Page:NIOSH Manual of Analytical Methods - 3800.pdf/5

 ORGANIC AND INORGANIC GASES by FTIR Spectrometry: METHOD 3800, Issue 1, dated 15 March 2003 - Page 5 of 47

S S S

Development of more accurate analyte or interferant reference spectra. Inclusion of reference spectra for additional compounds in the mathem atical analysis. Exclusion from the m athem atical analysis of analyte and/or interferant com pounds which are clearly absent in the samples. S De-resolution or w avenum ber ad jus tm ent of the reference spectral library to match that of the sam ple spectra (or vice versa). S Revision of the origina l data qua lity objectives (tho se inc luded in the test plan) to levels supported by the test data. NOTE: After performing any such corrective actions, the analyst must repeat Steps 13 through 16 and re-evaluate the LOD value for each analyte compound.

REPORTING: 18. Reporting requirements include the analyte and interferant concentrations, the concentration uncertainties, the FTIR spectrometer configuration, the sampling locations and conditions, the source(s) of the reference spectra, the CTS spectral analysis results, the results of QA/QC procedures, and certificates of analysis for all standard ga ses. Any va riations of the test procedu res and origina l data qua lity objectives from those included in the test plan should also be documented and reported. (Several of the term s us ed h ere a re de fined in Appen dix A and described in the following Ap pen dices. In particular, see T able D1 for a d esc ription of the F TIR spe ctrom eter c onfiguration pa ram eters .)

EVALUATION OF METHOD: Fie ld evaluations of extractive FTIR methods have been performed for many compounds (see, for example, Referen ces 7 an d 8) accord ing to EPA M ethod 301 (R eference 9).

REFERENCES: [1] U.S. EPA (proposed); Method 320 - Measurement of vapor phase organic and inorganic emissions by extractive FTIR spectroscopy; Federal Register V63 No.56, pp.14219-14228 (March 24 1998); also available (on Ma y 19 19 99) a t http://ww w.ep a.go v/ttn/oarpg/t3 /fr_notices /, file frprop .pdf. [2] U.S. EPA (propo sed ); Addendum to Method 320 - Protocol for the use of FTIR spectrometry for the analysis of gaseous emissions from stationary sources; Federal Register V63 No.56, pp.14229-14237 (March 24 1998); also ava ilable (o n M ay 19 1999) at http://www .ep a.g ov/ttn/oa rpg/t3 /fr_ notice s/, file frprop.pdf. [3] ASTM Designation D 6348. Standard test method for determination of gaseous compounds by extractive direct interface fo urier tra nsform infrare d (FTIR ) spe ctros cop y. [4] ASTM Designation D 1356. Standard terminology related to sampling and analysis of atmospheres. [5] ASTM Designation E 168. Practice for general techniques of infrared quantitative analysis. [6] ASTM Designation E 1252. Practice for general techniques for obtaining infrared spectra for qualitative analysis. [7] EPA – Fourier Transform Infrared (FTIR) method validation at a coal-fired boiler, available (on May 19 1999) at http ://www .ep a.g ov/ttnem c01/ftir/reports, file r03.htm l. [8] W .K. Reagen et al., Environmental Science and Technology 33, pp. 1752-1759 (1999). [9] EPA – Validation Protoc ol, M eth od 301, available (o n M ay 19, 1999) through link s provided in the docum ent http://ww w.e pa.go v/ttn /em c/p rom gate.h tm l. [10] EPA FTIR Library of Hazardous Air Pollutants, available (on May 19 1999) at http://www.ep a.go v/ttnem c01 /ftir/data/e ntrop y/. This library contains m ultiple quantitative spectra for approxim ate ly 100 com pou nds with 0.25 cm -1 resolution (bo xca r apo dization). The us er m ust c alculate spectra for the des ired M IL and apod ization fro m the interfero m etric data provide d at the site http://www.epa.gov/ttnemc01/ftir/data/igram/ (see Re ference 2, Ap pendix K). Som e of these spe ctra were recorded at elevated gas te m peratures and m ay not be suita ble for quantitative workspace air ana lyses.

NIOSH Manual of Analytical Methods, Fourth Edition