Page:NIOSH Manual of Analytical Methods - 5046.pdf/5

 TETRAKIS(HYDROXYMETHYL)PHOSPHONIUM CHLORIDE: METHOD 5046, Issue 1, dated 15 March 2003 - Page 5 of 5

The possibility of migration of formaldehyde from the front filter to the backup filter during storage at 5 oC in sealed three-piece cassettes was investigated. Front filters in six three-p iece cas settes we re fortified with 31.4-µg quantities of THPC, and the cassettes were sealed. The six cassettes were stored for 10 days at 5 o C in the dark and then front and backup filters were analyzed. Average recoveries of THPC from front and backup filters we re 10 2% a nd 11 %, respectively (RSDs were 5.7% and 23%, respectively). The average total recovery of THPC from front and backup filters was 113% (RSD = 5.0%). These data provide evidence that (a) formaldehyde from TH PC can indeed migrate from one DNPH-coated filter to another and (b) one needs to analyze both the front and backup DNPH-coated filters for THPC in case there is migration. Yields of formaldehyde from TH PC were determined in order to study the stoichiometry of the breakdown of THPC. DNPH-coated glass fiber filters in 4-mL vials were fortified with known quantities of THPC at four levels (n = 23 samples). The sam ples were treated with acetonitrile and heat by the usual procedure and analyzed with liquid standards (standard solutions of form aldehyde-DNPH in acetonitrile). Theoretical quantities of formaldehyde were calculated on the basis that one mole of THPC releases one mole of formaldehyde in the presence of DNPH and heat. The average of the four average yields of formaldehyde was 100 .3%. The upper limit for collection of THPC on a filter is calculated at 1 mg. Since at 100% yield one mole of THPC releases one m ole of formaldehyde in the presence of DNPH and heat, 1 mg of THPC would release 158 µg of form aldehyde, a quantity w hich theoretica lly would react with 1.04 mg of DNPH. One DNPH -coated filter contains 2 mg of DNPH, a quantity which allows for the presence of excess DNPH when 1 m g of THPC is collected.

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Tucker SP, Striley CA [2002]. Te trakis(hydroxym ethyl)ph osp hon ium Chloride B ack up D ata Report for Method 5046. National Institute for Occupational Safety and Health, DART, Cincinnati, OH. Unpublished report for evaluation of method. NIOSH [1994]. Formaldehyde by HPLC, m ethod 2016, issue 2, NIOSH M anual of Analytical Methods, 4 th ed., Eller P M and C assinelli ME (eds.), U.S. Department of Health an d Hum an S ervices, P ublic H ealth Service, Centers for Disease Control and Prevention, National Institute for Occupational Safety and Health, Cincinnati, OH. DHHS (NIOSH) Publication No. 94-113. Kleindienst TE, Corse EW, and Blanchard FT [1998]. Evaluation of the Performance of DNP H-Coated Silica Gel and C 18 Cartridges in the Measurement of Formaldehyde in the Presence and Absence of Ozone. Environmental Science & Technology, 32(1), 124-130. W orld Health Organization [2000]. Environmental Health Criteria 218, International Programm e on Chemical S a f e t y, In t e rn a t io n a l Labour Orga nization, Geneva, http ://www .inc hem .org/d ocum ents/ehc/e hc/eh c218.htm l. Elizey SE Jr. and Connick W J Jr. [1973]. G asom etric Analysis of TH PC., Am erican Dyestuff Rep orter, 62 (6), pp. 47 and 50. Loewe ngart G and Van Duuren BL [1 977 ]. Evaluatio n of Chem ical Flam e R eta rdants for Ca rcinogenic Potential, Jo urna l of Toxicology and E nviron m enta l Hea lth, 2, 539-546. Otson R and F ellin P [19 88]. A Review o f Te chn iques for Me asu rem ent of Airbo rne A ldehydes. Science of the To tal Environm ent, 77 (2/3), 95-131. Aldrich Chem ical Co. [2000]. Potentiometric titration of tetrakis(hydroxymethyl)phosphonium chloride with silver nitrate and silver electrod e, pro duc t 40,486-1, Lot 10 715 B1, Techn ical Se rvice Departm ent, Aldrich Chem ical Co., Milwaukee, W I (August 18, 2000). Unpublis hed procedure by Fluka in Backup Da ta Repo rt [1].

METHOD DEVELOPED BY: Samuel P. Tucker, Ph.D., NIOSH/DART

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition