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Formaldehyde Analysis

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1 Formaldehyde Analysis
Industrial Hygiene Formaldehyde Analysis Adapted from Morawska, L. and Salthammer, T. (eds.) (2004) Indoor Environment. Wiley-VCH. Copyright © by DBS

2 Contents Colorimetric Analysis Acetylacetone Method NIOSH 3500

3 Sampling Complaint area, non-complaint area and outside
Vapor phase extraction followed by analysis

4 Measurement Methods Colorimetric
Acetylacetone colorimetric method (Nash, 1953) NIOSH 3500 Pararosaniline Method HPLC GC See Schultz, M. and Salthammer, T (1999) for discussion of methods

5 Measurement Acetylacetone Colorimetric Method
Acetylacetone colorimetric method (Nash, 1953) Hantzsch reagent (acetylacetone) 2M ammonium acetate, 0.05 M acetic acid, 0.02 M acetylacetone See Shimadzu paper No. A262 for method

6 Measurement Acetylacetone Colorimetric Method
Stock HCHO solution = 37.7 % (m/m), ρ = g/mL Require HCHO std. (1000 ppm), how much of the 37.7 % solution should be taken to make a 100 mL solution of 1000 ppm HCHO? Dilutions of 1000 ppm to make a 1,2, and 5 standard? 1:100 to make a 10 ppm std., then 1:10, 2:10 and 1:2

7 Measurement Acetylacetone Colorimetric Method
Measure out 2x 25 mL of absorption liquid (DI water) into 2 impingers (sample and equipment blank) Pass air through one of the impingers at 1 L/min for 40 minutes Perform the following to: a 5 mL reagent blank, a 5 mL 1000 ppm Std., 5 mL of the air sample and the sample blank Add 5 mL acetlyacetone reagent and 5 mL DI water Heat for 30 mins at 40 °C Leave for color developemnt (30 mins) Dilute the standard to 1, 2, and 5 ppm Read standards and sample tubes at 412 nm, slit width 2.0 nm

8 Measurement Acetylacetone Colorimetric Method
Shimadzu Paper No. A262

9 Measurement Acetylacetone Colorimetric Method

10 Measurement NIOSH 3500: Chromotropic Acid Method
UV-Vis NIOSH 3500 method uses chromotropic acid Detection limit: 0.5 µg per sample

11 Measurement HPLC HPLC

12 Health Effects Acute Exposure
NYT April 17, 1987: Formaldehyde Found a Cancer hazard Hess-Kosa, 2002

13 Summary Used in a wide variety of processes and products
Carcinogenic, irritant poses safety hazard Max permissible exposure 2.0 – 0.1 mg/m3 very close to demonstrated rodent carcinogenic dose of 5.6 mg/m3 and NOEL of 2 mg/m3

14 Books Hess-Kosa, K. (2002) Indoor Air Quality. Lewis Publishers.
Leslie, G.B. and Lunau, F.W. (1992) Indoor Air Pollution: Problems and Priorities. Cambridge University Press. Turco, R.P. (2002) Earth Under Seige: From Air Pollution to Global Change. Oxford University Press, London. Turoski, V. (ed.) (1985) Formaldehyde: Analytical Chemistry and Toxicology (Advances in Chemistry Series). ACS, Washington DC.

15 References Beasley, R.K., Hoffman, C.E., Rueppel, M.L., and Worley, J.W. (1980) Sampling of Formaldehyde in Air with Coated Solid Sorbent and Determination by High Performance Liquid Chromatography. Analytical Chemistry, Vol. 52, pp Fregert, S., Dahlquist, I., and Gruvberger, B. (1984) A simple method for the detection of formaldehyde. Contact Dermititis, Vol. 10, No. 3, pp Gammage, R.B. and Gupta, K.C., “Formaldehyde”, in: Walsh, P.J., Dudney, C.S., and Copenhaver, E.D., eds. (1984) Indoor Air Quality. CRC Press, Boca Raton, Florida. Gasparini, F., Weinert, P.L., Lima, L.S., Pezza, L., and Pezza, H.R. (2008) A simple and green analytical method for the determination of formaldehyde. Journal of the Brazillian Chemical Society, Vol. 19, No. 8, pp Kleindienst, T.E. et al (1988) An intercomparison of formaldehyde measurement techniques at ambient concentration. Atmospheric Environment, Vo. 22, No. 9, pp Larson, A., Jentoft, N.A., and Greibrokk, T. (1992) Determination of ppb levels of formaldehyde in air. Science of the Total Environment, Vol. 120, No. 3, pp Lowe, D.C., Schmidt, U., Ehhalt, D.H., Frishkorn, C.G.B., and Nürnberg, H.W. (1981) Determination of formaldehyde in clean air. Environmental Science and Technology, Vol. 15, No. 7, pp Luks, E., Kiss, E. (1992) Formaldehyde determination by the colorimetric method with acetylacetone. Part I. Formaldehyde determination in certain cosmetic products. Roczniki Panstwowego Zakladu Higieny, Vol. 43, No., 3-4, pp Matthews, T.G., Hawthorne, A.R., Howell, T.C. et al (1982) Evaluation of selected monitoring methods for formaldehyde in domestic environments. Environment International. Vol. 8, No. 1-6, p Matthews, T.G. and Howell, T.C. (1981) Visual colorimetric formaldehyde screening analysis for indoor air. Journal of the Air Pollution Control Association, Vol. 31, No. 11, pp

16 References Miksch, R.R., Anthon, D.W., Fanning, L.Z., Hollowell, C.D., Revzan, K., and Glanville, J. (1981) Modified Pararosaniline Method for the Determination of Formaldehyde in Air. Analytical Chemistry, Vol. 53, pp Monsen, R.M. and Stock, T.H. (1986) A comparison of formaldehyde monitoring methods for the residential environment. Journal of Environmental Health, Vol. 49, No. 2, pp Murai, K., Okano, M., Kuramitz, H., Hata, N., Kawakami, T., and Taguchi, S. (2008) Investigation of formaldehyde pollution of tap water and rain water using a novel visual colorimetry. Water Science and Technology, Vol. 58, No. 5, pp Nash, T. (1952) Colorimetric Determination of Formaldehyde under Mild Conditions. Nature, Vol. 170, No. 4336, pp. 976. Nash, T. (1953) The Colorimetric Estimation of Formaldehyde by Means of the Hantzsch Reaction. Biochemistry, Vol. 55, p Peatreas, M., Twist, S., Pon, D., and Miles, I. (1984) Evaluation of Two Methods for Measuring Formaldehyde at ppb Levels. Proceedings, Annual Meeting – Air Pollution Control Association, Vol. 6, 10p. Trebig, G., Schaller, K.-H., Beyer, B., Muller, J., and Valentin, H. (1989) Formaldehyde exposure at various workplaces. Science of the Total Environment, Vol. 79, No. 2, pp West, P.W. and Sen, B. (1956) Spectrophotometric determination of traces of formaldehyde. Fresenius’ Zeitschrift fur Analytische Chemie, Vol. 153, No. 3, pp

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