[Code of Federal Regulations]

[Title 40, Volume 16]

[Revised as of July 1, 2006]

From the U.S. Government Printing Office via GPO Access

[CITE: 40CFR80.55]



[Page 663-664]

 

                   TITLE 40--PROTECTION OF ENVIRONMENT

 

         CHAPTER I--ENVIRONMENTAL PROTECTION AGENCY (CONTINUED)

 

PART 80_REGULATION OF FUELS AND FUEL ADDITIVES--Table of Contents

 

                     Subpart D_Reformulated Gasoline

 

Sec.  80.55  Measurement methods for benzene and 1,3-butadiene.



    (a) Sampling for benzene and 1,3-butadiene must be accomplished by 

bag sampling as used for total hydrocarbons determination. This 

procedure is detailed in 40 CFR 86.109.

    (b) Benzene and 1,3-butadiene must be analyzed by gas 

chromatography. Expected values for benzene and 1,3-butadiene in bag 

samples for the baseline fuel are 4.0 ppm and 0.30 ppm respectively. At 

least three standards ranging from at minimum 50% to 150% of these 

expected values must be used to calibrate the detector. An additional 

standard of at most 0.01 ppm must also be measured to determine the 

required limit of quantification as described in paragraph (d) of this 

section.

    (c) The sample injection size used in the chromatograph must be 

sufficient to be above the laboratory determined limit of quantification 

(LOQ) as defined in paragraph (d) of this section for at least one of 

the bag samples. A control chart of the measurements of the standards 

used to determine the response, repeatability, and limit of quantitation 

of the instrumental method for 1,3-butadiene and benzene must be 

reported.

    (d) As in all types of sampling and analysis procedures, good 

laboratory practices must be used. See, Lawrence, Principals of 

Environmental Analysis, 55 Analytical Chemistry 14, at 2210-2218 (1983) 

(copies may be obtained from the publisher, American Chemical Society, 

1155 16th Street NW., Washington, DC 20036). Reporting reproducibility 

control charts and limits of detection measurements are integral 

procedures to assess the validity of the chosen analytical method. The 

repeatability of the test method must be determined by measuring a 

standard periodically during testing and recording the measured values 

on a control chart. The control chart shows the error between the 

measured standard and the prepared standard concentration for the 

periodic testing. The error between the measured standard and the actual 

standard indicates the uncertainty in the analysis. The limit of 

detection (LOD) is determined by repeatedly measuring a



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blank and a standard prepared at a concentration near an assumed value 

of the limit of detection. If the average concentration minus the 

average of the blanks is greater than three standard deviations of these 

measurements, then the limit of detection is at least as low as the 

prepared standard. The limit of quantitation (LOQ) is defined as ten 

times the standard deviation of these measurements. This quantity 

defines the amount of sample required to be measured for a valid 

analysis.

    (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.