80.56—Measurement methods for formaldehyde and acetaldehyde.
(a)
Formaldehyde and acetaldehyde will be measured by drawing exhaust samples from heated lines through either 2,4-Dinitrophenylhydrazine (DNPH) impregnated cartridges or impingers filled with solutions of DNPH in acetonitrile (ACN) as described in §§ 86.109 and 86.140 of this chapter for formaldehyde analysis. Diluted exhaust sample volumes must be at least 15 L for impingers containing 20 ml of absorbing solution (using more absorbing solution in the impinger requires proportionally more gas sample to be taken) and at least 4 L for cartridges. As required in § 86.109 of this chapter, two impingers or cartridges must be connected in series to detect breakthrough of the first impinger or cartridge.
(b)
In addition, sufficient sample must be drawn through the collecting cartridges or impingers so that the measured quantity of aldehyde is sufficiently greater than the minimum limit of quantitation of the test method for at least a portion of the exhaust test procedure. The limit of quantitation is determined using the technique defined in § 80.55(d).
(c)
Each of the impinger samples are quantitatively transferred to a 25 mL volumetric flask (5 mL more than the sample impinger volume) and brought to volume with ACN. The cartridge samples are eluted in reversed direction by gravity feed with 6mL of ACN. The eluate is collected in a graduated test tube and made up to the 5mL mark with ACN. Both the impinger and cartridge samples must be analyzed by HPLC without additional sample preparation.
(d)
The analysis of the aldehyde derivatives collected is accomplished with a high performance liquid chromatograph (HPLC). Standards consisting of the hydrazone derivative of formaldehyde and acetaldehyde are used to determine the response, repeatability, and limit of quantitation of the HPLC method chosen for acetaldehyde and formaldehyde.
(e)
Other sampling and analytical techniques will be allowed if they can be proven to have equal specificity and equal or better limits of quantitation. Data from alternative methods that can be demonstrated to have equivalent or superior limits of detection, precision, and accuracy may be accepted by the Administrator with individual prior approval.