EPA-AA-TSS-PA-86-03
                   Analysis of Fuel Samples
           from Baltimore,  Detroit,  and Philadelphia
      (Report from Work Assignment 8,  Contract 68-03-3192
              with Southwest Research  Institute)
           Mary Ann Warner-Selph and Charles T. Hare
                 Southwest Research  Institute
            Craig A. Harvey and Jonathan Adler, EPA
                           July 1986
                            NOTICE
Technical  Reports  do   not   necessarily  represent  final  EPA
decisions or positions.   They are  intended to present technical
analysis  of  issues using data  which  are  currently  available.
The purpose in the  release of such  reports is to facilitate the
exchange  of  technical  information and  to inform the  public  of
technical developments which  may form  the basis  for a final EPA
decision, position or regulatory action.

                    Technical Support Staff
             Emission Control Technology Division
                    Office of  Mobile  Sources
                  Office of Air and Radiation
             U.S. Environmental  Protection Agency

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I.   INTRODUCTION

     The  objective  of  this  Work  Assignment  was  to  analyze
samples of  in-use  gasoline from  a  representative selection  of
gasoline outlets  that were  not major  (national) brands.   The
samples were  obtained under Work Assignment  No.  1  of  Contract
68-03-3192   from   three   cities:   Baltimore,   Detroit,   and
Philadelphia.   Thirty-nine   fuel   samples   originated   from
Baltimore,   36 from  Detroit,  and  48 from  Philadelphia,  for  a
total of  123 samples.  Single  samples  from most  of the  major
brand outlets in each city were included for comparison.

     Selection of  "minor" (regional) outlets  was done using  a
random selection weighted by sales  volume as  reported by  the
Lundberg Letter.   In other words,  each minor outlet  listed by
Lundberg  for  each   of  the   three  cities  was   assigned  a
probability  of selection proportional  to  its  reported  sales
volume.   Then,  using  a   random  number   generator,   forty  minor
outlets  from  each  city  were  selected so  as to   ensure  that
thirty  currently   operational   outlets   could  be  found  during
sample  collection.    (The Lundberg  data were not  fully up to
date for some  of the outlets,  so some  of the  outlets  no longer
existed.)   The major  outlets  (and ARCO  Oxinol  outlets)  were
chosen  arbitrarily  with  some  emphasis  on  selecting  larger
volume outlets of  each brand.  Premium Gasoline  was chosen for
every fourth sample;  current data indicate  that 25%  of unleaded
gasoline sold is premium grade.

     Fuel samples  were collected and stored in  sealed  cans as
is done  with MVMA fuel  samples.   For  the  first  few months of
storage these  cans were  kept in  a  refrigerated enclosure.   Due
to space  limitations  they  were  then  moved  to   an  underground
unrefrigerated storage room  with  an  estimated  temperature of
about 60°F.

     These  cities  and  this  sampling  bias  toward  non-major
outlets  were  chosen for a  combination of reasons.  The  MVMA
national fuel survey includes mostly major  brand  outlets,  while
non-major outlets tend to have  a greater use of alcohol blends,
which EPA wished to  characterize.   Also, in  Philadelphia,  ARCO
markets a gaspline/Oxinol1  blend, and  only one  sample  of  this
was included  in the  summer  1984 MVMA survey.  Therefore eleven
samples  of  this   fuel  were collected and  analyzed  in  this
program.  Section  V  of  this report  provides a  comparison  of
summer 1984 MVMA data with the results of this program.


1    A  fuel  additive  composed  of methanol  and  tertiary  butyl
     alcohol (TBA).

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                              -2-

     All samples  were  analyzed for Reid  Vapor Pressure  (RVP),
distillation  temperature  curve,   methanol,   ethanol,   tertiary
butyl  alcohol  (TEA),   water  content,   and   lead  content.   In
addition,  the  "Evaporative  Index"2  (El)  was  calculated  for
each fuel.   This parameter was developed by DuPont  to  correlate
volatility   characteristics  of   fuels  to   the   evaporative
emissions of vehicles.   Fuel control and  reference  samples were
also  analyzed  to fulfill  quality assurance  requirements  for
this Work Assignment.   The  reference  fuel samples were used to
determine procedural  accuracy and  repeatability.  The  control
fuel samples were  analyzed  periodically to assure repeatability
and reproducibility.                          ,   ;

     The test  plan was written up  as part  of the Work  Plan,
which is included  as  Appendix A.  The  test  plan describes  the
analysis sequence for  control  samples, reference  samples,  and
fuel samples.   Reference and control  samples  were analyzed in
duplicate   prior  to    fuel   sample   analysis.    Batches   of
approximately  twenty   fuel  samples  were  analyzed   for   RVP,
distillation  temperature curve,  alcohols,  water content,  and
lead content,  alternating  with  duplicate analyses of  control
samples.

     Fuel samples  were  originally  scheduled  for all analyses at
the  Engines,  Fuels   and  Lubricants  Division   of   Southwest
Research  Institute  (SwRI).  Due  to   scheduling  difficulties,
however, it became necessary to have the  water and distillation
analyses conducted at  other  laboratories.   The  measurement of
water  was  conducted   at  the  Fuels  and  Lubricants  Research
Division of SwRI.  Fuel distillations were  conducted by King
Laboratories in San Antonio.  All  other analyses  were conducted
at SwRI by the Engines, Fuels and Lubricants Division.


II.  ANALYTICAL PROCEDURES

     The  analytical    procedures  and   calculations   used   in
evaluating the gasoline samples are as follows:

     REID  VAPOR  PRESSURE  (RVP)  -  Automatic  RVP  Instrument
     Method.   It  has.  been  determined  by  the  ASTM  that  the
     conventional   "wet-bomb"   method   (ASTM-D-323)   is   not
     satisfactory  for analysis of  gasoline-alcohol  blends.  The
     Automatic  RVP Instrument,  developed at  SwRI  and used to
     analyze all  MVNA  survey samples,  has  been  found  to be  a
     satisfactory  alternate method.   This  method  is  described
     in Appendix B.
     El = 0.85 RVP +0.14 (percent evaporated at 200°F)
            - 0.32 (percent evaporated at 100°F).

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                              -3-

     DISTILLATION - ASTM D-86.

     METHANOL,  ETHANOL,   AND   TERTIARY  BUTYL   ALCOHOL   (Volume
     Percent) - Water Extraction/Gas Chromatography.  There  are
     currently no standard ASTM Procedures for  determination of
     alcohols  in  gasoline.    SwRI   has   developed  a   reliable
     analytical procedure  based on  extraction  of the  gasoline
     with  2  volumes  of water  and  gas  chromatography  of  the
     extract  using  a flame  ionization detector.  Full  details
     are given in Appendix B.   This method  is  used to  analyze
     MVMA survey samples.

     WATER   (Weight   Percent)   -   ASTM  D-1533'  Karl   Fischer
     Automatic Titration (pyridine  free),  using the Photo  Volt
     Aquatest IV instrument.

     LEAD  (Weight  Percent)  -  ASTM D-3237,  Atomic Absorption
     Spectrometry.

     EVAPORATIVE  INDEX  (El)  - From  RVP  and  distillation  data:
     El = 0.85XRVP - 0.32x(% EVAP @100°F) + 0.14x(%EVAP  @200°F)
                         r

III. RESULTS

     A description of the  fuel  samples is given in  Appendix C.
The  fuels,  which  were  obtained  from  Baltimore,  Detroit,  and
Philadelphia,  are  designated   as  either  regular  unleaded  or
premium unleaded.   The  locations of the gas stations where the
fuel samples were obtained are also given in  Appendix C.

     Table 1  summarizes  the average RVP data  grouped   by  city
and  by  alcohol   content.   The  results  of  RVP,  distillation,
alcohol, water,  and lead  analyses  are listed   in  Tables 2,  3,
and   4  for   fuel   samples   from   Baltimore,   Detroit,   and
Philadelphia,   respectively.    RVP  was   measured   in   psi,
distillation  in  °F,  alcohols  (methanol, ethanol,  and   TEA)  in
percent by volume, water by weight percent,  and lead in  g/gal.

     Fuel samples were  collected in mid September,  1984,  from
Baltimore,  Detroit,  and Philadelphia.   The  recommended limits
for RVP (as given in ASTM  Designation: D439-83)  of gasoline are
based  on the month of  the year as well as  location.   The  ASTM
specification  for   maximum  gasoline.  RVP   in   Baltimore   in
September  is  11.5  psi  (Class  C).   The  ASTM specification  for
maximum RVP  in Detroit  and  Philadelphia in  September   is  13.5
psi  (class C/D),  but September  is  a transition month,  so  fuel
conforming to the  11.5  psi standard  may  also be  sold.   The
specification  for both  of these  cities  in August  is 11.5  psi.
Seventy-seven  percent   of  the  Baltimore  fuel  samples   had
measured RVP  below  11.5  psi,  ten  percent had  measured  RVP
between 12.4 and 12.7 psi,  and thirteen  percent  were above  12.7

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                              -4-

psi.    Thirty-one   percent   of   the   Detroit   samples    and
twenty-three percent of the Philadelphia samples (or 3,0% if  the
Oxinol samples are  excluded) had RVP  less  than  or  equal to  11.5
psi.  All the fuel samples from Detroit, and ninety-six percent
of  the  Philadelphia  fuel samples  had measured RVP  less  than
13.5 psi.  The highest RVP of any  of the Philadelphia samples
was 13.7 psi.

     The  average  RVP  for  the   samples  in  Philadelphia   not
containing alcohol  (less  than 3% total  alcohol)  was 11.9  psi,
while the  average  RVP for the  gasoline/alcohol  blend samples
was  13.3  psi.    All  of   the  samples  in Philadelphia  which
contained alcohol were Oxinol samples.   It is possible  that all
of  the   Oxinol   samples   were   formulated  to   a   class   D
specification, which would explain  why their RVP's were so  much
higher than the other samples.   For Detroit, the average RVP of
samples  with  alcohol  (all  of  which  contained  7.7  -   10.5%
ethanol)  was  12.4   psi,  while  the  average  RVP   for  samples
without alcohol was 11.8 psi.

     Alcohol  content  and water  content  of  the  fuel samples
appeared to  be  related  variables.    These values  were plotted
and are presented in Figure 1.   Two major clusters of  data are
apparent:  relatively low  alcohol with low water and  relatively
high  alcohol with  high  water.   When total alcohol  (methanol,
ethanol, and  TBA) was  less than  1.0 percent (by volume) of  the
fuel  sample, water content  was  less  than  or equal  to  0.05
percent (by weight).  When total alcohols  exceeded 7.0  percent,
water content was greater than  or equal to 0.15 percent  of the
fuel sample.  One fuel sample had a high water  content  relative
to  the  other  samples.    Sample  70,   with  8.0  percent   total
alcohol, had  a water content of  0.48 percent.

     The  distillation curve  data  from the  fuel  samples  are
given  in  Tables  5,  6,   and 7  for   Baltimore,  Detroit,   and
Philadelphia.  In general,  the  samples  which contained alcohol
needed  lower temperatures   to  achieve  a  given   amount  of
evaporation  than those  which did  not contain  alcohol.   The
Evaporative   Index  was calculated  from  RVP  and  distillation
curve data.  These El values are reported  in Table 8.   Figure 2
shows  the  frequency  distributions  of  the  El values  of  the
samples grouped by city and fuel type.   The distillation  values
of  some  control  samples,  which were  periodically  analyzed  with
the three-city fuel samples, were out  of the range specified in
the Quality  Assurance  Plan.   This  situation is  discussed  in the
Quality Assurance Assessment  section,  and  should be  taken  into
consideration when  using  the  distillation  and El  values for the
sampled fuels.

     The EPA  specified maximum lead level  in unleaded  gasoline
is  0.05 g/gal.   All but  one fuel sample had lead concentrations
below this level.  Fuel sample 58 contained 0.83 g/gal-of  lead.

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                              -5-

           Table 1  Summary of RVP Data, Grouped by
                    City and Alcohol  Content
                                   Avq.  RVP (psi)
             Brand            less than    more than
City         Distribution"     3% alcohol    3% alcohol

Baltimore


Detroit


Philadelphia
*  Oxinol  is  considered separately  from national  and  regional
groups.
National
Regional
National
Regional
National
Regional
(Oxinol)
11.3
11.1
11.2
12.0
12.0
11.9


12.:7
12/4

13.3

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                      -6-
Table 2.  RVP, Alcohol Fraction, Water Fraction,
   and Lead Content of Baltimore Fuel Samples
Sample
Identification3
1 AMOCO (R)
2 ARCO(R)
3 BPOU(R)
4 Exxon (P)
5 Getty (R)
6 Gulf(R)
7 Mobil (R)
8 Shell (P)
9 Sunoco (R)
10 Texaco (R)
11 Merit (R)
12 Merit (P)
13 Crown (R)
1* Crown (R)
15 Crown (R)
16 Crown (P)
17 Citgo(R)
18 Merit (R)
19 Crown (R)
20 Hess(R)
21 Crown (P)
22 Crown (R)
RVP, psi
Automatic
11.0*
11.20
11.13
10.52
12.46
11.21
11.37
11.09
11.93
11.21
11.50
10.8*
10.47
11.25
10.99
10.40
11.20
10.96
10.29
11.43
10.72
10.36
% by Volume
Methanol Ethanoi TBA
NATIONAL
~b « 0.42.
0.14
0.37
__
._
0.11
0.19
..
0.15
0.54
REGIONAL
—
—
—
__
0.12
—
-- — 0.54
--
—
—
0.14 — 0.11
-- -- --
Water,
Wgt. %
0.01
0.01
0.02
0.02
0.01
0.01
0.01
0.02
0.02
0.02
0.01
0.02
0.01
0.01
0.02
0.02
0.02
0.02
0.02
0.02
0.04
0.05
Lead,
g/gal
0.005
0.006
0.007
0.003
0.001
0.004
0.007
0.006
0.003
0.008
0.007
0.008
0.004
0.005
0.005
0.003
0.006
0.010
0.004
0.006
0.002
0.005

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                                -7-
   Table 2.  (Cont'd)  RVP,  Alcohol Fraction,  Water Fraction,
           and  Lead Content of Baltimore Fuel Samples
Sample
Identification3

23 Crown (R)
21 Crown (R)
25 Merit (P)
26 BPOil(R)
27 Crown (R)
28 Merit (R)
29 Citgo(R)
30 Citgo(R)
31 Citgo(R)
32 BPOU(R)
33 No Brand (R)
3* Big Red (R)
35 Crown (R)
36 BPOil(P)
37 7-11 (R)
38 Merit (R)
39 Crown (P)
Avg. with alcohol0
Avg. without alcohol
S.D. with alcoholc
S.O. without alcohol
RVP. psi % by Volume
Automatic Methanoi Ethanoi
REGIONAL
10.62
10.79
10.91 0.11
12.62
10.91
11.61
12.51
10.86 0.15.
10.73 0.17
12.67 0.12
11.81
11.63
10.23
10.56
11.58
11. *9
10.72
000
11.2 0.02 0
0 ' 0 0
0.6 0.05 0
- Water,
TBA Wet. %
'
0.0*
— '* 0.05
0.05
0.03
0.03
0.0*
0.0*
0.15 0.03
0.15 0.03
0.03
0.22 0.0*
0.0*
0.0*
0.03
0.02
. — 0.0*
0.10 0.03
0 0
0.08. 0.03
0 " 0
0.15 0.01
Lead,
g/gal

0.00*
0.00*
0.006
0.00*
0.005
0.006
0.00*
0.005
0.010
0.00*
0.006
0.010
0.00*
0.003
0.010
0.006
0,002
0
0.005
0
0.002
a3% total alcohols

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Table 3.
and
Sample
Identification3
40 Boron (R)
41 Shell (R)
42 Union 76 (R)
43 Sunoco (R)
44 Union 76 (R)
45 AMOCO (P)
46 Mobil (P)
47 Total (R)
48 No Brand (R)
49 Speedway (P)
50 Martin (R)
51 No Brand (R)
52 Total (R)
53 Total (P)
54 Total (R)
55 Speedway (R)
56 Total (P)
57 Clark (R)
58 Citgo(R)
59 Tulsa(R)
60 Total (P)
RVP, Alcohol Fraction, Water Fraction,
Lead Content of Detroit Fuel Samples
RVP. psi % by Volume
Automatic Methanol Ethanol
NATIONAL
12.11 -b
11.06
12.74 ~ 7.70
11.22
10.36
11.32
11.05
REGIONAL
12.09
12.39
11-. 46
12.09
10.88 — 10.1
11.02
12.27 — 10.3
12.00
12.40
11.97 — 10.1
12.75
11.94
13.22 — 10.2
11.10 — 10.5
.Water,
TBA Wgt. %
0.04
0.03
0.20
0.01
0.02
0.04
0.04
0.02
0.03
0.03
0.02
0.20
0.02
0.19
0.02'
0.02
0.21
0.02
0.02
0.17
0.21
Lead,
g/gal
0.002
0.002
0.005
0.001
0.001
0.003
0.002
0.004
0.001
0.002
0.005
0.001
0.004
0.016
0.004
0.001
0.004
0.003
0.83C
0.001
0.004

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                                -9-
   Table 3. (Cont'd) RVP, Alcohol Fraction,
            and Lead Content  of  Detroit Fuel
    Sample
% by Volume
Water  Fraction,
Samples

       Water,   Lead,
4
Identification3

61 Speedway (R)
62 Clark (R)
63 Total (R)
6* Pennzoil (R)
65 Clark (R)
66 No Brand (R)
67 Gas & Go (R)
68 Host(P)
69 Citgo(R)
70 Martin (R)
71 Tulsa(R)
72 Hi-Fy(P)
73 Clark (R)
7* Total (R)
75 Total (R)
Avg. with alcohol^
Avg. without alcohol
S.D. with alcohold
S.D. without alcohol
_ j t 	
Automatic

12.19
13.19
11.46
11.66
12.89
13.06
12.23
12.41
13.34
13.19
12.38
12.03
11.64
11.85
10.46
12.4
11.8
0.8
0.7
Methanol Ethanol
REGIONAL
—
—
—
—
—
9.22
—
9.38
9.83'
8.89
9.86
9.77
—
._
0.16
0 9.6
0 0.01
0 0.8
0 0.03
TEA Wgt. %

0.04
- '* 0.05
0.04
0.04
0.04
0.18
0.04
0.22
0.19
0.48
0.20
0.19
0.04
0.04
0.04
0 0.22
0 0.03
0 0.08
0 0.01
g/gal

0.001
0.002
0.004
0.002
0.002
0.003
0.002
0.005
0.004
0.005
0.002
0.002
0.002
0.005
0.003
0.004
0.003
0.004
0.001
a(R) = Regular, (P) = Premium
b=<0.1%
C5ample 58 lead value not included in averaging
^Includes samples with > 3% total alcohols

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                      -10-
Table 4.  RVP, Alcohol Fraction,  Water Fraction,
  and Lead Content of Philadelphia Fuel Samples
Sample
Identification3
76 BPOil(R)
77 Gulf(R)
78 Amoco (R)
79 Exxon (P)
80 Sunoco (R)
81 Mobil (R)
82 Texaco (R)
83 Citgo(R)
84 Hess(R)
85 BPOil(R)
86 Alert (P)
87 Merit (R)
88 Hess(R)
89 Hess(R)
90 Citgo(P)
91 Golden (R)
92 BPOU(R)
93 7-11 (R)
94 BPOU(P)
95 Citgo(R)
RVP, psi
Automatic
13.38
11.79
11.71
10.66
11.80
11.84
12.74
12.48
12.31
12.81
12.99
11.91
10.93
10.58
12.22
11.63
11.40
12.37
9.76
12.14
% by Volume
Methanol Ethanoi TBA
NATIONAL
-b
0.19
2.08
0.21
..
—
__
REGIONAL
0.40
0.13
..
__
0.13
—
__
1.60
._
0.18 — 0.18
0.64
—
0.70
Water,
Wgt. %
0.02
0.03
0.08
0.03
0.04
0.03
0.03
0.03
0.03
0.02
0.02
0.03
0.03
0.02
0.04
0.03
0.03
0.03
0.03
0.04
Lead,
<0.001
<0.001
0.009
0.003
0.002
0.002
0.001
0.002
0.003
0.001
0.001
0.003
0.005
0.005
0.005
0.003
0.005
0.002
0.002
0.002

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                          -11-
Table 4. (Cont'd)  RVP,  Alcohol Fraction,  Water Fraction,
      and Lead Content of Philadelphia Fuel Samples
Sample
Identification*

96 Merit (R)
97 Merit (R)
98 Hess(P)
99 Merit (R)
100 T.F.C.O. (R)
101 Merit (R)
102 Hess(P)
103 Hess(R)
104 BP Oil (R)
105 Hess(R)
106 BPOil(P)
107 Citgo(R)
108 Merit (R)
109 Alert (R)
110 Merit (P)
111 Citgo(R)
112 Wm. Penn(R)

113 ARCO(R)
11* ARCO(R)
115 ARCO(R)
RVP. osi % by Volume
Automatic Methanol Ethanoi
REGIONAL
11.48
11.08
11.97
11.47
12.08
11.12
12.04
11.86
13.11
11.93
13.01
12.31
11.38
12.53
11.16
12.13
12.02
*
OXINOL
13.38 4.13
13.61 4.03
13.52 4.00

TBA

0.10,.
—
—
0.10
0.11
—
—
0.12
—
0.14
—
0.45
—
—
0.14
0.60
--

3.76
3.75
3.65
Water,
Wgt. %

0.03
0.03
0.04
0.04
0.05
0.04
0.05
0.03
0.03
0.03
0.04
0.04
0.04
0.04
0.04
0.04
0.04

0.16
0.19
0.17
Lead,
g/gal

0.004
0.004
0.006
0.005
0.006
0.005
0.007
0.003
0.001
0.003
0.001
0.002
0.004
0.001
0.004
0.002
0.002

0.002
0.002
0.002

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                                -12-
     Table 4. (Cont'd)  RVP,  Alcohol Fraction,  Water Fraction,
           and Lead Content of Philadelphia Fuel  Samples
Sample
Identification3
116 ARCO(R)
117 ARCO(P)
118 ARCO(R)
119 ARCO(R)
120 ARCO(R)
121 ARCO(P)
122 ARCO(R)
123 ARCO(R)
Avg. with alcohol0
Avg. without alcohol
S.D. with alcohoic
S.D. without alcohol
RVP, psi
Automatic
13. 48
12.71
13.19
13.46
13.74
12.90
13.19
13.16
13.3
11.9
0.3
0.8
%by
Methanol
OXINOL
4.18
4.32
4.06
3.94
4.03
4.06
3.81
4.20
4.1
0.02
0.1
0.05
Volume
Ethanol

--
• •V
—
—
^^
—
v«
0
0
0
0

TBA
3.77
3.96
3.72
3.61
3.72
3.64
3.67
3.76
3.7
0.21
0.1
0.44
Water,
Wgt. %
0.16
'* 0.15
0.17
0.17
0.16
0.16
0.23
0.15
0.17
0.03
0.02
0.01
Lead,
g/gal
0.002
0.002
0.002
0.002
0.003
0.002
0.002
0,002
0.002
0.003
0.000
0.002
*(RT= Regular, (P) = Premium
b=<0.1%
Includes samples with >3% total alcohols

-------
   0.3
   0.2
ao
T-l
0)
2  o.i
   0.0
                                          -13-
                                                           0
                                                                    
-------
Table 5.   Distillation  Data  from Baltimore  Fuel Samples
Sample
Number

1
2
3
4
5
6
7
8
9
10

11
I2a
13
14
15
16
17
18
2?a
22
23
24
25
26
27
28
29
30
31
33
34 '
35
36
37
38
39
Temperature, °F at % Evaporated
IBP 5%
National
91 115
91 120
88 108
95 122
81 99
84 108
84 112
89 116
83 109
94 113
Regional
90 114
87 106
90 124
89 115
93 122
93 122
99 122
100 124
92 114
98 119
100 129
98 125
99 122
93 116
94 123
91 121
99 120
99 126
97 118
97 124
91 120
102 128
102 139
97 117
91 113
100 131
10%

126
133
117
133
107
120
122
127
120
123

123
120
138
126
133
135
129
131
128
130
142
138
134
128
135
132
131
139
129
138
134
136
156
129
124
146
15%

135
144
124
140
115
129
132
136
129
132

133
131
147
136
144
147
136
140
140
140
153
147
144
136
146
140
142
143
138
147
144
144
168
138
133
156
20%

145
151
135
149
122
138
141
145
140
142

143
141
156
148
154
158
147
149
150
151
158
156
152
147
156
151
151
153
149
156
151
158
178
149
143
165
30%

165
160
158
170
137
156
160
158
160
163

162
161
172
169
175
176
167
171
174
172
169
176
170
158
174
171
167
176
171
177
169
179
190
169
165
185
40%

190
181
183
192
160
180
185
175
183
188

182
187
190
193
195
192
190
194
201
195
192
198
188
190
194
194
187
196
194
199
186
203
205
192
190
207
50%

216
212
211
217
181
208
207
193
207
208

210
214
210
216
214
219
216
221
221
222
217
218
201
214
212
212
212
219
221
219
205
217
230
212
219
228
60%

242
237
239
239
210
234
235
219
234 .
240

240
233
234
233
241
241
242
246
241
246
234
243
225
239
235
243
235
241
246
244
225
240
247
230
246
246
70%

268
264
268
264
241
264
264
235
264
267

268
248
262
266
268
263
271
273
262
270
268
270
243
265
263
261
262
268
273
271
251
268
269
257
273
262
80%

300
297
305
300
281
300
300
257
298
301

300
271
295
298
302
297
306
306
291
302
300
306
265
296
293
297
295
306
307
301
275
302
299
297
307
297
90%

345
342
356
342
325
356
343
298
351
342

342
305
338
345
343
330
352
349
330
340
342
345
300
334
338
346
331
356
349
340
351
340
334
363
351
329
95% EP

372 418
372 414
394 420
358 399
356 390
387 430
372 421
334 379
385 424
380 418

378 412
343 385
365 417
376 421
380 424
361 402
390 419
376 423
357 403
370 410
369 423
376 421
328 382
366 398
364 414
381 419
360 403
396 432
383 423
369 417
390 423
376 421
355 410
405 433
379 423
367 419
alnstruinent 02
bNo data
                                                                      Residue (%)   Recovered (%)
                                                                         1.5
                                                                         1.5
                                                                         1.5
                                                                         1.0
                                                                         1.5
                                                                         1.5
                                                                         1.0
                                                                         1.5
                                                                         1.0
                                                                         1.0
98.5
98.0
97.5
98.5
98.5
98.5
98.5
98.0
98.5
98.5
                                                                                      98.0
                                                                                      98.0
                                                                                      98.0
                                                                                      98.5
                                                                                      98.5
                                                                                      98.5
                                                                                      98.0
                                                                                      98.0
                                                                                      99.0
                                                                                      99.0
                                                                                      99.0
                                                                                      98.5
                                                                                      99.0
                                                                                      97.0
                                                                                      99.0
                                                                                      98.0
                                                                                      98.5
                                                                                      98.0
                                                                                      98.0

                                                                                      98.5
                                                                                      98.0
                                                                                      98.5
                                                                                      99.0
                                                                                      98.0
                                                                                      99.0
                                                                                      98.0

-------
Table 6.    Distillation Data  from Detroit Fuel  Samples
Sample
Number IBP
Temperature, °F at % Evaporated
5%
10%
15%
20%
30%
40%
50%
60%
70%
80%
90%
95% EP
National
40a 87
41 95
42 96
43 86
44 98
45 95
46a 89
107
118
112
108
120
124
116
120
. 130
118
120
131
139
135
131
140
123
133
' 139
149
' 153
145
150
128
143
147
160
170
173
171
139
163
165
181
203
201
194
150
182
186
205 '
218
228
210
192
210
214
230
230
253
236
230 |
240
241
245
243
279
260
263
269
269
273
263
309
288
297
304
305
316
298
348
326
342
350
346
347
337
386 425
360 424
378 412
400 440
382 425
370 403
372 421
Regional
47 89
48a 86
49 92
50 90
5la 99
52a 91
53 95
54 87
55 86
57 94
58 86
59 94
60 102
61 84
62 87
63 89
64 91
65 90
66 84
67 91
68 91
69 90
70 98
71 90
72 96
73 97
74 89
75a 96
aliistruineiit It 2
bNo data
108
105
136
111
116
109
113
108
117
115
110
114
122
106
110
112
124
114
113
III
108
104
115
109
111
122
112
117

119
118
143
117
122
119
120
120
130
128
121
121
127
118
120
122
136
126
120
124
117
113
122
118
117
134
121
130

130
130
153
121
127
128
125
130
. 139
140
130
128
133
129
130
130
148
135
126
136
123
118
129
126
124
145
130
140

140
140
168
131
131
138
130
140
150
150
138
134
137
144
140
138
160
145
131
149
131
123
132
132
130
156
139
143

158
167
198
151
141
146
139
161
168
171
156
144
146
167
163
158
187
165
141
180
144
133
145
145
144
178
158
157

184
195
218
174
150
181
150
187
188
193
177
155
158
196
192
179
214
190
151
208
153
144
155
155
156
203
182
ISO

214
223
233
200
172
208
177
215
219
218
197
206
187
221
237
206
239
214
181
235
189
154
210
199
208
230
207
207

240
250
250
229
222
235
228
243
244
240
228
238
229
250
243
234
262
247
225
261
234
208
244
238
219
257
236
236

269
276
273
259
254
264
260
275
271
268
260
266
266
279
270
265
288
279
254
288
265
248
274
260
264
284
264
264

302
309
307
293
285
300
293
307
310
304
301
302
302
318
308
300
311
315
293
318
299
288
309
300
298
318
295
298

340
351
350
341
330
325
337
346
357
355
350
352
345
372
362
337
354
365
347
367
343
336
362
347
343
358
330
332

369 429
381 419
390 420
375 426
361 409
362 420
365 412
381 426
397 427
390 426
382 424
384 421
374 414
414 425
404 424
363 423
392 437
399 430
379 420
403 430
372 420
374 406
406 425
383 420
381 403
394 434
366 410
364 417

                                                                           1.5
                                                                           1.0
                                                                           1.5
                                                                           1.0
                                                                           1.0
                                                                           1.0
                                                                           1.5
                                                                            .0
                                                                            .0
                                                                            .5
                                                                            .0
                                                                            .0
                                                                            .0
                                                                            .0
                                                                            .0
                                                                            .5

                                                                            .0
                                                                            .5
                                                                            .5
                                                                            .0
                                                                            .5
                                                                            .5
                                                                            .0
                                                                            .0
                                                                            .5
                                                                            .0
                                                                            .5
                                                                            .5
                                                                            .5
                                                                            .5
                                                                            .0
                                                                            .5
                                                                            .5
                                                                            .0
                                                                            .0
                                                                                    Recovered (%)
98.0
99.0
98.5
98.5
98.5
98.5
98.0
99.0
99.0
97.0
99.0
99.0
99.0
99.0
98.0
97.0

98.5
98.5
98.5
99.0
97.0
97.5
99.0
99.0
97.5
99.0
97.5
98.5
98.0
98.0
99.0
98.0
98.0
99.0
99.0
Ul
I

-------
Table  7.   Distillation  Data from Philadelphia  Fuel  Samples
Number
IBP
3%
10%
U*
' JM4 '
• mi"
~W~
M*
co«
70%
80%
90%
m
JP
National
76
77
7Sa
79
to
lla
82
89
91
90
90
88
90
92
107
121
108
109
110
114
110
120
132
116
120
119
121
120
130
141
12)
130
126
130
I2S
141
149
13)
141
137
140
13)
164
1))
1)6
162
1)4
162
149
188
17)
ISO
190
179
186
160
206
201
20S
218
206
212
182
232
223
238
238
241
240
208
2)9
246
2)8
2)7
277
270
241
289
27)
307
290
310
308
276
326
321
34)
336
3)3
3))
31)
3)6
3)6
370
3)7
386
387
346
399
408
419
403
42)
416
402
Regional
83*
S4a
8$
86*
87a
88
89
90*
913
92*»
936
94*
9)3
963
97
98a
99»
100*
101
102^
103
104
10)
106
I07a
108
109
110
Ilia
1123

113
114
11)
116
Il7a
ii8a
Il9a
1203
121
122
123
86
8)
90
84
87
86
90
8)
90


94
86
88
92
93
90
87
92
84
88
90
94
83
86
91
8)
90
85
93
Oninol
88
92
92
91
90
89
90
90
9J
91
86
108
100
120
119
101
114
II)
107
114

.
132
109
108
107
III
110
103
121
106
112
III
114
137
10)
112
112
116
108
100

102
106
106
107
III
101
104
103
III
III
101
122
III
131
140
113
126
126
117
129


144
120
120
IIS
122
122
II)
131
120
120 .
12)
122
1)3
118
123
124
130
120
III

109
113
III
113
120
110
110
110
IIS
117
110
132
121
140
1)7
123
136
13)
128
139


D)
130
I2S
127
131
132
124
136
134
12S
136
130
166
127
131
133
140
131
119

117
117
117
117
12)
II)
II)
116
122
121
II)
140
130
149
17)
131
146
14)
137
I4S


170
140
137
136
141
140
134
143
14)
137
144
137
177
137
141
140
1)0
140
128

123
122
122
123
133
121
121
121
129
126
120
1)4
149
167
201
DO
164
160
160
162


19)
160
1)8
1)6
163
160
1)4
164
172
1)2
148
1)6
184
1)8
160
1)7
170
160
148

136
13)
134
136
1)8
134
134
133
144
142
133
17)
169
183
217
172
IS)
181
1S4
190


214
ISO
ISI
180
192
181
17)
182
197
1)4
162
178
211
176
181
177
183
182
172

1)7
1)6
1)6
1)7
186
1)6
I))
1)4
171
163
1)7
200
190
207
232
197
19)
20)
207
220


228
203
208
207
218
198
206
206
219
199
I8S
203
227
200
210
19)
201
204
204

177
178
181
IS3
217
182
ISO
179
196
191
183
222
219
226
24)
22)
221
234
236
248


241
226
236
236
238
228
242
23)
236
227
214
238
241
222
23)
217
234
226
242

210
208
212
209
246
211
208
206
226
218
212
246
2)0
2)1
267
2)6
248
2)3
264
277


260
2)0
266
264
2)6
260
276
26)
2)4
2)8
242
260
260
244
264
246
2)4
2)0
282

246
242
247
244
26S
244
24)
241
2)9
248
24)
27S
286
283
300
292
281
299
297
31)


288
280
297
301
280
297
311
297
278
294
276
29)
290
27S
296
27S
280
283
311

284
280
2SO
279
294
281
280
281
293
284
279
318
330
313
340
334
314
339
340
360


317
316
334
340
330
338
3)3
337
330
333
314
336
328
3IS
332
320
314
316
3)3

3D
314
319
318
334
323
323
321
331
32)
3D
3)1
3)7
3)1
388
362
344
369
372
394


344
343
362
370
368
370
387
360
372
364
343
372
368
34S
3)9
3)3
346
3)6
384

3)8
3)8
3)7
3)8
3)8
346
343
3)7
371
3)8
343
389
384
399
39S
400
402
414
412
421


399
406
40)
411
408
401
421
40)
412
40)
394
406
406
393
408
399
404
407
421

410
401
404
401
400
401
406
399
408
400
406
instrument 12
bNo data














                                                                         Residue (%)   Recovered (%)
                                                                             I.)
                                                                             I.)
                                                                             1.0
                                                                             1.0
                                                                             1.0
                                                                             I.)
                                                                             1.0
98.0
98.)
99.0
99.0
99.0
98.0
98.)
                                                                                        98.0
                                                                                        98.0
                                                                                        98.)
                                                                                        96.)
                                                                                        98.0
                                                                                        99.0
                                                                                        99.0
                                                                                        98.0
                                                                                        97.)
                                                                                         99.0
                                                                                         99.)
                                                                                         99.0
                                                                                         98.)
                                                                                         97.)
                                                                                         97.)
                                                                                         97.)
                                                                                         99.0
                                                                                         9S.O
                                                                                         98.0
                                                                                         98.)
                                                                                         98.0
                                                                                         97.0
                                                                                         98.)
                                                                                         99.0
                                                                                         98.)
                                                                                         99.0
                                                                                         9S.O
                                                                                         99.0
                                                                                         99.0
                                                                                         98.)
                                                                                         99.0
                                                                                         98.
                                                                                         97.
                                                                                         98.
                                                                                         98.
                                                                                         98.
                                                                                         98.0
                                                                                         99.0
                                                                                         99.0
                         O\
                          I

-------
                          -17-

   -Table 8.   Evaporative Index (El)  of Fuel Samples'

Baltimore           Detroit             Philadelphia
                                     Sample      El

                                        76        16.8
                                        77        16.5
                                        78        15.7
                                        79        14.3
                                        80        15.9
                                        81        15.7
                                        82        18.0
                                        83        16.4
                                        84        16.2
                                        85        16.9
                                        86        14.1
                                        87        15.7
                                        88        15.8
                                        89        15.1
                                        90        15.8
                                        91        15.1
                                        92b       	
                                        93b       	
                                        94        12.6
                                        95        16.2
                                        96        15.4
                                        97        15.1
                                        98        15.4
                                        99        15.9
                                        100       15.5
                                        101       15.7
                                        102       14.8
                                        103       16.2
                                        104       17.9
                                        105       16.4
                                        106       15.3
                                        107       16.3
                                        108       15.5
                                        109       17.1
                                        110       15.8
                                        111       15.9
                                        112       15.4
                                        113d      18.0
                                        114d      18.7
                                        115d      18.4
                                        116d      18.5
                                        117d      16.1
                                        118d      17.5
                                        119d      18.3
                                        120d      18.6
                                        121d      17.5
                                        122d      18.0
                                        12:
                                       Avg
                                       Std dev     1.3
Sample El
1 14.9
2 15.4
3 14.8
4 14.7
5 16.7
6 15.1
7 15.2
8 16.1
9 15.6
10 15.4
11 15.5
12 14.2
13 14.6
14 14.8
15 14.8
16 14.4
17 15.5
18 15.1
19 b 	
20b 	
21 14.1
22 14.5
23 15.1
24 14.7
25 16.1
26 16.2
27 15.0
28 15.4
29 16.8
30 14.9
31 14.7
32b 	
33 15.4
34 15.9
35 14.0
36 14.1
37 15.7
38 15.2
39 14.2
Avg 15.1
Std dev 0.7
a El =. 0.85 x RVP
(% Evap @100
Sample
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56b
57
58
59
60
61
62
63
64
65
66
67
68
69
70
71
72
73
74
75
Avg
Std dev



- 0.32 x
°F) +
El
14.7
15.2
17. 7C
14.9
14.9
14.6
12.7
15.2
15.2
13.5
16.5
16. 9e
15.1
17. 6C
15.3
15.7
	
16.3
16.4
17. 6C
16. 9C
14.8
16.0
15.7
14.3
16.3
17. 6e
14.7
17. lc
18. 3C
17. 7C
16. 7C
16. 5C
15.0
15.9
15.2
15.8
1.3





0.14 x (% Evap @200°F)
b No data
c Gasohol fuels
( approximately
d Oxinol fuels


10% ethanol)






-------
                               -18-
         DETROIT    DETROIT   BALTIMORE  PHILADELPHIA  PHILADELPHIA
MIDPOINT  GASOHOL    GASOLINE   GASOLINE   GASOLINE     OXINOL

 12.6     +         +X        +         +X          *
 13.0     +         +         +         +           +
 13.4     +         +X        +     .    +           +
 13.8     +         +         +         +           +
 14.2     +         *X        +XXXXX    *XX         +
 14.6     +         +XXX      +XXXXXX    +           +
 15.0     •(•         +XXXXX    ^XXXXXXXXX +XXXX        +
 15.4     +         +XXXXX    +XXXXXXXX  +XXXXXX      +
 15.8     *         +XXX      +XXX      +XXXXXXXXXX  +
 16.2     +         +XXX      -t-XXX      +XXXX        +X
 16.6     +XX        +XX       +X        +XXX         *
 17.0     "^AAA       "*"         "*"A        "* AAA         *
 17.4+         +         +         -i-           +XXX
 17.8     +XXXX      +X        +         +X          +
 18.2     +X        +         +         +X          +XXX
 18.6     +         *         +         +           +XXXX
 19.0     +         +         +         +           +
     Figure 2.  Distributions  of Evaporative  Index

-------
                              -19-

IV.  QUALITY ASSURANCE ASSESSMENT

     Six  refernce  and  two   control  fuels  were  subjected  to
several  initial   analyses.    Descriptions  of  these  fuels   are
listed  below.   Reference  fuel  4  was  replaced with  Reference
fuel  6,  which  has  500  ppm  (0.05  weight  percent)  of  added
water.  Reference  fuel  4 was  spiked  with 100  ppm  (0.01  weight
percent)  water,   which   appeared to  be  at   the  detectability
limits   of   the   water   analysis    method   for   use   with
gasoline-alcohol  blends.

Fuel Sample  	Description	'•_	

Reference 1  2,2-dimethylbutane, 9.9  psi at 100°F (for RVP analysis)
Reference 2  5% methanol, 5% TEA in unleaded Indolene (by volume)
Reference 3  10%  ethanol in unleaded Indolene (by volume)
Reference 5  Two lead samples provided  by the EPA: 5a = 0.717 g/gal,
             5b = 0.0166 mg/gal
Reference 6  0.05 weight percent (500 ppm) added water in Reference 2

Control 1    Unleaded Indolene
Control 2    Same fuel batch  as Reference 2


     The samples  were analyzed  according  to  the schedule shown
in Table  9,  and the  results are given in Table  10.   Detailed
listings  of  distillation data  for  Reference  2  (also  called
Control 2) and Control 1 are  presented  in  Appendix D.   With one
exception,  the  reported  values  fell  within  the  precision,
accuracy,  and  confidence   limits   specified  in  the  quality
assurance  plan   (Table   11).    An  exception  occurred  with
Reference I, in which one of  the RVP values using the ASTM D323
method  was  outside the limit specified  in  the QA plan  by 0.1
psi.   The  ASTM  D323  method  appears  to  give a  somewhat wider
dispersion   of   values   than   initially  anticipated.    After
discussion  with  the  EPA  Project Officer,  it  was decided  to
accept  the  RVP values  and  SwRI was authorized to proceed with
sample analyses.

     Analysis of an initial  Reference  1 sample was considerably
outside  reasonable  limits,   indicating  some   apparent  problem
with  that  sample.   Therefore,  that  sample  was  discarded and
another Reference l sample was used.

     In  addition  to  the  initial   analyses   of  reference  and
control  fuels,  the  two  control   samples   were  analyzed  in
duplicate between  batches of  samples.  The  results of the Reid
vapor pressure analyses  of  Controls  1 and 2  are  given in Table
12.  The  average Control 1  RVP for both  the automatic and the
bomb methods was  8.9  psi.   The  average Control  2  RVP  using the

-------
                              -20-

automatic method was'10.5 psi, and  for  the bomb method  it  was
10.4 psi.  All but one  set  of controls fell within the quality
assurance  guidelines.   The  controls  analyzed  between  sample
batches  4  and 5  were  slightly  outside   the  reproducibility
specifications of only  one  value in 20,  differing by more than
0.6 psi.   A  fresh  set  of  controls  was analyzed  and several
samples  within  batch  5  were  re-analyzed.   The  new control
values  agreed within the  allowed limits,  and the  re-analyzed
samples  of  batch 5  agreed within two percent of the  original
values.

     Alcohol analyses of Control 1 showed less than  0.1 percent
methanol, ethanol,  and  TEA  for  all  analyses.  'The results of
analyses of Control  2  for alcohols  are  presented in Table  13.
The average measured methanol  level  in  the standards was 5.0,
percent and the average measured  level of  TBA was 4.7  percent.
Ethanol was not  detected in  any  of the samples  (detectability
limit is 0.1 percent).   The measurement  of  methanol  fell  within
the range given in the  Quality Assurance Plan, however,  several
TBA measurements  were  out  of  the  range given  for TBA.   Some
measured  TBA  values were  up  to ten percent  lower  than  the
concentrations  to   which  the  corresponding   controls   were
prepared.  One possible explanation is  that  samples giving low
TBA values may have  been  drawn from a fuel can  which  was lower
in  TBA  than other  cans.    It  is  also  possible  that  the
variability in the procedure  for  measuring TBA is on  the order
of ten percent rather than five percent.

     Water  analysis  results for  the control  samples  are given
in Table  14.   The average  water  content was  about 0.1  weight
percent for Control  2 and about 0.02 weight percent for Control
1.  Considerable  variation  in  measured  water levels  occurred.
The reason  for the variation is  not known.   However,  since the
water  content of the  initial  samples  was  about half  of  the
latter values,  it can be speculated that  the controls absorbed
water from the atmosphere over  time.  Repeatabilities  have not
been    previously   established   for    water   analysis   of
gasoline-methanol blends, or  even for gasolines  not  containing
alcohols.  Analysis  of  the control fuels for  lead  yielded  lead
values less than the detection  limit of  the method,  0.001 g/gal
of lead.

     The  two  specified control  samples  and an  additional  fuel
sample, a regular unleaded  gasoline  on which  distillation data
were  available,   were  analyzed  for  distillation  temperature
curve.  Due to stringent time constraints,  two instruments were
utilized  to  analyze the  controls  and samples.   The  second
instrument, however,  was  not  available until   over  half  the
total analyses had been completed.

-------
                              -21-

     This situation came  about as a result of several  factors.
The samples were collected in a previous project in  late  summer
of  1984,   with  the   understanding  that  analyses  would  be
conducted in the fall  of 1984 in the same manner as  was  applied
in  the analyses  given in Report  EPA 460/3-84-009.   In  that
study, a reasonable number of data checks were applied to those
analyses considered to be  of  primary  importance  to  the  intended
usage of the  data.  The laboratory at  SwRI  that was scheduled
to conduct  the  fuels  analyses has a relatively relaxed  schedule
in  the fall  and spring,  and  a  very  hectic  schedule  in  the
winter and summer.

     Authorization  to  proceed  with  the  analyses  was  not
received  until  well   into  the  spring  of   1985.   With  the
incorporation of numerous  quality assurance requirements  to be
conducted prior  to  beginning analyses  of  the  fuel  samples,  it
was not  possible to begin these  analyses before the beginning
of  the already  busy  summer  schedule.   The laboratory  at  the
time,   thought it was  still  possible  to conduct the analyses,
but it eventually became evident  that  the  distillation  analyses
could  not  be completed before  the September 30,  1985 deadline.
Therefore,  an effort  was  made  to locate another fuel  analysis
laboratory,  and one  was   located  in  San Antonio.   With  the
verbal  approval of  the  EPA Project  Officer,  the fuels  were
delivered  to that  laboratory  for  distillation  analyses  on a
rush   basis.    A   question   has   become   evident   on   the
reproducibility of the  two instruments used,  relative to one of
the control  fuels.  Due to the September 30 deadline,  however,
it  was not possible  to incorporate any  additional evaluations
in  an attempt  to  resolve the question.   It also  should  be
pointed out that the ASTM is reviewing the precision  for ASTM
D86,  and  that it is  not  clear how to specifically apply the
given precisions to the data generated.

     The   results   from   the  analyses  of   control   and  the
additional  fuel  sample   (SwRI  Fuel  EM-616-F)   are given  in
Appendix  D,  and are   summarized in  Tables   15 and  16.   The
repeatability between duplicate injections  for Control  fuels 1
and 2  were within the guidelines in the Quality Assurance Plan
for 19 out of 20 analyses  (95 percent).   Duplicate  distillation
analyses   were   not.   performed   on   fuel    EM-616-F.    The
reproducibilities of  distillation temperatures  for Controls 1
and  2  on  each  instrument  separately were  also  within  the
quality assurance guidelines.  Reproducibility between  the two
instruments for  Control fuel 1 and EM-616 were  outside  the 95%
guidelines  given by ASTM.  Again, however,  it should be noted
that  the  precision for  ASTM  D86  is  under   review,  and  that
specific applications  of the precision values  given by  ASTM are
not defined.

-------
                                       -22-
             Table 9.   Schedule for  Initial Analysis  of Reference
                               and Control Samples
                                     Number of Evaluations
Sample RVP
Number Automatic
Reference I
Reference 2
(Control 2)
Reference 3
Reference 5a
Reference 5b
Reference 6
Control 1
2b
2

0
0
0
0
2
RVP, ASTM
D323(bomb)
2
2

0
0
0
0
2
Distillation
0
2

0
0
0
0
2
Alcohols*
0:
2

2
0
0
0
2
Water
0
2

0
0
0
2
2
Lead
0
2

0
2
2
0
2
aMethanol, ethanol, TBA
     repetitive analyses

-------
       Table  10.   Results  of  Initial Analyses of Reference  and  Control Sample
Sample RVP, psi
Number Automatic
Reference 1 10. la
Reference 2 10.6,10.7
(Control 2)
Reference 3
Reference 5a
Final analyses
Reference 5b
Final analyses
Reference 6C • —
Control 1 8.8,9.1
RVH, psi Distillation,
ASTM °F at % Evap/ Alcohols, % by vol.
D323(bomb) 10% 50% 90% Methanol Ethanol TBA Water, wt % Lead, g/gal
9.7,9.2,9.3 -- b
10.3,10.6 - — - 5.21,5.16 < 0.1, < 0.1 5.08,5.01 0.037,0.039 < 0.001, < 0.001
<0.l, <0.l 10.1,10.1 <0.1,<0.l
0.07,0.07 jj,
to
1
0.015,0.015
0.0899,0.0830
9.0,9.1 -- - -- <0.1, <0.1 <0.1, <0.l <0.l, <0.1 0.011,0.009 <0.001, 
-------
                                    -24-
   Table 11.  Objectives for Precision, Accuracy,  and  Completeness
Analytical
Procedure

Alcohol
  Content
Distillation

Lead Content

RVP

RVP
                                              Precision3
             Experimental   Repeat-  Reproduo-
Reference     Conditions    ability  ibility.
FID Chroma-  Fuel  Sample
tography
(SwRI)
2.5%b'c'   5%b'c
                               c,e
                                                       c,e
ASTM D86     Fuel Sample

ASTM D3237   Fuel Sample 0.005g/galc 0.01g/galc

ASTM D323    Fuel Sample 0.25 psic'9 0.55 psic'g

Automatic RVPFuel Sample 0.25 psic'n 0.55 psic'9
Instrument
Method
Water Content   ASTM D-1744  Fuel Sample
                               Complete-
                     Accuracy   ness 3
>95%
f
d
d
d
>95%
>95%
>95%
>95%
                                                            >95%
.The ASTM defines precision  in terms of repeatability and reproducibility.
 The percents given are  percents of the measured alcohols content.
 Based on 95% confidence limits  (i.e., 19 out of 20 measurements should
 ,be within the limits given) .
 vChe measured concentration  for the blended standard solution should be within
 five percent of the concentration to which it was blended.
 Repeatability and reproducibility are given in Fig. 2 and Fig.  3 in
 ASTM D86;  these criteria can not be reduced to only a few numerical
f values.
 Accura'cy is obtained through procedural operating requirements  (i.e.,  by
 following the procedure ) .
u    samples having an RVP  of 0 to  15 psi.
 The Automatic RVP Instrument Method is designed to be an efficient re-
 placement to the ASTM D323 method  and has the same precision given for
.ASTM D323.
.The precision has not been determined for use with gasoline samples.
 Unless stated otherwise  in a specific work plan, the objective for com-
 pleteness will be 95%, or  better.
 To be determined.
   Reproduced  from  section  3E  of  Quality Assurance  Project  Plan
   for this  contract.

-------
   Table 12.   RVP of Control  Fuel  Samples  as Measured by two  Methods


                        Control 1—Unleaded Indolene               Control 2—Indolene-Alcohol Blenda
Auto., psi
1 2
Initial - first set 8.8 9.1
- repeat
Later repeat -9.1
Between batches
land 2 8.9 8.9
Between batches
2 and 3 9.0 8.8
Between batches
3 and 1 8.7 8.9
Between batches
4 and 5 8.4b 8.4b

Between batches
5 and 6 8.9 9.2
Between batches
6 and 7 8.9 8.9
Between batch
7 and reruns
from batch 5C 8.9 9.0
Avg.
i
AVR.
9.0

9.1

8.9

8.9

8.8

8.4


9.0

8.9


9.0
8.9
Bomb, psi
1 2 AVR.
9.0 9.1 9.1 '

9.4 9.4
.
8.9 9.0 9.0

9.0 8.9 9.0

8.9 8.8 8.9

8.3b 8.lb 8.2b


8.9 9.0 9.0

8.8 9.0 8.9


8.9 8.9
8.9
Auto, psi
1 2
10.9 10.9
10.6 10.7
10.5

10.6 10.5

10.5 10.4

10.5 10.3

10. 2b 10.3


10.6 10.6

10.6 10.5


10.6 10.6


AVR.
10.9
10.6
10.5

10.6

10.4

10.4

10.3


10.6

10.6


10.6
10.5
Bomb, psi
1 2 AVR.
10.6 10.8 10.7
10.3 10.6 10.4
10.5 10.5

10.5 10.5 10.5

10.4 10.4 10.4

10.4 10.4 10.4

10. 0>> 10.lt> 10. 1


10.5 10.5 10.5

10.5 10.5 10.5


10.4
10.4











1
10
Ul
1







aFive percent methanol and five percent TBA (by volume) added to unleaded indolene
bThese RVP values were outside the reproducibility specification of 0.6 psi.
 The two cans of fuel samples were discarded and fresh samples were analyzed
 for the remaining analyses.
c£very fifth sample of the fifth batch was reanalyzed with the fresh standard

-------
                                   -26-



           Table  13.  Alcohol Content  of Control Sample  2*



                  	Alcohol Content in Percent by Volume	
                       Methanol            Ethanol             TBA	
                  ~T"   "T""   Avg.    "T~   T~      1       2~   AvgT
Initial
  First set         5.21   5.16    5.2     0.0    0.0    5.08   5.01    5.0

  Later repeat      4.86           4.9     0.0           4*68           4.7

Between batches
  land 2          4.95   4.96            0.0    0.0    4.73   4.74
Repeat            4.86           4.9     0.0           4.65           4.7

Between batches
  2 and 3          4.85   4.85            0.0    0.0    4.68   4.65
Repeat            5.13           4.9     0.0           4.89           4.7

Between batches
  3 and 4          5.08   5.11            0.0    0.0    4.87   4.88
Repeat            4.95           5.0     0.0           4.78           4.8

Between batches
  4 and 5          4.93   4.92    4.9     0.0    0.0    4.76   4.76    4.8

Between batches
  5 and 6          4.87   4.87    4.9     0.0    0.0    4.53   4.51    4.5

Between batches
  6 and 7          4.89   4.91    4.9     0.0    0.0    4.54   4.55    4.6
After batch 7
Repeat
Later repeat






5.02
5.01
4.90
4.86
4.98
4.98
4.93
4.86

5.05
5.02 5.0
4.85
5.01
.4.89
4.86
5.01
4.9
Avg. ' 5.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0


0.0
0.0
0.0
0.0
0.0
0.0



4.66
4.65
4.84
4.77
4.85
4.88
4.87
4.75

4.68
4.64
4.77
4.88
4.80
4.83
4.87

Avg.

4.7





4.8
4.7
        sample 2 is unleaded Indolene with 5 percent methanol and
 5 percent TBA added (by volume)
bAbout 40 percent of the values varied over 0.25 volume percent from
 the five volume percent TBA that was added.  See text for pertinent
 discussion
C0.0 means <0.1%

-------
                                 -27-
        Table 14.  Water Content  of Control Fuel Samples
                               Water Content in Weight Percent
Initial
     First set
     Later repeat

Between batches
   1 and 2
Repeat

Between batches
   2 and 3
Repeat

Between batches
   3 and 4
Repeat

Between batches
   4 and 5
Repeat

Between batches
   5 and 6

Between batches
   6 and 7

After batch 7
                           Control 1
                        Unleaded Indolene
                       1
                 Avg.
0.011   0.009   0.010
0.007   0.009   0.008
0.025   0.024   0.02*
0.009           0.009
0.029   0.030   0.030
0.039
0.032
0.025
0.030
0.031
0.032
0.035
0.032
0.031
0.028   0.02*   0.026
0.033   0.030   0.032

0.03*   0.03*   0.03*
        Avg.     0.02
                                  Control 2
                               Unleaded Indolene
                            +5% Methanol +5% TBA
  1
AYR.
0.037   0.039   0.038
0.087   0.093   0.090
0.107   0.121
0.120           0.116
0.1*2   0.132
0.139           0.138
                            0.103   0.103   0.103
                            0.108   0.126
                            0.117           0.113
0.10*   0.108   0.106
0.125   0.127   0.126

0.152   0.1*9   0.150
        Avg.      0.1

-------
Table 15.   Distillation Temperature Repeatability of Control Fuels

Temperature Difference at Percent Evaporated, °F
Control
Fuel Instrument IBP 5% 10% 15% 20% 30% 40% 50% 60% 70% 80%

1 1 43331322223
2 1 33321231233
1 2 344b3333334b3
2 2 5,21221112 24b
Precision for ASTM D86 is under review.
Indications are that precision for IBP and EP may be indeterminate.
"One °F above values given in guidelines
CTwo or more °F above values given in guidelines
dASTM D86 bases the repeatability guidelines on 95% probability
and makes the statement given in the preceeding note a.
Table 16. Distillation Temperature Reproducibility
Temperature Difference at Percent Evaporated, °F
Control
Fuel Instrument IBP 5% 10% 15% 20% 30% 40% 50% 60% 70% 80%
Guidelines in ASTM D86a '12 10 76666 66 6 7
1 1 7667b6744«69C
2 1 45533432454
1 2 76 8b 43343343
2 2 5643334 56 7b8C
I 142 12 I8C I8C I3C 9C 7b 5 6 6 10^ I|C
2 142 5664344 567b8b
616 142 39 IOC 8C IOC IOC 2 56 3 7
'Precision for ASTM D86 is under review.
Indications are that precision for IBP and EP may be indeterminate.
"One °F above values given in guidelines
cTwo or more °F above values given in guidelines
dASTM O86 bases the repeatability guidelines on 95% probability
Number of Values
Above Guidlines
Acceptance
90% 95% EP Observed Basis*. d

3 8C 2 1 3
132 0 3 to 4
1 2 8c>d 2 1 to 2
3 3 6b>d 2 1 to 2


of Control Fuels
Number of Values
Above Guidlines
Acceptance
90% 95% EP Observed Basis3' d
10 13 10
6 |4b I2C 0 5 to 6
553 4 7
128 1 3
4 5 "6 ' ' 2 3
9 |4b 28C 30 8 to 9
777 2 12
I3C 9 |6<: 7 5 to 6












1
to
00
1












-------
                              -29-

V.   COMPARISON WITH MVMA SURVEY DATA

     ASTM guidelines  indicate that  the  samples from  Baltimore
should be  class C  in September while  those  from Detroit  and
Philadelphia  may be  either  class  C or  D.   There  are  some
samples of  Oxinol  which were  collected  from  ARCO stations  in
Philadelphia which  are  examined separately here.  The data are
further stratified  by the type  of petroleum  company,  that  is
whether  it  is  a  regional   (e.g.,  small  or  independent)  or
national company as listed in the report.

     MVMA  does  not  take  samples  in  September,  so   direct
comparisons with MVMA data for the same  month and city  are not
possible.   However,  it  is possible  to  compare  the  results  in
this study with the data in  the MVMA national survey  for fuels
with the same ASTM  class.  The distributions of the RVP,  lead,
methanol,  ethanol,  and  butyl alcohol within the groups  of data
were compared  to MVMA  survey data  from June  and December  of
1984.   The   MVMA  data   used  for   the  comparison   to  the
Philadelphia and Detroit  distributions  include all fuels taken
from class C or D  areas/seasons.  The data from the  two  classes
are simply combined for  all  of the parameters except  RVP.   RVP
is the parameter most likely to be affected by  the ASTM class.
The comparison  between  the RVP data taken  in this program and
that of  the MVMA  survey is  shown by  the histograms  in figure
3.  The data  used  for the comparison  to the  Baltimore  samples
include only  fuels  from class C areas/seasons.  These analyses
show that  the distributions  of  measurements from the national
companies  were  distributed   roughly  equally  to  those   of  the
regional companies,  except as noted.

RVP
           The  Baltimore samples have RVP's  which  were slightly
     higher  than  those  of  the  class  C  fuels  in  the  MVMA
     surveys.    Ninety percent of the Baltimore  samples  fall in
     the range  of 10.4  - 12.6 psi;  ninety  percent of the MVMA
     class C  fuels  fall in  the  range of  9.5  - 12.0  psi.   The
     RVP distributions of the Detroit and Philadelphia  samples
     (not  including  the Oxinol samples  which were  taken  in
     Philadelphia)   fell  between  the distributions  for  class  C
     and class  D, but they were closer to that of  class  D.  The
     ninety percent range for these two cities  is 10.6  - 13.4
     psi.    The  Oxinol  samples  had higher  RVP's,  ranging from
     12.7-13.7.

Lead
           The  lead  levels  found in the  samples taken  by SwRI
     are close  to but slightly higher than  those  found  in the
     MVMA survey.

-------
Sample  Distribution





OB
PI

ft
H-
B
n
at










^j
o>
ft
n
H-
ft








^x
o
a IS
M" £T
O M
HJ ft!
a
elphia
Exclud
&
^•*

MIDPOINT
8.8000
9.2000
9.6000
10.000
10.400
10.800
1 1 .200
1 1 .600
12.000
12.400
12.800
13.200
13.600
14.000
14.400
14.800
MIDPOINT
8.8000
9.2000
9.6000
10.000
10.400
10.800
1 1 .200
1 1 .600
12.000
12.400
12.800
13.200
13.600
14.000
14.400
14.800
15.200
MIDPOINT
8.8000
9.2000
9.6000
10.000
10.400
10.800
1 1 .200
1 1 .600
12.000
12.400
12.800
13.200
13.600
14.000
14.400
14.800
15.200
National
Brands
0 +
0 +
0 +
0 +
1 +X
0 +
7 tXXXXXXX
0 +
1 +X
1 +X
0 +
0 +
0 +
0 *
0 +
0 +
0 +
0 +
0 +
0 +
1 +X
0 +
4 +XXXX
0 +
1 +X
0 +
1 +X
0 +
0 +
0 +
0 +
0 +

0 +
0 +
0 +
0 +
0 +
1 +X
0 +
2 +XX
2 +XX
0 -i-
J +X
1 +X
0 +
0 *
0 *
0 +

Regional
Brands
0 +
0 +
0 +
0 +
6 +XXXXXX
1 1 +XXXXXXXXXXX
2 +XX
6 +XXXXXX
1 +X
1 +X
2 +XX
0 +
0 +
0 +
0 +
0 +
0 +
0 +
0 +
0 +
1 +X
1 +X
2 +XX
4 *XXXX
8 +XXXXXXXX
6 +XXXXXX
2 +XX
5 +XXXXX
0 +
0 +
0 +
0 +

0 +
0 +
1 +X
0 +
1 +X
1 +X
4 *XXXX
4 +XXXX
9 +XXXXXXXXX
6 +XXXXXX
2 +XX
2 +XX
0 +
0 +
0 +
0 *



2 +X,
3 +x:
14 +x;
16 +x:
21 +x;
27 +x;
40 +x;
38 +x:
12 +x;
4 +x;
1 +X
1 +X
1 +X
0 *
0 *
0 +
2 +Xi
3 +x;
14 -t-x;
16 +X)
21 +X)
27 +X)
40 +X)
38 +X)
12 +X)
4 +X)
1 +X
1 +X
1 +X
0 +
0 +
0 +
0 +
2 +XJ
3 +X>
14 +X)
16 +X>
21 +X>
27 +X)
40 +X>
38 +X>
12 +X>
4 +X>
1 +X
1 +X
1 +X
0 +
0 +
0 +
0 +
Figure  3.   Histograms of  RVP

                         MVMA Reference  Distributions
                                      Class C
                                                          Class D
                             +XXXXXXXXXXXXXX
                             +XXXXXXXXXXXXXXXX
                             +XXXXXXXXXXXXXXXXXXXXX
                             +XXXXXXXXXXXXXXXXXXXXXXXXXXX
                             +XXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXX
                              xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx
                             +XXXXXXXXXXXX
                              xxxxxxxxxxxxxx
                          16- -t-XXXXXXXXXXXXXXXX
                          21  +XXXXXXXXXXXXXXXXXXXXX
                              xxxxxxxxxxxxxxxxxxxxxxxxxxx
                          40  +XXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXX
                          38  +XXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXX
                            +XXXXXXXXXXXXXX
                            +XXXXXXXXXXXXXXXX
                             xxxxxxxxxxxxxxxxxxxxx
                            +XXXXXXXXXXXXXXXXXXXXXXXXXXX
                            -t-XXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXXX
                             xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx
                             xxxxxxxxxxxx
                                               0 +
                                               0 +
                                               0 *
                                               0 +
                                               1 +X
                                               2 +XX
                                               2 +XX
                                               5 +XXXXX
                                               16 +XXXXXXXXXXXXXXXX
                                               26 +XXXXXXXXXXXXXXXXXXXXXXXXXX
                                               24 +XXXXXXXXXXXXXXXXXXXXXXXX
                                               23 +XXXXXXXXXXXXXXXXXXXXXXX
                                               12 +XXXXXXXXXXXX
                                               0 +
                                               1 +X
                                               1 +X
                                               1 +X
 0
 0
 0
 0
 1
 2
 2
 5
16
26
24
23
12
 0
 1
 1
 1
                                                                                                 o
                                                                                                  I
                                                 +X
                                                 +XX
                                                 + XX
                                                 +XXXXX
                                                 +XXXXXXXXXXXXXXXX
                                                 +XXXXXXXXXXXXXXXXXXXXXXXXXX
                                                 +XXXXXXXXXXXXXXXXXXXXXXXX
                                                 +XXXXXXXXXXXXXXXXXXXXXXX
                                                 +XXXXXXXXXXXX
                                                                     +X
                                                                     +X
                                                                     +X

-------
                              -31-
Methanol
           Less than  0.25%  methanol is  found  at  the  ninety
     fifth percentile in  all of the  groups  except the  Oxinol.
     The Oxinol samples  have roughly four  percent  methanol.

Ethanol
           One of  the seven national samples  taken in  Detroit
     had  7.7%  ethanol.    Eleven of  the  twenty  nine   regional
     samples had  approximately 9% ethanol.  None of the other
     samples  contained  significant  amounts  of  ethanol.   The
     MVMA  survey  shows  only small amounts of ethanol (0.1%)  at
     the ninety-fifth percentile.

Butyl Alcohol
           Small  amounts   of butyl  alcohol  (up  to  0.6%)  are
     present in many  of  the samples measured by  SwRI.    One  of
     the national brand samples from Philadelphia contains 2.1%
     butyl alcohol, and one  of  the regional  brand samples  from
     Philadelphia  contains  1.6%.    The  samples of Oxinol  have
     roughly 3.7%  butyl  alcohol.   The  rest have levels  below
     1%.   The MVMA  survey  reports  no  more  than  0.1%  butyl
     alcohol at the ninety-fifth percentile.

-------
APPENDIX A



  Work Plan

-------
SOUTHWEST  RESEARCH  INSTITUTE
POST OFFICE ORAWEB 28610 • 6220 CULEBRA ROAD • SAN ANTONIO. TEXAS. USA 78284 • (512) 684-8111-TELEX 76-7387
ENGINES. EMISSIONS AND VEHICLE RESEARCH DIVISION
TWX: 91047MOM
                            March "19', 1-985
 TO:        Mr.  Albert W. Ahlquist, Contracting Officer
           Contracts Management Division
           Contracts Branch A
           Environmental Protection Agency
           Cincinnati, OH  45268

 FROM:      Charles M. Urban and Charles T. Hare
           Department of Emissions Research
           Southwest Research Institute
           6220 Culebra Road
           San  Antonio, TX  78284

 SUBJECT:   Revision B to the Work Plan in response to Work  Assignment  No.  8 of
           Contract 68-03-3192, received by SwRI on  December 20,  1984
           and  revised by verbal technical directives in  February and  March
           1985;  SwRI Project 03-7774.

           Contract Title:      "Pollution Control Assessment for the
                                Emission Control Technology Division,
                                Aon Arbor, Michigan"

           Assignment 8 Title:  "Analysis of Fuel Samples"   (Analysis
                                of In-Use Gasolines  and Gasoline/
                                Methanol Blends)

 I.    INTRODUCTION

      Southwest Research Institute will comply with  the revised technical
 and quality assurance (Q/A) type requirements of Work  Assignment Number 8,
 and will  put forth efforts to do so within the 1985 fiscal year.  It  will
 be  necessary,  however, to coordinate this effort with  analyses of fuel
 samples from MVMA and other currently scheduled fuel surveys.   The initial
 Scope  of  Work  for Work Assignment Number 8 is attached as  an Appendix for
 information purposes.

 II.   STATEMENT OF TECHNICAL APPROACH

      This Work Plan describes the manner in which our  understanding of
 the  requirements will be met.  Should there be a necessity for changes in
 the  Work  Plan  which are within the level of effort  proposed, they can be
 documented in  a letter or a monthly progress report.

      A.   Gasoline and Blend Analysis

           The  following analyses will be performed  on  each of  the one
 hundred thirty (130) gasoline samples collected from three cities under
           SAN  ANTONIO,  TEXAS
           WITH 0 » * i c « s IN  HOUSTON. T e x A s . AND WASHINGTON, o c
                                  A-2

-------
Work Assignment No. 14 of Contract 68-03-3162,'and on selected  reference
and control samples:

          1.  RVP - Automatic B.VP Instrument Method.  The
              Automatic KVP instrument developed at SwBI
              is used to analyze all MVMA survey samples.

          2.  Distillation - ASTM D-86.

          3*  Jfethanol, Ethanol, and Tertiary  Butyl Alcohol
              (Volume Percent) - Water Extraction/Gas Chroma-
              tography.  This SwRI-developed analytical pro-
              cedure is based on extraction of Che gasoline
              with 2 volumes of water and gas  chromatography
              of the extract using a flame ionization detector.

          4.  Water (Weight Percent) - ASTM D-1744, Karl Fischer
              Titration.

          5.  Lead Content (Weight *) - ASTM D-3237, Atomic
              Absorption Spectrometry.

          6.  FE7I and El volatility indices - In accord with the.
              Statement of'Work*, no calculations of indices have
              been Included in this Work Plan.

          The procedures described are the same as were previously used •
in the  fuel analyses conducted under Work Assignment No. 14 of  EPA Con-
tract No. 68-03-3162.  They were reported in the  final report EPA 460/3-
84-009.

     B.   Discussion of the Procedures and Q/A

          The ASTM maintains system accuracy by equipment  calibration
and/or  by Internal standards as appropriate to the specific analyses.
This approach is essentially the same as used  in Che Code  of Federal
Regulations  for emissions measurements.  The quality assurance  guide-
lines  given  in  QAMS-005/80 and in referenced handbooks and manuals are
specific only  for  environmental measurements.  A major difficulty relative
to chis Work Assignment has been chat definitive  guidelines  for applying
EPA QA requirements to  fuel.analyses were not  available.

          The ASTM incorporates quality control into its procedures, Co
Che maTrinrnm  extent  they consider co be practical  for widespread use.
When attempting co  apply Section 5.11 of QAMS-005/80 co a  project,
several questions  arise:

          • What specific level of control is  essential?

          • Who is co decermine level of concrol applied?

          • Is  che same level of concrol co be applied to  all analyses?.

          • What degree of quality assurance is co be applied Co  che
            reference standards used?

                                 A-3

-------
The Initial approach taken in developing this Work Plan was  to  attempt
to provide an adequate response without having  definition  of the specific
requirements.  This revision Incorporates the specific requests from the
EPA Project Officer.

     C.   Test Plan - Including Quality Control and  Assurance Provisions

          As has been decided, several specific quality control and-
assurance efforts have been incorporated into this Work. Assignment.   The
revised test plan incorporating those provisions is  as follows:

          1.  Obtain or  develop reference fuel  samples ("to determine
              procedural accuracy and repeatability):

              •RVP - Fuel Rl - pure grade  2,2-dimethybutane
                                (Neohexane), 9,9 psi at 100° F

              • Distillation - none  (D86 provides empirical results)

              • Alcohols - Fuel H2 - 5% pure grade methanol and 5%
                                     pure grade TBA  in unleaded Indo1ene

                           Fuel R3 - 10% pure grade  ethanol in  unleaded
                                     Indolene

              • Water content - Fuel R4 - Fuel  R2 plus 0.100 weight
                                          percent water

              • Lead content - Fuel  R5 - Reference  samples from the  EPA

          2.  Develop control fuel samples  (run periodically for
              repeatability and reproducibility) :

              • Fuel Cl  - unleaded Indolene

              • Fuel C2  - same fuel  batch as Reference  Fuel R2

          3.  Conduct Reference and  Control Fuel analyses:

              • RVP  (automatic and ASTM D323) - Two  repetitive
                evaluations of the following fuel set - Rl,  Cl, C2

            .  • Distillation" - Two repetitive evaluations  of the
                following" fuels - Q, C2

              • Alcohols - Two repetitive evaluations of  Che following
                fuel set - R3, Q, C2

              -  Water Content  - Two repetitive  evaluations of the
                following fuel set - R4,  Q, C2

              •  Lead Content - Two repetitive evaluations  of the
                following fuels  -  R5, CL,  C2

NOTE:. A third evaluation will be run for any result falling outside the
       Q/A repeatability objectives.

                                A-4

-------
          4.  After accuracy and repeatability have been established,
              evaluate the fuel samples*  To the extent possible,  conduct
              the evaluation in sets per city sampled  (control  fuels to
              be used are Indolene, Cl, and Indolene -I- 5% M&TBA, 02) :

              BALTIMORE  (=40 fuels)

              a.  Check tiae elapsed since last analyses of control samples*

              b.  Analyze 20 fuel samples (without ASTM D323)

              c.-  Replicate tests of control fuels (with ASTM D323)

              d.  Hepeat b and c

              * If over one week, run single test of control fuels (with
                ASTM D323)

              DETROIT («40 fuels)

              Same sequence as for BALTIMORE

              PHILADELPHIA ("40 malors  & minors)

              Same sequence as for BALTIMORE

              PHTT.ATWiPHIA (g10 Oadnol  samples)

              Steps a, b (except only 10 fuel samples), and c of the
              sequence used for BALTIMORE
NOTE:  Run a repeat of any control sample result falling outside the  Q/A
reproducibility objectives.  If-the repeat result is outside  the Q/A
objectives for reproducibility, determine the reason and resolve the
cause-for being outside the control limits.

     D.   Reporting

          Data will be reported in the monthly progress reports in the
form of a complete set of all data for each of the cities in which fuel
samples were taken.  All data generated under this Work Assignment, along
with a Q/A assessment, will be provided as a Submittal of Test Results at
the end of the project.  The format for this submittal will be similar Co
that used in Work Assignment No. 18 under EPA Contract 68-03-3162.  This
submittal will provide a. brief description of what was done and will
report all the data generated.  It is planned to report the data separately
for each of the three cities using the formats previously used in Tables 1

-------
through 3 in the Final. Report  EPA 460/3-84-009.  In accord with the
Statement of Work, no provisions are included in this Work Plan for any
analyses of other than the Q/A results.

III. SCHEDULE OP COMPLETION.

     The Statement of Work for Assignment Number 8 requests a technical
effort period of performance of 3 months.  We project that obtaining the
reference standards, blending .the control fuels, verifying-accuracy and
repeatability, and conducting the analyses of the gasoline and control
samples, will require five months.

IV.  STAFF ASSIGNMENTS                  • .

     The Task Leader and principal investigator of the Division 08 effort
called for in Work Assignment No. 8 will be Kathleen M. Olson.  Project
Manager is Charles T. Hare of the Department of Emissions Research, and
the Division 03 Task Leader will be Charles M. Urban.

V.   PROJECTED LABOR HOURS BY CATEGORY AND OTHER DIRECT COSTS

     Based on our understanding of the requirements of the Work Assignment,
we project the following breakdown of employee utilization by category:

               Labor Category         Div. 03 Employee Hours Projected

          Professional Level 4                        6
          Professional Level 3                       12
          Professional Level 2                       40
          Professional Level 1                       16
          Senior Technical                           16
          Technical                                  16
          Clerical                                   32
          Laboratory Assistant                        8

                                      .Total         146

     We also project the following other elements of direct cost, not
including fee:

          Direct  Cost Elements        Cost, Exclusive of  Fee

          Fuel Analyses  (Div 08)                $36,456
          Purchased parts and
            supplies                                650
          Photography, report
            services, and com-
            munications

                                      Total
                                 A-6

-------
VI.  SUMMARY

     Southwest Research Institute has replied in accord with our
understanding of Work Assignment No. 8, as revised verbally, Con-
tract No. 68-03-3192, in a full and complete manner.  Should any
technical questions arise, please contact Mr. Hare at Area  Code 512,
684-5111, extension 2646, or Mr. Urban at exntesion 2644..  If  cost
questions arise, please contact. Gerald R, Krisch at extension  2236.
Submitted by:
Charles M. Urban                      Charles T. Hare
Senior Research Engineer              Manager, Advanced Technology
Department of Emissions Research      Department of Emissions  Research
Engines, Emissions and Vehicl'e        Engines j Emissions  and Vehicle
  Research Division                     Research Division
                               A-7

-------
            APPENDIX B



      ANALYTICAL PROCEDURES



B-l  Alcohol Content of Unleaded Gasoline

-------
                             APPENDIX B-l
             ALCOHOL CONTENT IN UNLEADED GASOLINE
% Methanol, Ethanol, and TEA in Gasoline
     An internal standard, isopropanol, is added in known concentrations, along
with a pre-determined volume of gasoline sample, to distilled  water.  The
alcohols present in the gasoline are extracted with the distilled water and the
extract is introduced into a gas chromatography column.  The eluted alcohols
are detected by a flame ionization detector and peak areas are measured with
an integrator. The peak areas are applied to the appropriate calibration curve,
from which the volume percent is obtained.
Method
     1.   Insert the column  for alcohols in  side "A"  of  G.C.  - Column-SS
          Porapak QS 80-100 mesh.
     2.   Set instrument on FID.
     3.   Carrier gas is helium - Auxiliary gases are hydrogen and air to light
          the detector.
Conditions
     He - Carrier gas           25 cc/min at 60 psi
          Hydrogen            30 cc/min at 13.5 psi
          Air                 250 cc/min at 28 psi
Temperature
     Oven 175°C
     Injection Port 200°C
     Detector 250°C
Integrator
FID
     Delay - off
     Stop - 5 min.
     Area reject - 100 - (102)
     Chart Speed - 1 cm/min
     Slope Sens. - 1.00
     Attenuation  - 64
     Range - 10
     Single Channel
     Atten. set on integrator
     Zero - as needed for baseline
     A & B side (not Diff.)
                                     B-2

-------
                        APPENDIX B-l (CONPD)
Sample Size

     0.75 u
     1.    Light detector and wait  15 min for instrument to stabilize.  During
           this period make up standard and extract the sample and standards.

Standard Preparation

     Stock  Standards - all of the  standards must be  extracted  before being
     injected.

                Std. Cone.      MeOH. ETOH. & TBA

                   0.0%                 -
                   0.1%                 25  y£
                   0.5%                 125  y£
                   1.0%                 250  y£
                   3.0%                 750  y£
                   5.0%               ,1250y£
                   7.0%                1750  vi
                  10.0%                2500  yJl
                  12.0%                3000  yZ

                Dilute to 25 m£  with Indolene.
Extraction of Alcohol - for Std. 
-------
                       APPENDIX B-l (CONPD)

Notes

     Do not use acetone to clean the syringe between samples - use the next
     sample to be injected and rinse the syringe 4-5 times before injecting the
     sample.
                                   B-4

-------
                            APPENDIX B-2
                AUTOMATIC RVP INSTRUMENT METHOD

        (Excerpts from the Maintenance and Operating Instructions)
                            DESCRIPTION

     The  Reid Vapor  Pressure  Instrument operates automatically  - after
sample loading - to determine the Reid Vapor Pressure of gasolines and other
hydrocarbons. The instrument reproduces manual ASTM test data.*
              CALIBRATION PROCEDURES, FULL RANGE

     This instrument measures the vapor pressure in psia of  hydrocarbons at
100°F, expanded to five times its liquid volume.  An equation relating absolute
pressure to Reid Vapor Pressure has been developed by computer analysis of
instrument data  versus ASTM 0-323 data for a large number of hydrocarbon
samples.  The instrument zero and span controls have been adjusted to convert
absolute pressure signals from the pressure transducer to equivalent RVP values
for the direct display of RVP on the meter.
                             OPERATION

     Sample handling, including filling the sample cup, follows the ASTM D-323
procedure - except the cup is kept dry. (No water can be permitted in the
sample or sample system, and the sample need not be air-saturated).

     The cup containing the sample is coupled to the instrument inlet fitting,
and a push-button "start" switch is momentarily depressed. The start light wUl
illuminate.   At the  end  of 4 minutes, this light will go out, indicating
completion of the analysis. The RVP value for the sample will be locked on the
digital panel meter and may be read and recorded anytime before starting the
next test.

     Depression of the "start" switch provides the impulse to start a ^-minute
cycle.  The timer operates to produce the required analysis program.
*ASTM Method D-323, "Test for Reid Vapor Pressure of Petroleum," Part 23 of
ASTM Book of Standards. •
                                  B-5

-------
     APPENDIX C



Fuel Sample Identification

-------
           TABLE C-l.  FUEL SAMPLE IDENTIFICATION
Baltimore
Sample
Number
1
2
3
4

5
6
7

8

9
10
Fuel
Type
R
R
R
P

R
R
R

P

R
R
Fuel
Brand
Amoco
ARCO
BP
Exxon

Getty
Gulf
Mobil

Shell

Sunoco .
Texaco
MAJORS
Gas Station Address.
Gallagar's Amoco
5931 Balto National Pike
Reedy Interprise
7001 Liberty Rd.
Corbin Auto Repair
18830 York Rd.
Eastern Ave. 
-------
TABLE C-l (CONTD). FUEL SAMPLE IDENTIFICATION
Baltimore
Sample
Number
1*

15

16

17

IS

19

20

21

22

23

24

25

26

27
Fuel
Type
R

R

P

R

R

R

R

P

R

R

R

P

R

R
Fuel
Brand
Crown

Crown

Crown

Citgo

Merit

Crown

Hess

Crown

Crown

Crown

Crown

Merit

BP

Crown
MINORS
Gas Station Address-
Hillendale Crown
6819 Lock Raven Blvd.
Orleans Crown
1920 Orleans St.
Perry Hall Crown
8644 Belair Rd.
Marco Citgo
9301 Liberty Rd.
Merit Reisterstown
5128 Reisterstown Rd.
Charring Cross Crown
5217 Balto National Pike
Ken's Hess
9715 York Rd.
Catonsville Crown
500 Frederick Rd.
Ed's Crown
4500 W. Northern Pkwy.
Merritt Crown
1521 Merritt Blvd.
Towson Crown
935 York Rd.
Charles St. Merit
1801 N. Charles
Calvert's BP Station
8716 Liberty Rd.
Rodgers Forge Crown
                    7210 York Rd.
                      C-3

-------
TABLE C-l (CONPD).  FUEL SAMPLE IDENTIFICATION
Baltimore
MINORS
Sample
Number
28
29
30
31
32
33
34
35
36
37
38
39
Fuel
Type
R
R
R
R
R
R
R
R
P
R
R
P
Fuel
Brand
Merit
Citgo
Citgo
Citgo
BP
No Brand
Big Red
Crown
BP
Seven-Eleven
Merit
Crown
Gas Station Address
Merit Franklintown
510 Franklintown Rd.
Whiz Milford Car Wash <3c Citgo^
8120 Liberty Rd.
Whiz Dolfield Car Wash <5c Citgo
3321 W. Colespring La
Fell Pt. Auto Repair
1500 Eastern Avenue
Jimen Enterprises
8913 Belair Rd.
Racetrac
8235 Eastern Ave.
Big Red Compass
1 Compass Rd.
Tony's Crown
8623 Lock Raven Blvd.
Weddmpn BP Gas 
-------
TABLE C-2. FUEL SAMPLE IDENTIFICATION
Detroit
Sample
Number
40
41
42
43
44
45
46
47
48
49
50
51
52
Fuel
Type
R
R
R
R
R
•P
P
R
R
P
R
R
R
Fuel
Brand
Boron
Shell
Union 76
Sunoco
Union 76
Amoco
Mobil
Total
No Brand
Speedway
Martin
No Brand
Total
MAJORS
Gas Station Address-
Gas and Go
Harper at Metro Pkway
Richard Aronki Shell
4000 N. Woodward, Royal Oak
Dallas
10350 Woodward at Harmon
Aranki Service
2931 E. Six Mile
Pat's Service
1102 Nine Mile, Hazel Park
Auto Elec. Center
4399 Highland Rd, Pontiac
Tillard's Mobil
Adams at Maple, Birmingham
MINORS
Total
14900 Gratiot
Frank's Full Service
26701 Gratiot, Roseville
Speedway
31015 Hoover & 13 .Mi. Warren
Blue Island Mini-Mart
5938 Michigan (at Joe St.)
You Save - Rubin Service
6641 Michigan Ave. At Clippert
Total #1187
                 Plymouth at Southfield
                  C-5

-------
TABLE C-2 (CONTD). FUEL SAMPLE IDENTIFICATION
Detroit
Sample
Number
53
54
55
56
57
58
59
60
61
62
63
64
65
66
Fuel
Type
P
R
R
P
R
" R
R
P
R
R
R
R
R
R
Fuel
Brand
Total
Total
Speedway
Total
Clark
Citgo
Tulsa
Total
Speedway
Clark
Total
Pennzoil
Clark
No Brand
MAJORS
Gas Station Address
//11601
Wyoming at Plymouth
Total
19018 Woodward at 7 Mile
#2268
22000 Lahser Rd.
Total
27360 Grand River
Clark
27480 W. Seven Mile, Livonia
Phil's Auto Service
29835 W. 8 mi. at Louise
Tulsa
3640 Six Mile, McNichols
Total
15 Mi. <5c Kelly, Fraser
Speedway Service
34977 Groesbeck, Fraser
Clark
30990 Utica Rd., Roseville
Total
12 mi <5c Utica
Pennzoil
DeQuindre at Greig
Clark Super 100
6800 Highland, Pontiac
K&C
                     3910 Grand River, Avery
                      C-6

-------
TABLE C-2 (CONPD).  FUEL SAMPLE IDENTIFICATION
Detroit
Sample
Number
67
68
69
70
72
73
74
75
Fuel
Type
R
P
R
R
P
R
R
R
Fuel
Brand
Gas & Go
Host
Citgo
Martin
Hi-Fy
Clark
Total
Total
MAJORS
Gas Station Address
Gas & Go
3200 W. Warren
Dearborn Wheels
6425 Telegraph, Dearborn Hgts.
Citgo Enterprises
Telephone Rd.
Martin
26050 Ford Rd.
Hi-Fy
34010 Ford
Clark Super 100
111 Middlebelt, Garden City
Total
Cherry Hill and Venoy
Total
                     N. Mill and Wilcox, Plymouth
                      C-7

-------
TABLE A-3. FUEL SAMPLE IDENTIFICATION
Philadelphia
Sample
Number
76
77
78
79
80
SI
82
83
8*
85
86
87
88
Fuel
Type
R
R
R
P
R
R
R
R
R
R
P
R
R
Fuel
Brand
BPOil
Gulf
Amoco
Exxon
Sunoco
Mobil
Texaco
Citgo
Hess
BPOil
Alert
Merit
Hess
MAJORS
Gas Station Address
BP Oil #6896
Delaware Ave <5c Springgarden St.
#00*295*8
*8th 
-------
TABLE C-3 (CONPD). FUEL SAMPLE IDENTIFICATION
Philadelphia
MINORS
Sample
Number
89
90
91
92
93

94

95
96

97
98

99
100

101

102
Fuel
Type
R
P
R
R
R

P

R
R

R
P

R
R

R

P
Fuel
Brand
Hess
Citgo
Golden
BPOil
Seven-Eleven

BPOil

Citgo
Merit

Merit
Hess

Merit
T.F.C.O.

Merit

Hess
Gas Station Address
#3821*
Rt. 202 <5c 422, Norristown
Norristown Citgo
Markley St. <5c Spruce, Norristown
Cinelli's Garage
2501 W. Main St. (Ridge Pk), Norristown
6870 BP Oil Inc.
Rt. 309 <5c Broad St., Colmar (Lansdale)
(7-11) - #20*35
Bethlehem Pk. and Butler, Ambler
#6912
Bethlehem Pk. <5c Penn Ave., Ft. Washington
Citgo Quick-Mart
Easton Rd. and Keswick, Glenside
Merit Self-Serve
Broad St. <5c Godfrey Ave.
Merit Bainbridge
Broad St. & Bainbridge
#38211
Torresdale Ave. <5c Harbison Ave.
Lehigh Merit
Lehigh <5c 5th St.
T.F.C.O. Fuel Co.
4201 Aramingo
Merit Self-Serve
Frankford 
-------
TABLE C-3 (CONPD). FUEL SAMPLE IDENTIFICATION
Philadelphia
Sample
Number
103
104
105
106
107
108
109
110
111
112

Fuel
Type
R
R
R
P
R
R
R
P
R
R

Fuel
Brand
Hess
BPOil
Hess
BPOil
Citgo
Merit
Alert
Merit
Citgo
Wm. Penn

MINORS
Gas Station Address
#38216
Rt. 132 & 513, Bensalem
#6902
7999 Newfalls Rd., Levittown
#38275
Rd. 1 <$c Woodbourne, Langhorne
#6915
St. Rd. 
-------
TABLE C-3 (CONPD).  FUEL SAMPLE IDENTIFICATION
Philadelphia
Sample
Number
116
117
118
119
120
121
122
123
Fuel
Type
R
P
R
R
R
P
R
R
Fuel
Brand
ARCO
ARCO
ARCO
ARCO
ARCO
ARCO
ARCO
ARCO
OXINOL
Gas Station Address
A.M.-P.M. Mini-Market
Broad St. <5c Lehigh Ave.
Blvd. ARCO
Rt. 1 Festrvl Trevose
Paul Lopresti A.M.-P.M. Mini-Market
Passyunk Ave. 
-------
 APPENDIX D



Distillation Data

-------
TABLE D-l. DISTILLATION TEMPERATURES OF CONTROL
IBP 5%
Instrument 1
98 128
95 125
97 131
98 131
95 130
91 129
92 131
O
1 92 129
ho
Instrument 2
86 116
88 113
93 119
90 115
10%
144
142
146
148
146
143
146
146
133
130
138
134
15%
156
153
160
160
160
158
160
160
150
147
152
151
20%
168
167
172
172
171
170
173
172
166
163
166
166
30%
194
196
194
192
194
191
195
198
196
193
193
194
40%
212
214
211
212
211
210
212
214
213
210
209
210
50%
226
227
223
224
223
225
225
227
224
221
221
222
60%
239
239
235
235
238
236
237
238
236
233
234
233
' 70%
254
254
248
250
250
248
250
251
248
244
246
246
80%
279
267
275
274
273
270
278
276
270
267
270
268
90%
322
322
317
319
318
316
321
318
314
314
314
313
95%
349
350
343
343
340
337
351
343
338
338
338
336
FBP
396
394
385
384
385
386
386
388
376
368
374
372
Residue (%)
1.5
1.5
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
Recoverec
98.5
98.0
99.0
99.0
99.0
99.0
98.0
99.0
98.5
99.0
98.0
99.0

-------
                                                 TABLE D-2. DISTILLATION TEMPERATURES OF CONTROL 2
O
lap
5%
10%
15%
20%
30%
40%
50%
60%
70%
80%
90%
95% EP Residue
Instrument 1
99
96
98
95
95
96
97
97
97
97
118
115
120
117
117
115
117
117
117
117
124
123
128
125
124
123
124
124
124
124
132
132
134
132
132
131
131
132
131
131
140
140
141
140
139
138
138
138
139
139
163
161
165
165
163
163
161
163
163
163
195
195
193
196
195
195
195
196
196
196
216
217
216
217
217
218
217
218
217
218
230
230
232
230
230
231
234
233
231
231
243
244
246
244
242
245
246
247
245
245
264
265
268
266
264
267
268
268
267
266
306
307
311
310
311
310
310
311
310
310
335 379 1
333 380 1
335 379 1
338 378 1
337 379 1
335 381 I
337 380 1
338 379 1
337 380 1
337 380 1
Instrument 2
100
100
95
100
118
116
112
114
126
125
122
122
133
131
130
131
141
139
138
138
165
165
163
162
196
197
193
194
218
219
214
215
233
234
228
230
247
248
241
243
270
269
262
266
313
312
309
312
340 -a 1.5
338 376 1
335 374 1
338 380 V
Recovered (%)








     99



     99




     99




     99




     99




     99








     99




     99








     99




     99
                                                                                                                              98.5




                                                                                                                               99






                                                                                                                               99




                                                                                                                               99
                   a No data

-------
                                  TABLE D-3. DISTILLATION TEMPERATURES OF FUEL EM-6I6-F






IBP    _5%.   10%     15%   20%   30%   10%   50%   60%    70%    80%    90%    95%    EP_    Residue (%)     Recovered (%)




Instrument  i



 88    114    127     136    It7    165    186   209   236    263    289    324    350    406         1               99






 90    115    127     135    146    164    188   210   238    264    291    326    352    398        1.5             98






 90    118    130     138    150    172    ~a    207   236    264    296    334    —a    414         I               99






 90    114    128     137    148    168    186   208   237    263    295    327    355    409         1               99






Instrument  2



 90    111    124     132    144    164    186   210   237    262    289    321    346    408         1               99






 91     112    125     133    144    165    188   212   237    264    290    328.   348    401        1.5             98






 89    110    123     133    143    164    187   210   236    263    296    332    354    405         I               98






 91     109    120     130    140    162    186   207   232    261    291    327    350    404         I               99
   a No data

-------