preventing their interference. ' IV. SENSITIVITY, PRECISION, AND ACCURACY . A sample containing more than 1% asbestos gives a positive color reaction. `. \ A total of 198 various field samples were tested before the Ac La ..aan steps were added to the Iron Test procedure. Results arc lieted be low: Results of the screening tent without the Acid Wash. No. of Samples 7. of Total True Positive 79 9 False Positive 50 AO 25 True Negative False Negative 69 ; . . 35 0 ; 0 000044 With the AcicI Wash, the following result:; were obtained from 13 samples. Results of the screening test with the Acid Wash. No. of Samples % of Total True Positive 5 38 False Positive 0 0 True Negative 8 . 62 False Negative 0 0 APPARATUS 1. Teflon dish or white plastic plate 2. Plastic or glass rod 3. Dropping plastic pipet A. 15 mL disposable plastic beaker 5. 25 run size 0.8 pm mixed cellulose ester filter 6. 25 irua size polyvinyl chloride filter 7. 25 cn Swinnex filter holder and gasket 8. 10 raL disposable plastic syringe REAGENTS (Reagent Grade) to f>Dl 1. Phosphoric acid, concentrated 2. 10 N sodium hydroxide - Dissolve 40 g of NaOH of water. 3. Mg Reagent - Dissolve 1 mg of p-nitrophenylazo-a-naphthol in 1QQ mL of 2 N NaOH. Age at least a day. This reagent is stable over a month. ... A, Hydrofluoric acid -- Dilute 20 mL of HE with 20 mL of water. Add 0.6 mL of concentrated HC1. 5. Fe Reagent -- Dissolve 2 g of 1,10-phenanthroline in 50 mL of ethanol. This reagent is stable over a month. 0. Glycerin, reagent grade. 7. Acetic acid, concentrated glacial. 8, Sulfuric acid, concentrated. 9. Double de-ionized water. 000045 VJ . . A, Magnesium Test 1. Add a few drops of Mg Reagent directly to the sample. If blue color appears, wash the sample with glycerin before the test. Any sample containing plaster is also washed with glycerin. Glycerin Wash a. Place a .small portion of sample, about the size of a large pea, in a plastic beaker. b. Add 5 drops of glycerin and mix well with a plastic rod or spatula. c. Rinse the plastic rod with a small amount of water into the beaker. d. Filter the sample through the filtration assembly consist ing of a syringe attached to the Swinncx filter holder loaded with a mixed cellulose ester filter' and a gasket. /* e. Filter with a minimum of 5 washings or about 50 mL of v/nter. * f. Transfer the filter to a Teflon dish for the Magnesium test. 2. Add a drop of H^PO^ and mix well by grinding the sample with a plastic rod. 3. Add 2 drops of 10 N NaOH and mix well. A. Add 5 drops of Mg Reagent and stir briefly. Mote any color change. 5. Add 5 more drops of Mg Reagent and observe the final color. 6. A blue color indicates that chrysotile may be present. 7. Samples giving a positive test may be sent to a laboratory for confirmation. If the magnesium test is negative, the samole must be tested for iron. E. Iron Test 1. Add few drops of Fc Reagent directly to the sample. If a red ' color appears, wash the cample v;ith the acetic--sulfuric acid mixture before the test.- Samples containing fiberglass ot mineral wooL are also washed with the acid mixture. 000046 Acid Wash 1. Pl.ace a small portion of the sample, about the size of a large pen* in a plastic beaker. 2. Add 5 drops of concentrated acetic acid. * 3. Add 5 drops of concentrated sulfuric acid. A. Mix well and ultrasonicate if available for 5 ninutes. 5, Filter Che sample through a polyvinyl chloride filter with a minimum of 5 washings or about 50 mL of water. 6, Transfer the filter to a Teflon dish t.id proceed with the Iron Test. 2. Add a drop of 11F solution and mix well. 3. Add 5 drops of Fe Reagent and observe the development of red color! ..." A, The red color indicates that amosite or crocidolite may be present, .. C. Notes If both pacts of the test give negative responses, there is a low probability that any asbestos is present. Once the presence of mag nesium and/or' iron is. indicated, further analysis, if needed, is done in the laboratory to confirm, identify the' type, and quantitate the percentage of asbestos. VIII. REFERENCE 1. Caution: Asbestos Dust. A scriptographic booklet by Channing L. Bate Co., Tnc., Greenfield, Mass. Prepared in cooperation with U.S. DHEN, PHS, COC, National Institute for Occupational Safety and Health, Cincinnati, Ohio (1973). 2. Pritz Feigl: Spot Tests - In Inorganic Analysis. Translated by Ralph E. Ocsper. 5th Edition. Elsevier Publishing Company, Amsterdam. (1958) p. 225-227. 3. Walter S. Kim, James Wr Carter, II, and Richard E. Kupel: Quid: Screening Test for Asbestos. U.P. DHEW, PHS, CDC, NtOSH, Cincinnati, Ohio. To be published in AIILAJ. TV.- Miy?? r'.-TT\'- E33T v --T'SJriircrvvxtyrm;r*r?.*'.:i. 000047 */vrrRr rv.''.Rv, r* - r t"': i *****