PAGE 4 CONVERTER SURFACE AREA ANALYSIS

teacetensetecetYeaete

atenee

x

tee

0350

tee

0345

tee be ee tee

tee ee

0330

tee

0315
X/VA-X)

0300

+0285

20255

ea
a ee a a es

0240 x +

ate sVeteceetsccateceetecsctaccetecneteasetscectaccetecastecsetocsetessete

2042 2054 086 078 090 +102 2118 126
048 060 072 084 «096 +108 2120

N= 2

Con= 1,000 P/PO
MEAN ST.DEV, REGRESSION LINE RES.NS.

x .08351 04962 X= 5.7103*Y-,08931 0.0000

Y 03026 00869 Y= .17512°X+ .01564 0.0000

VARIABLE 4 P/PO VERSUS VARIABLE 2 X/V SYMBOL=X

Figure B-33. Plot of BET equation versus relative pressure for
Converter A240/0007-A-LL3

B-34


INLET

OUTLET

Figure A-2. X-Ray Radiograph of A246/0092


TABLE 1. LIST OF CATALYSTS FOR EVALUATION

Converter
Number ‘Manufacturer Engine Family Type of Catalyst

A221/0198 Chrysler DCR2.2V2HAC3 Dual biscuit 3W-OX
A221/0310 Chrysler DCR2.2V2HAC3 Dual biscuit 3W-OX
A280/0005L Chrysler ECR2.2V2HAC4 Dual] biscuit 3W-OX
A220/0400 GM D4G3.8V2NEA3 Dual biscuit 3W-OX
A230/0649 GM D1G2,0V2XAJ4 Dual biscuit 3W
A230/0734 GM D1G2.0V2XAJ4 Dual biscuit 3W
A246/0092 GM D1G3.8V2NDA4 Dual biscuit 3W-OX
4240/0007 Ford DFM1.6V2GDK6 Dual biscuit 3W-OX
A240/0270 Ford DFM1.6V2GDK6 Dual biscuit 3W-OX
A254/0037 Toyota DTY2.4V5FBB2 Dual biscuit 3W-OX
A254/0191 Toyota DTY2.4V5FBB2 Dual biscuit 3W-OX


PAGE 4 CONVERTER SURFACE AREA ANALYSIS A240/0270~8-UR UR-2

teeenteccataccetrcceteseetX

oteeee

,
:
:
:

Fe ecctoaneteccataccetncccteseetecvet

~0300
20825
0750
wWV(1-x)
.0875
0800
0525
0450
0375

:
:

ateceateccetesceteccatecccteventeceateccetrscctecsctaccetescete

054 066 .078 2090 2102 4 2126
080 2072 084 098 108 2120

P/PO

MEAN = ST.DEV, REGRESSION LINE RES.MS.
X 08462 = 0351.4 X= 1,2998°Y+ .00339 2486-7
Y ,08249 02691) Y= .76170*X-,00196 1445-7

VARIABLE 1 P/PI) VERSUS VARIABLE 2 X/V ‘SYMBOL=X

Figure B-42, Plot of BET equation versus relative pressure for
Converter A240/0270-B-UR2

B-43


PAGE 4 CONVERTER SURFACE AREA ANALYSIS 4254/01918 (UR-1)

+

:
06s +
.0g0 +

2055

W/V(1-X]
2050
2045

iM
:
:
ca
oan +
.095 +
:

+

YX

030
aatecceteccetvccotoscctesceteccctecceteseatsscetecnetrvcctecestoces
6055 2065 2075 2085 095 2105
050 080 070 080 090 «100 +110
Ne 3
cOR= 9898 P/PO

MEAN ST.DEV. REGRESSION LINE RES.MS,
X 08482 9.03484 X= 1,8581*Y- 00521 6785-9
Y 04845 .01875 Y= .53803*X+ 00282 1965-9

VARIABLE 1 P/PO VERSUS VARIABLE 2 X/V SYMBOL=X

Figure B-53. Plot of BET equation versus relative pressure for
Converter A254/0191-B-UR1

B-54

et ecactaccateccataccetecccteccsteccstaacateccstacveteccatoccetosce

+

+

0115


TABLE 10. QUALITY ASSURANCE OF SURFACE AREA STANDARDS

Standard Standard Surface Measured Surface Percent
Composition Area, m2/g Area, m2/g Difference
Zinc oxide 0.6240.04 0.61 -1.6
Alpha alumina 0.78 NBS 0.73 -6.4
Alumina 1.3940.12 1.38 -0.7
Alumina 3.0440.25 3.21 5.6
Titanium dioxide 7.0520.7 6.97 -1.l
Alumina 14.040.6 14.00 0.0
Graphitized Carbon 71.3 NBS 73.13 2.6
Black

Alumina 81.4%6.2 82.37 1.2
Alumina 265211 220.5 -16.8

Average -1.926.5

19


PAGE 4 CONVERTER SURFACE AREA ANALYSIS © A284/0037-8 (UR-2]
oot F+eeoer eceeteccete, ot
:
078 + :
. xv
: :
072 + :
: :
: :
066 + +
. .
060 + +
XNV(A-K) .
: x :
054 + :
: :
04g + +
. .
: :
04g + ;
: :
038 + +
x :
Y :
090 + +
. erthertl + renee
‘ : 8
080 100 110
Ne 3
COs .9987 p/eo
MEAN ST.DEV. REGRESSION LINE —_RES.MS,
X 08482 03484 x= 1,6183"y-,00504  126E-8
Y 108853 102152 Y= .61769°x+ .00314 4826-9
VARIABLE 1 P/PO ‘VERSUS VARIABLE 2 X/V SyMBOL=X

Figure B-48. Plot of BET equation versus relative pressure for

Converter A254/0037-B-UR2

B-49


PAGE 4 CONVERTER SURFACE AREA ANALYSIS A221/0310-3 (UA-2)

Kat

20975

«0900

0825

XVII)

0750

0675

Pe ee ee oe

+0600

bee ee

0525

0450

/

x

ne ee

a aera

sar ecreteceetaacetocsetensetesestocesTeseatsncstensatescatevestecsetesees

2055 065 075 «085 .095 105 2115
050 .060 .070 +030 .0S80 2100 6140

tog 3
COR= 1,900 P/PO
MEAN ST.OEV. REGRESSION LINE RES.HS,

X 08482 = .03484 X= 1,1699°Y+ 855E-8 126-10
Y 07177, ,02978 Y= .85475*X-730E-8 86E-11

VARIABLE 1 2/P) VERSUS VARIABLE 2 /V SYMBOLSK

Figure B-6. Plot of BET equation versus relative pressure for
Converter A221/0310-B-UR2

B-7


APPENDIX E

BET EQUATION VERSUS RELATIVE PRESSURE
FOR CORRELATION SAMPLES


PAGE 4 CONVERTER SURFACE AREA ANALYSIS A220/0400-A [LL-1)}

+ +

0490

+9455

re eres

0420

.0385
WAX)

Coe Te

0350

20315

.0280

ee ee eee

20245

see ate

.0210 +x +
VivecsetecsctecceteccetecsetesseticcetecstesseteseeTesestecsstessetenens
: 1068 1075 108s 10385 $108 48
.050 .060 .970 .080 .030 100 10
um 3
coa= 9889 P/PO
EAN ST.DEV, REGRESSION LINE —AES.IIS.
xX 08481 03484 X= 2,4164"Y-,90129 S79E-9
Y 103563 lo1aa2 Y= .41374°X+ S4de-G  99E-9

VARIABLE 4 P/PO VERSUS VARIABLE 2 X/V SYNBOL=X

Figure B-13. Plot of BET equation versus relative pressure for
Converter A220/0400-A-LL1

B-14


PAGE 4 CONVERTER SURFACE AREA ANALYSIS 2240/0270-A~LL [{LL~2)

atecentencotecceteccetescctossetocseteccetessatassstessetes
:
: x
.070 +
065 +
060 +
x/VUA=X)
.055 +
: x
.0s0 +
045 +
04g +
:
.035 + y
weeYaetes t+ ecceteccetescetecentesesteccetocsetsccctessetenseteans
‘oda 1054 1068 1078 ‘oso 1102 iia
.048 .080 .072 .084 .086 108 120
Nw O38
cone .9939 i)
MEAN ST.DEV. REGRESSION LINE RES.MS.
X 08482 03514. X= 1,8608°Y-.01317  30GE-7
Y 108255 (01877 Y= .S30819X+ 00783 8B3E-€
VARIABLE 1 P/PO —-VERSUS VARIABLE 2 X/V SYMBOL=x

Figure B-38. Plot of BET equation versus relative pressure for
Converter A240/0270-A-LL2

B-39

Ce ee oe or

+

2128


PAGE 4

etencetascstece

+1875

+1750

«1625

«1500

<NXx

01375

21250

01125

1000

i SR

0875

by

Ne 2
COR= 1.000

NEAN
xX 08351
Y 13933

VARIABLE

oY

CONVERTER SURFACE AREA ANALYSIS

x
a

048

ST.DEV.

1

04962
207222

p/eo

eet,

054 066 2078 080

+ + Feeect + +

ac catecseteseetacceteceeteveet

060 .072 2084
P/PO

REGRESSION LINE RES.HS.

X= .68716°V-,01224 0.0000

Y= 1,4553*X+ .01781 0.0000

VERSUS VARIABLE 2 X/V

A280/005L-A-LL-3

secctecseteces

a ceetaccetaces

102

096 108

SYNBOL=X

+

+

wanoteceetVacate

x

Se er

tees

ee

+

sevetaccetevee >

0114

Figure B-9. Plot of BET equation versus relative pressure for

Converter A280/0005L-A-LL3

B-10

126
120


PAGE 4 CONVERTER SURFACE AREA ANALYSIS A240/0270-B-UR = UR=1

+.

Hone eteccetencstaccetsccetessstucnetecneteccstiscatvsvstevestevecte

x
«1050

20975

0300

0825

WV(1-X)

0750

+
+
+
+
+
+

FO be ee te ee te ee tee ee te ee te eee te eee tee

.0875
.0600 +
«0525 +
0450 x +
ete eeVteewetesnet
1.042 1084 .
048 -060 .072 084 +096 108 120
Ne 3
CoR= ,9998 P/PO

MEAN ST.DEV, REGRESSION LINE RES.MS.
xX 08462 = ,03514 X= 1,14539°Y~-,00267 102E-8
Y 07622 «09068 == .87278%%+ 00237 775E-9

VARTABLE 1 P/PO VERSUS VARIABLE 2 X/V SYMBOL=K

Figure B-41. Plot of BET equation versus relative pressure for
Converter A240/0270-B-UR1

B-42


PAGE 4 CONVERTER SURFACE AREA ANALYSIS = A221/0447-A BAND C
aanataccetacsetasceteccctecseteceetassetsscateesstensetecset +oe¥
: xt
21750 + +
.1575 + ;
1400 + i
XVI) :
21225 + +
toga + +
: x :
.DB78 + :
.o700 + x i
.0525 + +
: x :
. a4 .
aeVetovcetevcateccatecceteccetecaateccatecsatacsstoccetscastecsetescetoee
104s 1078 1108 1138 1165 1198 1288
.080 .080 120 .180 .180 240 .240
Ne 4
core 1,000 9/0

MEAN ST.DEV. REGRESSION LINE RES.MS.

X 12178 .07987 X= 1.3488*Y~-,00721 203E-3
Y 09856 .05902 Y= .74081°X+ 00534 112E-9
VARTABLE 1 P/PO VERSUS VARIABLE 2 X/V ‘SYMBOL=X

Figure E-1. Plot of BET Equation Versus Relative Pressure for
Converter A221/0447-A (Powder Sample)

E-2


PAGE 4 CONVERTER SURFACE AREA ANALYSIS A230/0649-A-LL1
ateeneteccetecenteccstecccteccotascatovcetecsetecsetocsetassetuasatesX¥ ts

x
0975

-03900

0825

+ +
+ +
+ +
.0750 + L
XIX) :
-0875 + t
: x :
.o600 + :
.0525 + :
.0aso + :
075+ x ;
tee net eVactenseteccntevceteccetacceteccatevccteccetossstecestocsntescete
toaa 1054 1086 1078 ‘080 1102 ia” "Shed
048 .080 .072 .084 .096 108 120
Ne 3
Cor .9907 P/PO

MEAN ST.DEV. REGRESSION LINE RES.MS.
X 08462 = .03514 X= 1,1154"¥+ 01043 9 457E-7
Y 06654 03121 Y= ,87993°X-,00792  360E-7

VARIABLE 4 P/PO VERSUS VARIABLE 2 X/V SYMBOL=X

Figure B-19. Plot of BET equation versus relative pressure for
Converter A230/0649-A-LL1

B-20


RUN DESCRIPTION:

DATE OF XRAY ANALYSIS
SAMPLE TYFE: BRIQUETTE

AUICAT1 - ALTO CATALYST

04/30/37

SITE (Oi N/A
MISCELLANEOLS INFO! NONE
SAMPLE SEQUENE NU 7
SAMPLE ID ALZ30/0724-B
ELEMENT DETN LIM

NA 0

Mo

AL

Pp

“173412
2742E-OF
OR4E-OS

«S77676E-O3
LIS D4E-O2
572648E-03
B27 9E-O3
345 10SE-02
425 4E-03
aa 3016-03

2LU6S517E
»2O714E-02
SOLS32E-02

TOTAL DETECTED BY XRF

2 SE
Sl4104
~.SATLLIE-04
+» 607008E-02
21623526 -02

»174804E- ot

C-7

SWRI

MO CLE-O,:
SL 2416-02



12

the catalytic activity. Aluminum (Al), silicon (Si), and magnesium (Mg) are major
constituents of the support material, and were not quantitatively determined. The
minor constituents such as sodium (Na), potassium (K), titanium (Ti), iron (Fe),
cerium (Ce), and barium (Ba) were also not quantified. The elements Na, K, and Ti
are present in small amounts from the clays used to make the cordierite ceramic.
Titanium is also probably present in the converters as a whitening agent for the
ceramic substrate. Cerium was added to inhibit the conversion of gamma-alumina
with a higher surface area to alpha alumina with a lower surface area at the
elevated temperatures experienced within the converters, and also to increase the
catalytic activity of the converter when present in concentrations of one percent or
more. Iron was probably from the engine, as a wear product, the exhaust system
due to rust, or as an impurity in the ceramic substrate. Barium was also found in
some of the samples.

The samples were prepared by grinding the entire pieces to a coarse powder
(approximately 50 mesh). Approximately 10 grams of the coarse powder were taken
and ground in its entirety to a very fine powder (400 mesh). The analysis was
conducted by Dr. Sene Bauman, Element Analysis Corporation. Matrix corrections
and data analysis were performed at Elemental Analysis Corporation and reviewed
by SwRL

The weight percentages of each element are included in Table 6, Where the
concentration of an element was at the detection limit of the analytical procedure,
the word "trace" was used, and an asterisk (*) was used to identify those elements
with concentrations below the detection limit. Table 6 also includes the other
elements found in each sample which were not quantified.

H. X-Ray Fluorescence

In addition to PIXE, a sample from the rear biscuit was also analyzed by x-ray
fluorescence. This technique uses x-rays as the incident radiation rather than
protons to cause the characteristic x-rays to fluoresce for each element. The
samples were prepared using the sample procedure described for PIXE. The samples
were sent to Mr. F:ank Black, EPA, Research Triangle Park, and analyzed by Mr.
Robert Kellog, Northrup Services, Inc. Matrix connections and data analysis were
performed at Northrup Services, Inc. and reviewed by SwRI. The data are
summarized in Table 7, and the individual results are included in Appendix C.

L Miscellaneous

In Work Assignment No. 20 of EPA Contract 68-03-3192, the normalized
weight percent ratios were calculated for P, S, Ca, Mn, Pb, and Si from the
SEM/EDX spectra. Zinc was not included in that work assignment. The data were
resurrected in order to calculate the normalized weight percent ratios for zinc.
Each element was normalized to the aluminum concentration in each sample. The
data are summarized in Table 8,

IV. Quality Assurance and Correlation

The quality assurance plan for this work assignment is covered under sections
1 and 2D-11D of the Quality Assurance Plan for Contract 68-03-3353 "Emission
Characterization ancl Control Studies for ECTD." This document discusses in detail
project organization, responsibility, objectives, procedures, sample custody, control
checks, preventive raaintenance, and other aspects of the program to assure the


Rear lace

Upper Right*

Upper Left

baa

27\\N

\ \\ Lower Right *

Lower Left

PIXE
XRD

Front Face

FIGURE 2. SAMPLE SECTIONS AND SAMPLE LOCATIONS FOR DOWNSTREAM (B) BISCUIT

*Sample location for XRD shown on
lower right quarter for clarity.
Actual sample location from upper
right quarter.


PAGE 4 CONVERTER SURFACE ARGA ANALYSIS A220/0400-A [LL-1,100 NESH)

20825

0750

bee te be eee te

0675

+0800

XN(A-X)

20525

20450

ee a err

0375

.0300

x
/

re ed

x

.0625

0500
ik 4
con= .9990
MEAN ST.DEV.
x .19752 —,07133
Y 04454 —_,02568

VARIABLE 1 P/PO

/

aT

aFeweetenentercateceateseetaeatesaetessetsses sere

«0875 61125, 01375
0750 «1000 21250

P/PO
REGRESSION LINE RES.HS.
= 2.7752*Y— 00608 148E-7
= .35964%X+ 00227 192-8

VERSUS VARIABLE 2 X/V

21525

1500 +1750 +2090

SYNBOL=X

Figure B-16. Plot of BET equation versus relative pressure for
Converter A220/0400-A-LL1 (Powder)

B-17

i ee er

de eee tenee


PAGE 4 CONVERTER SURFACE AREA ANALYSIS  A254/0037-8 [UR-4)

+ + + teneet, +

ateeeeteccatecceteceetevsetocvetencetoccatscvetecvetscsstossatecsetesces

070 +

x

2055

wiI-x)

050

2045

2040

Se te ee tee te ee te ee te ee te ee tee

030

N= 3
CoR= .9898

MEAN = ST, DEV. REGRESSION LINE RES.NS.
X 08482 03484 X= 1,8950°Y+ ,00173 762E-9
Y 04802 02055 Y= .58879*X~,00101 265E-3

VARIABLE 1 P/PO VERSUS VARIABLE 2 X/V SYMBOL=X

Figure B-47. Plot of BET equation versus relative pressure for
Converter A254/0037-B-UR1

B48


RUN DESCRIPTION: AUCATL -— ALITO CATALYST
DATE iF XRAY ANALYSI%
SAMPLE TYFE! BRICUETTE
SITE ID
MISCELLANEGIL
MPLE SECUENTE NU.

AMPLE IL

ELEMENT

NA

Mo

AL

SI

e

CL x

f

cA

TI

v

cr

MN
x
Xx
x
x
x
oa]
x
x
K

HG x

PR

O4/ 20/127

N/A

INF: NONE

ALl1 OL:

DEIN Lim

.115017
2147776
~.164228-0

110024
- 249 3028-02
57401 18~
-487141E-03 —.4146495E-
L427653E-03 13654
«249948 -03

- 202105E-03
527 BGE-O3
3422 16-03
+2441 196-~¢

» S05474E-02

-.170802E-
71147 834E-02

1 405042E- OL

TOTAL DETECTED BY XRF = 44,5413

C-2

SWRI



SOUTHWEST RESEARCH INSTITUTE

POST OFFICE DRAWER 28510 » 6220 CULEBRA ROAD # SAN ANTONIO, TEXAS. USA 78284 @ (512) 684-5111 © TELEX 244846

August 15, 1987

TO: Mr. Craig A. Harvey, Project Officer
Emission Control Technology Division
Environmental Protection Agency
2565 Plymouth Road
Ann Arbor, Michigan 48105

FROM: E, Robert Fanick and Charles T. Hare
Department of Emissions Research
Southwest Research Institute
6220 ‘Culebra Road
San Antonio, Texas 78284

SUBJECT: Final Report for Work Assignment No. B-8, Contract 68-03-3353,
"Catalyst Evaluation (Cert. FY 87)," SwRI Project 03-1193-008

This work assignment was intended to evaluate the condition of catalysts
removed from in-use vehicles. The catalysts were removed by EPA from 1983
Model Year In-Use Technology Assessment (IUTA) vehicles, and one low-mileage in-
use vehicle. Eleven catalysts were analyzed under this work assignment. The
catalysts represented monolith technology. Catalysts used by several different
manufacturers were included in the evaluation, The catalysts were either three-way
or three-way plus oxidation catalysts, with dual biscuits.

This letter report, along with the included data, is intended to be the final
report of the results from the catalyst evaluation testing. It includes all the results
from the laboratory analyses by whole converter x-ray, BET surface area, x-ray
fluorescence (XRF), proton induced x-ray emission (PIXE), and x-ray diffraction
(XRD). Only a brief discussion of the analytical procedure, and no discussion of the
trends observed in the evaluation of each catalyst, is included. A total of 11
converters (4 whole and 7 partial samples) were examined. A list of the converters
evaluated in the program is presented in Table 1. Only two of the converters
underwent whole catalyst x-ray; two had been x-rayed in a previous work assignment
(A254/0037 and A254/0191). Of the eleven converters, two underwent XRF, XRD,
and PIXE of the rear biscuit, and nine received all of the analytical procedures.
Only the rear biscaits were analyzed by XRF. A detailed description of the
laboratory analytical procedures is presented in the final reports for Work
Assignments No. 10 and 17 of Contract 68-03-3162, with the exception of PIXE.

L Laboratory Analysis
The laboratory analysis of the catalyst samples consisted of whole converter
x-ray, BET surface area, x-ray fluorescence (XRF) , PIXE, and x-ray diffraction

(XRD). The catalyst samples were examined as follows:

1. Only whole converters were examined by whole converter x-ray
radiographs.

SAN ANTONIO, TEXAS
DALLAS, TEXAS @ DETROIT. MICHIGAN @ HOUSTON, TEXAS @ WASHINGTON, DC



PAGE 4

0750

20875

0800

WVI-X)

CONVERTER SURFACE AREA ANALYSIS-A230/0177X-A SAMPLE 8

aratoccetoncctecsetocccteveet teeectace

woanteccetevcetascetevos

\

Ce ee ee ee 2 a ard

Pe ee ee ee ce ee eer er ah

.0300 ;
. x .
0225 + +
: Xx :
.o1s0 + ba
¥ acceteanetecceteccetecnetecsetecsetaccetescstacsetecaets sectessetocs
048 ‘075 1108 1138 168 1195 1228
080 .080 120 180 180 210 240
ne4
cone 9885 p/pa
WEAN ST.DEV, REGRESSION LINE —RES.MS,

xX .12178 ,07988 X= 3,4599"Y~,01082 102E-7
Y 03833 02302 Y= .28872*X+ .00377 sSOE-9

VARIABLE

1 -P/PO VERSUS VARIABLE 2 X/V SYMBOL=X

Figure E-5. Plot of BET Equation Versus Relative Pressure for
Converter A230/0177X-A (Powder Sample)

E-~6


Rear Face

\e
\ \ Upper
Upper Left \ Right

LL3 \G

afte )

LL2

—— hw.

u

i NG a

\ ~ Lower Right*

Lower Left LLL y XRD

Front Fece

FIGURE 1. SAMPLE SECTIONS AND SAMPLE LOCATION FOR UPSTREAM (A) BISCUIT

*Sample location for XRD shown on lower ~~
right quarter for clarity. Actual
sample location from upper right quarter.


PAGE 4

CONVERTER SURFACE AREA ANALYSIS-A230/0177X-8 SAMPLE B

oso + 7
: x
ost +
072 +
063 +
VIX)
:
054 +
048 +
.
: x
038 +
: x
027 + /
. /
ome + xX
y a ccetevcstsccetoccetecceteccatesnetescsteccsteccetoceet
104s ‘078 $105 1195 1168
.080 080 120 180 180 210
Ld 4
cons .9988 P/eo
EAN ST,DEV, ‘REGRESSION LINE ——RES.HS.
X 92178 07867 x= -2.7572"7-.00198 2576-7
Y 104488 «102888 Y= .361716X B13E-6 3976-2
VARIABLE 1 P/PO —«-VERSUS VARIABLE 2 X/V SYMBOL

Figure E-6. Plot of BET Equation Versus Relative Pressure for
Coaverter A230/0177X-B (Powder Sample)

CC ee i ee er oe ears


PAGE 4 CONVERTER SURFACE AREA ANALYSIS A221/0310-A ‘LL-1,100 MESH

ceteccetescetaccataccetaceetacvatassataccatacsetecsatesnatessetecne reece

: Y
: a
250 + t
1225 + :
200 + L
WK} t :
175+ +
150 + x +
tes + i
. x7 :
100 + L
075 + / :
wv :
lestessetaces weet ceataceatancaTacnatoae . veceTecesTeseeTeses tenes
foses"""Yaa7s"* 734188" Tiazs"” ""lis]as” “7 14a78""“"laaas
.oseo” «750° 1000"—«t@s6"—Ss S00" =S«750' =. arao
He 4
coR= .9990 P/O

MEAN ST.DEV. REGRESSION LINE RES.IIS.
X 41975207130) X= .87828%Y-.01542 146E-7
Y 415136 208116 Y= 1,13G4*X+ .01781 189E-7

VARIABLE 1 P/PC VERSUS VARIABLE 2 3/V SYMBOL=%

Figure B-4. Plot of BET equation versus relative pressure for
Converter A221/0310-A-LL1 (Powder)


RUN DESCRIFTICNW: ALICATL - AUTO CATALYST =WR1
DATE OF XRAY ANALYSIS! 04/30/87

SAMPLE TYPE: BRIQUETTE

SITE [Dt N/A

MIGCELLANEOUIS (NFCI NONE

SAMPLE SEQUENCE NO.Lt 4

SAMPLE IDs AD40/0007-B-LL

ELEMENT DETN LIM

NA 0 /f1L9US1E-o1
MG «20571 SE:
AL . S7E-O1
‘h . 7E-OL
: ZE-O3
2 2 L707 SE-OL
cL xX -I7SILSE-O 3 7.29 7OLE-O2
i + 2D14E-03 2 F545.

~172475E-0.2 ~7OSLL3E-O1
-174°01E-a3 + 344354
+ 3842541E-03 «44507 2E-

»107255E-02 »Sl0715E-

+ 527627E-03 2704608 2E-02
» 5301 266-03 2390247
» S2532E-03 49758 18-03
+ 2S501SE-08 2104985
27961 5E-03 « SOL6NSE-0 3
+ 273167E-03 2 SIL965E-O1

.2E491S5E-038 —.1032146E-02
»£10L21 26-02 -. 26506E-02
+4A7807E-O2 ~.1421lcE-o2
»651379E-O2 -.141279E-02
-1VS25E-02
»1LL297E-
IE
OTE
+ 2034 25E-02
~ 7414 36-0
lo TLE

TOTAL DETECTED BY XRF = 45.7047

Cc-9


RUN DESCRIPTION: AUCATL
DATE OF XRAY ANALYSIS:
‘SAMPLE TYFE: BRICWETTE

- AUTO
04/30

TE 102 N/A
MTS ELLANEL INFO! NONE
SAMPLE REUUIENLE Ald iu

‘SAMPLE ID: AZHO/ONOSL -B

ELEMENT

x »"30765E-03
»216487E-08
+176364E-03
+» 148437E-023
»S1224E-03
+ V7O4IZE—
+ F212 4E-¢

x
x
x
x
x
x

4 x

2B OX

GA

re

PT

HG XK

PE

TOTAL DETECTED BY XRF =

c-~4

CATALYST

22630526
T4685 74E-02
«1557 346E-O1

SWRI

OL



16

accuracy and precision of the results presented in this report. A listing of
precision, accuracy, and completeness is presented in Table 9. All measurements
are representative of the catalyst properties and conditions being measured.

The Micromeritics Flowsorb II dynamic surface area analyzer was set up to
analyze the catalyst samples "in-house." Two NBS Standard Reference Materials
and seven standards from Duke Scientific Corporation were used to establish the
instrument operatiig range and linearity, as well as confidence in the analytical
procedure. In this work assignment, the surface areas were determined with a
multipoint technique. A curve was established for the various gas concentrations to
determine the calitration knob setting for the instrument (Figure 3). The standards
were analyzed using this technique, and the results are given in Table 10. A plot of
the BET equation versus the relative pressure for the standards is presented in
Appendix D. In general, the standards repeated within the published confidence
limits for the entire range of standards (0.62 m2@/g to 265 m2/g).

In an effort :o correlate the data from this work assignment with previous
work assignments, an alternative procedure for preparing the samples for surface
area was used. The coarse powder (approximately 50 mesh) from ten samples was
analyzed for surface area and compared to the results for the bulk strips which were
cut from the center core of the biscuit and analyzed as a single sample. The results
for the two sampling techniques are presented in Table 11, and the plots of the BET
equation versus the relative pressure are included in Appendix E. The surface areas
for the ground samples were lower in all cases except for A220/0810-A, A221/0447-
A, and A155/0941-1-A. All three of these samples were from the A biscuits. The
A220/0810-A was tae only sample from the group which contained alpha alumina.
The other two catalysts were from Chrysler vehicles. Ground catalyst samples from
the upstream biscut apparently result in higher surface areas than the unground
samples. These results were also observed for front face samples listed in Table 4.
No conclusions can be drawn without additional work to confirm the sources of this
phenomenon.

In an effort tc: demonstrate the precision and accuracy for the XRF procedure,
a sample analyzed in Work Assignment No. 20 from EPA Contract 68-03-3192 was
selected at random and repeated during this work assignment. The results are listed
in Table 12 and Figure 4. In general, the current results agreed very well with the
previously published results. The largest error was for Ni, but the concentration was
so low that the error does not indicate a significant problem. When Ni is excluded,
the average percent difference is 0.3 43.8. Phosphorus and lead values were higher,
while sulfur and pla.inum were lower. The precision and accuracy for XRF depend
on the concentration of the elements, the elements present, the homogeneity of the
sample, and the size of the particles in the pellet.

Vv. Summary

In summary, a total of 11 catalysts were examined by whole converter x-ray,
x-ray fluorescence, x-ray diffraction, PIXE, and BET surface area analysis. Of
these 11 catalysts, 4 were whole converters and 7 were partial catalyst samples.
This letter report 1s a compilation of all of the data available at the time of
submittal, and is intended to serve as the final report of the results for the program.


PAGE 4 CONVERTER SURFACE AREA ANALYSIS A248/0092-A

sestissctescateccstenccteccstocssteccetunetecastassstevcstecsctesveteves
. . Y
At + Xyr
10 + ;
og + t
og + t
X/V(1-X) .
07 + +
: x :
08 + +
. .
05 + +
: x :
04 + }
. :
03 + +
v stossstessetesseteccetossstecectersstecestecsatessstenes
tosas”” ““taa7s"" “"l44a5°* “"S4a75"" “"Teas"” ““lie7s"” "13928
0500" «.0750'«1000"Ss 1250'S 1500' 1780 = .2000
Ne 4
cORe .9999 P/O
MEAN ST,DEV, REGRESSION LINE —RES,MS.

X 41753 607134 X= 2,0504*y~,00910 156E-8
Y 08176 = 03479 Y= ,48761°X+ .00445 3716-9

VARTABLE

1 P/PO VERSUS VARIABLE 2 X/V SYMBOL=X

Figure B-28. Plot of BET equation versus relative pressure for

Converter A246/0092-A-LL1 (Powder)

B-29


PAGE 4 CONVERTER SURFACE AREA ANALYSIS ALUMINA PART, 1.39 + 0.12

seeet seesteoes Y
.750 + +
675 + L
600 + i
xv(4ex} | :
525 + ;
.4s0 + +
: x :
375+ +
: x :
300 + +
1225 + L
ox :

7

Prceetoceetoee wootsccetvcceteoee
2045 075 105 2135
-080 .080 2120 «150 2180 2210 1240

te 4
coR2 1,000 P/PO
MEAN ST.DEV. REGRESSION LINE —RES.MS.
X 12178 07887 X= .32159"Y-,01600 — 249E-9
Y 48844 24774 Y= 3,1095*%+ .04976 241E-8

VARTABLE 1 P/PO VERSUS VARIABLE 2 X/V ‘SYMBOL=X

Figure D-3. Plot of BET equation versus relative pressure for
Alumina 1.3920.12

D-~4


PAGE 4 CONVERTER SURFACE AREA ANALYSIS A254/0191~-A  (LL~1)

:
056 +
:
.052 +
:
04g +
: x
104g +
XIX)
.040 +
036 +
.032 +
02a +
x
024 +
watecceteccetencatescctescetecsctassetosseteccetonsatescstoccstesseteces
1058 1086 1075 {08s 1055 1105
050 .060 .070 .080 .090 100 110
Ne 3
CoR= .9980 p/eo

MEAN ST.DEV. REGRESSION LINE RES.MS,
x = =,08482 = .03484 X= 2,2188*Y~,00852 198E-7
Y 0420701584 Y= ,44706*X+ ,00415 394E-8

VARIABLE 4 P/PO VERSUS VARIABLE 2 X/V SYMBOL=K

Figure B-49. Plot of BET equation versus relative pressure for
Converter A254/0191-A-LL1

B-50

atecceteccntecceteccetacectoccatossotanentessetecses

.
Mr

:
:
:
:
:
:
:
:


PAGE 4 CORVEFHTER SURFACE AREA ANALYSTS A280/GCOSL-A [LL-1,100 i1ESH}

+

an etecee een eteceeteceateceetavcatascstancatuseetacsaTensetosestscostones

><.

1250

*

tenes

«1925

fea

«1090

a ee as

bene

20875

X/V(1-V)

.0750

-0625

0500

re ee rs

20375

a

205: 98: 21425 212;
0500 0750 «1000 21250
ne 4
com 9998 P/PO
MEAN ST.DEV. REGRESSION LINE RESIS.
X 49752-07432 X= 1,8041*Y-,00539 346E-3
aa 03813 .03952 Y= ,55403*X+ ,00302 106E-8

VARIABLE 4 P/PO VERSUS VARIABLE 2 X/V SYNOOL=

Figure B~10. Plot of BET equation versus relative pressure for
Converter A280/0005L-A-LL1 (Powder)

B-11


PAGE 4 CONVERTER SURFACE AREA ANALYSIS A230/0649-A [(LL-1]
weotece +eenet .
me :
10+ +
.og + +
Vix) > :
ny + +
: :
: x :
a7 + :
0g + +
: x :
.05 + t
04 + J +
Tk :
Vooteccctecacteccctoccnteccsteccetocsetescoteccstesccteccetoccatevceteses
toe2s"" ““loa7s"” 7344887" ""Tazs"” “"ieas"" “"S4a7s"""la188
.0500 0750 .1000 21250 «1500 21750 2000
eS
cor: .9978 P/O
MEAN ST.DEV, REGRESSION LINE —_AES.HS.

X 611752 .07132
Y  =.08761 9.03568

VARTABLE

~9953°Y-,01739 361-7
49881°X+ 00889 S01E-8

1 P/PD VERSUS VARIABLE 2 X/V SYMBOL=X

Figure B-22. Plot of BET equation versus relative pressure for

Converter A230/0649-A-LL1 (Powder)

B-23


PAGE 4

CONVERTER SURFACE AREA ANALYSIS A246/0092-A [LL-3]

+

eeeetaceetacstecnctaaceteccetecesteccetacsce

teeectece

.0375 +" +
. Y
.0350 + .
.0925 + +
.0300 + +
VUI=X) 2 :
.0275 + x +
.02s0 + +
.0225 + +
.o200 + i
.0175 3X +
Y
Lite cateccetesseteccsteceatessctessetecesTssseTesseTsaeeteaselseesTesees
1055 1088 1078 1093 109s 1165 iis
.050 .080 .070 080 +990 .100 110
Ne 3
coR= 1,000 p/PO
WEAN ST.DEV, REGRESSION LINE —RES.MS.

X  ,08492 »« .03484 X= 3,6537*Y-.01455 26E-10
Y 02720 00854 Y= ,27369X+ .00398 1S&-11

VARIABLE

1 P/PO VERSUS VARIABLE 2 W/V SYMBOL=X

Figure B-27. Plot of BET equation versus relative pressure for

Converter A246/0092-A-LL3

B-28


PAGE 4 CONVERTER SURFACE AREA ANALYSIS © A230/0649B ([UR-1)

wotecvetaccctecceteccatescctossetessatecsetesestessetsccstecsetecsetecseee
056 +
: x:
: :
052 + ;
: :
04a + +
104g + ;
VK) 2 x :
040 + i
: :
036 + +
: :
032 + :
.o2a + :
024K ;
latecscteccstessstesscteccsteccstecsetscsetsccotescctscsetessstescetossee
1085 1086 1078 108s 1098 1108 is
.050 060 .070 .080 .090 400 140
ar)
cor= 9984 P/PO

MEAN = ST.DEV,.
x 08482 03484
Y ,04021 =,01548

VARIABLE 1 P/PO

Figure B-23.

REGRESSION LINE  RES.MS,
X= 2,2495*Y-,00563 7746-8
Y= ,44314°X+ .00262  152E-8

VERSUS VARIABLE 2 X/V ‘SYMBOL=X

Plot of BET equation versus relative pressure for
Converter A230/0649-B-UR1

B-24


PAGE 4 CONVERTER SURFACE AREA ANALYSIS A254/0191-A (LL-1, 100 MESH)

: :
: Y
-080 + a“
. x.
: :
om + +
. .
.072 + +
ia-x) :
01 + +
: x :
054 + +
: :
005 + +
. .

: x
036 + VA :
027 + +
y“x .
x :
ee ee tesectessctesssteccetoccetescstessctscscteccetescetoses

‘ 0875 01925 01875 01625 01875 22125
0500 21750, 1000 +1250 «1500 1750 2000
Ne

4
COR= .9880 P/PO
MEAN ST.DEV. REGRESSION LINE  RES.MS.
X 19752) ,07432 = 2,6481*Y-.02172 302-7
Y 05256 02687 Y= .37598*X+ .00837 429E-8

VARIABLE 1 P/PO VERSUS VARIABLE 2 X/V SYMBOL=K

Figure B-52. Plot of BET equation versus relative pressure for
Converter A254/0191-A-LL1 (Powder)

B-53


RUN DESCRIFTICN: ALICATL - AUTO CATALYST
DIATE OF XRAY ANALYSIS: 04/30/87
SAMPLE TYFE: BRICUETTE
TE 10 N/A
CELLANEUL's INFUP NONE

NV ED ML, a
MELE IDs Araé/c

ELEMENT LETN 11M

vA oD

Mo

AL

‘1

e

CL Xx

! 222885 E-0

cA L707 27E-€

TI »186917E-0

v ia} + BLLK07E-93

CR Q

MN

FE

co xX

NI

miu Xx
x
x
x ~.1315.34E-02 +-
x —. 444058 -04 iad
u wi? 7 ++
x +e
x +

+
x te
—

TOTAL DETENTED BY XRF =


PAGE 4 CONVERTER SURFACE AREA ANALYSIS A220/0400-8 (UR-1)

wet eccotencateacateccetsccctoccetscceteccetecsetocceteccetescetocsatocees
.078 + :
. Y
: x.
072 + ;
.oss + +
oso + +
wvit-x) . .
: :
: x :
054 + i
04g + :
: :
042 + +
«03a + +
: :
xX .
.030 + ;
: tecscteccctecsstecseteccetoccsteseetessstecces
1085 1085 1165 18
.080 .090 100 140
Ne 3
coR= .9997 P/O

MEAN = ST DEV, REGRESSION LINE RES.MS.
X = .08482  .03484 X= 1,6170*Y-.00408 168E-8
Y 05487 ,02154 Y= .61800*X+ 00255 641E-9

VARIABLE 1 P/PO VERSUS VARIABLE 2 X/V SYMBOL=X

Figure B-17. Plot of BET equation versus relative pressure for
Converter A220/0400-B-UR1

Ru1g


PAGE 4 CONVERTER SURFACE AREA ANALYSIS~A240/0334L-A SAMPILE 8 & C

WV(1-K)

N=

+

+

+

+

weateccctecectaccoteveeterectscestecee

+0780

0875

.0600

0480

Shee tee ee te ere tem ee tee ee tee ee teens te one tenes

oot

.150 7

4

COR= ,9895 P/PO

MEAN ST.DEV. REGRESSION LINE RES.MS.

X 612978 = .07887_ X= 2.9101%Y+ 00137 961E-8
Y 04137 = .02736 «Y= .34328°X-430E-3 136-8
VARIABLE 1 P/PO VERSUS VARIABLE 2 X/V SYMBOL=X

Figure E-10. Plot gf BET Equation Versus Relative Pressure for
Converter A240/0334L-A (Powder Sample)

E-11

saoutenceteceetecsYtoes

pe ee te ee te ee te eee tee ee th ee te we tee



2 The whole converters were visually inspected, weighed with and without
any heat shields, and then carefully cut to expose the catalyst material.
All catalyst samples were visually inspected and weighed.

3. Each converter was disassembled in a manner to expose the catalyst
material with a minimum of disturbance.

a. _In step one, the catalyst was sectioned into quarter pieces. The
upstream biscuit of the catalytic converter was sectioned as
pictured in Figure 1. Each quarter has a length "L" the same as the
length of the original uncut biscuit, but a height and width half of
tke original height and width (1/2H and 1/2W).

b. In step two, one of the quarter sections was further sectioned into
three pieces as shown in Figure 1. The front piece had a length of
0.5 inch, the rear piece had a length of 1.0 inch, and the middle
piece had a length of "L - 1.5 inches." From the center of the
middle piece, a 0.5-inch sample was taken. Each of these three
0.5-inch samples underwent surface area analysis. The opposite
quarter was submitted in its entirety for (XRD) analysis. Samples
were scraped from an area no larger than 0.25 cubic inches along
the center line of the catalyst. One sample each was taken 1 inch
from the front and rear faces, and the third sample was taken at
the midpoint of the length of the substrate and 0.5 inch from the
outside surface.

c. Two of the quarter sections shown in Figure 1 were not subjected
to any immediate analysis when a whole catalyst was supplied.
These samples were kept as additional material for future analysis.
Partial catalyst samples were sectioned starting with step two.

d. ‘The downstream biscuit was sectioned by cutting the substrate into
quarters similar to the upstream substrate. One sample each was
taken 0.5 inch from the front face and the rear face as shown in
Figure 2. Each of these two pieces underwent BET surface area
analysis. The remaining middle section was submitted for XRD.
The XRD samples from the B biscuit were scraped from an area
no: larger than 0.25 cubic inch along the center line and 1.0 inch
from the front face. This was the only sample for XRD from the B
biscuit. The entire quarter section positioned diagonally from the
section used for BET surface area analysis was used for PIXE
analysis. The remaining two quarter sections from the four whole
converters (when provided) did not undergo analysis at this time,
but were saved for future work.

A. Sample Identification

For the purpose of identifying the converters analyzed in this program, each
converter was designated with the seven or eight digit EPA identification code.
Once the converters were opened, the upstream biscuit was labeled "A," and the
downstream biscuit was labeled "B." Each quarter section from the A biscuit was
designated according to its location within the can (UL-upper left, UR-upper right,
LL-lower left, LR-lower right). The samples for BET surface area and PIXE were


PAGE 4 CONVERTER SURFACE AREA ANALYSIS-A220/0810 - 1-A

wacctacccteccctecsctowcetennet

Pecan

voeeteceeteccstevectooset

11

010

.09

ee ee

WVI-X)}

07

04

ee ee

x

ent eceFeaeets

oe

+225
2210

lad 4

CORs .9882 P/PO

MEAN ST.DEV. REGRESSION LINE RES.MS.
X  .12178 = .07967__ X= 2.1684*Y-,00790 3426-7
Y 05978 03666 Y= ,45831°X+ 00384 7256-8

VARIABLE 1 P/PO VERSUS VARIABLE 2 X/V SYMBOL=X

Figure E-3. Plot of BET Equation Versus Relative Pressure for
Converter A220/0810-1-A (Powder Sample)

E-4

«

SS

seeeteccatace

+240


PAGE 4 CONVERTER SURFACE AREA ANALYSIS  A240/0270A, LL~1 [100 MESH]

+. +

+ +,

atrccctencetoccatecnctescatvcretocsctessstassetevestoves

060

05S

x/VEA-x)

050

2045

040

ee ee ee ee ee rey

035

o tee

tee

030

/

x

/

coeetecentecceteccetsssetae oteweet

042 9054 2086 .080 102 +118
2048 080 072 2084 086 2108

Kees
+

Nw 3
COR= .9939 P/PO

MEAN ST.DEV. REGRESSION LINE RES.MS.
xX 08464 9.03514 X= 2,0098°Y-,00915 S63E-9
Y 04665 = 01748 Y= .49745°X+ 00456 139E-3

VARIABLE 1 P/PO VERSUS VARIABLE 2 X/V ‘SYMBOL=X

Figure B-40. Plot of BET equation versus relative pressure for
Converter A240/0270-A-LL1 (Powder)

Beal

‘secetees

‘eceetecestoceetoccetsccets

‘+

re ee ee ee er ere er oh

eee te ee tee

+

126


PAGE 4 CONVERTER SURFACE AREA ANALYSIS A24S/0092-A [LL-2)

cotvecetearotevcetvevetevectecceteccetssontecsate

«0325

+0300

20275

WAVE1=K)

0250

0225

0200

20175

0150

Pa 2 ee ce ca

ate caatecaataneatecceTeceets

055 065 07!
2050 +380 .070 0380
te 3

con ,9996 P/PO

WEAN ST.DEV. REGRESSION LINE RES.HS.
XX  ,08482 =.03484 X= 3,.5302*Y-597E-6 2046-8
Y 02420 00987 -28303*X+ 109E-6 1636-9

VARIABLE 1 P/PO VERSUS VARIABLE 2 X/V SYMBOL=K

Figure B-26. Plot of BET equation versus relative pressure for
Converter A246/0092-A-LL2

B-27

ceoteeeeten

*<

ce ee ee

- te

tee

a es


PAGE 4 CONVERTER SURFACE AREA ANALYSIS ALUMINA PARTICLES (81.4 + 6.2 M2/G)

secetecenteccetscceteccctoscctsccatresatsccctocsatecceteccatecseteccetete

.01250 + x +
: :
.01tas + +
.01000 + i
.00875 + i
wVUIX) :
.00780 + :
: x :
.00825 + +
: :
.oosoo + +
: x .
.00375 + +
2x / :
.ooaso + (/ i
Ve naeteccetecesteccetescatacactassatsscetsccetesestecseteccetece
{078 1108 1135 2165 1198 1235
.080 .080 120 150 180 .210 .240
4
cons 9989 P/e0

MEAN ST.DEV. REGRESSION LINE RES.MS.
X 1217707887 X= 19,035*Y-.00819 1926-8
Y ,00872 .00418 Y= .05252°X%+ 3276-6 S3E~10

” VARIABLE 1 P/PO VERSUS VARIABLE 2 X/V SYMBOL=X

Figure D-8. Plot of BET equation versus relative pressure for
Alumina 81.4%6.2

D-9


APPENDIX B

BET EQUATION VERSUS RELATIVE PRESSURE


INLET

\ *

OUTLET

Figure A-2. X-Ray Radiograph of A246/0092


PAGE 4 CONVERTIER SURFACE AREA ANALYSIS - A221/0447-3 B AND C

t+eevet +

eccetenne

teneetovee

°

01780
1575

1400

91225
WVU1-K)

0700

ee Hem we tee ee Hee we terre tere teres tenes toe

b
3
8
+

90" 4210"

i 4
COR= .3987
MEAN ST.DEV. REGRESSION LINE RES.MS.
X  .12176 = 07986 x= 1,3829*Y-.00833 SBBE-8
Y ,09407 .05788 Y= .72267*X+ 00808 2976-8

VARIABLE 41 P/PO VERSUS VARIABLE 2 X/V ‘SYMBOL=X

Figure E-2. Flot of BET Equation Versus Relative Pressure for
Ccnverter A221/0447-B (Powder Sample)

E-3

+

ok

a


PAGE 4 CONVERTER SURFACE ARGA ANALYSIS A2GO0/O005L-A [LL-2}

atecce ec ceteaetoccetescetecsetecset, +

+

15

+
1B +
130+

XVEA-X] |
e+
17+
10 +
09 +
08 +
ms
Yt
9420 .990 .
te 3
CoR= .9989 P/PO

MEAN ST.OEV. REGRESSION LINE RES.HS.
«08451 = ,03489 X= ,333944*Y- 00937 523E-3
Y  .11300 .94175 «1972X+ ,01145 = 759E-8

VARIABLE 1 P/FO VERSUS VARIABLE 2 X/V SYMBOL=K

Figure B-8. Plot of BET equation versus relative pressure for
Converter A280/0005L-A-LL2

B-9

+ +

eee et neat eres tecretecees

Y

Fee te ee te

ee



PAGE 4 CONVERTER SURFACE AREA ANALYSIS A240/0077-A LL2

+ + +

atacnetevcetaccatecsctecceteccstoccatescetsccataccetesscateseetescateaeXtY

x

0500

20475

20450

X/V[4-X)
60425

a ee ee oe re

ee

0400
0375 +
x :

.0380 +
0325 +
x 4 :

a

26

Ne 3

COR= ,9597 P/PO
MEAN ST.OEV. REGRESSION LINE RES.MS,

xX 08462 03514 X= 3,1485*%Y-.03915 195E-6

Y 03931 = .01071 “= ,292549X+ 01455 1816-7

VARIABLE 1 P/PO VERSUS VARIABLE 2 X/V SYMBOL=X

Figure B-32. Plot of BET equation versus relative pressure for
Converter A240/0007-A-LL2

B-33


PAGE 4 CONVERTER SURFACE AREA ANALYSIS —A240/O141L-8 «= AND
ancctaccateccetocsateccetssentassetocsetssvetecsetacestsccatooset
1250 +
1125 +
:
tooo +
087s +
AX)
.0780 +
.0825 +
: x
.osoo +
. x
.0975 +
> x
0250 +f
¥
sacateccataccetacnateseatecsateccataccatascatacsatasentanset
‘045 ‘078 1105 1135 1165 M138 123
080 .030 .120 .180 180 .210
ie 4
cone .gast °/P0
MEAN ST.DEV, ‘REGRESSION LINE —AES.MS.
xX 1217707987 X= 2,0947*Y-,00898  185E-7
Y [neae7 ‘oagt2 Y= .aenet*x+ 00369 3986-8
VARIABLE 1 P/PQ VERSUS VARIABLE 2 X/V SYMBOL =x

Figure E-9. Plot of BET Equation Versus Relative Pressure for
Converter A240/0141L-B (Powder Sample)

x

Fee

\

ec Sr Ss or aed

rettraat

2240


PAGE 4 CONVENTER SURFACE AREA ANALYSIS A254 10181A LL-2

<ee

x

060

2055

XV(A-X)

050

045

«035

Ce ee te ee tee ee te ee te eee tee

+
+
+
e
+
.
+
+
.
+
+
x
Y

Nw 3

Cor 1,000 P/PO
MEAN ST.DEV. REGRESSION LINE RES,MS.

x 08482 ,03484 X= 1,9582*Y-.00723 SSE~S

Y .04898 01778 Y= ,51040%X+ ,00369 146-9

VARIABLE 1 -P/PO VERSUS VARIABLE 2 X/V SYMBOL=X

Figure B-50. Plot of BET equation versus relative pressure for
Converter A254/0191-A-LL2

B-51


PAGE 4

CONVERTER SURFACE AREA ANALYS=S A221/0310-A (LL-2)

aa T acc eteccataccetecoetocvatesnerenretscentacsetecnstaasetssentacsetesnes

: Y
195 + t
180 + a
135+ +
XAVUA-K) :
so + x L
135 + :
20+ ‘
105 + +
«oso ix :
Y .
.070 *
ne 3
CoR= 1,000 #/P0
NEAN ST.DEV. —-REGRESSZON LINE RES. 1S.

xX 08492 © =©,03484 X= .63510*Y-.00752 A79E-S
Y 14538 05486 Y= 1.5742°X+ .01184 4435-9

VARIABLE

4 P/PO VERSUS VARIABLE 2 X/V SYMBOL=*

Figure B-2. Plot of BET equation versus relative pressure for

Converter A221/0310-A-LL2

B-3


PAGE 4 CONVERTER SURFACE AREA ANALYSIS ZINC OXIDE 0,62 + 0,04

Feccetsces

1.750

.
+
+

1.575

1,400

XWV1-X)
1,225

.8750

ee ee eee

+7000

5250

x

/

aateccoteccetevscteccetescetscceteccctevcoteccstoccatocssteces

048 075 105 135 0165 2195 2225
060 080 «120 «150 180 2210

ee ee are

a 4
COR= .9994 P/PO

MEAN ST.DEV. REGRESSION LINE RES.MS.
X > 612179 =,07968 X= .14269*Y-,01687 120E-7
Y .97176 55808 Y= 6.9994*X+ .11929 S89E-6

VARTABLE 1 P/PO VERSUS VARIABLE 2 X/V ‘SYMBOL=X

Figure D-1. Plot of BET equation versus relative pressure for
Zinc Oxide 0.6240.04

D-2

+ + +, Peseatae

2240

+

He ee te eee

a os

tee

ee errs


Biscult
Number

TABLE 6. ELEMENTAL ANALYSIS OF NOBLE METALS AND POISONS BY PIXE

Sample Welght Percent of Element
Location P s Ca Min NE Za RB Pa Pt Pb Others

A221/0198-B

A221/0310-A

A221/0310-B

‘A280/0005L-A

A280/0005L-B
A220/0400-A

A220/0400-B
A230/0649-A

A230/0649-B
A230/0734-B

A246/0092-A

A246/0092-B
A240/0007-A

A240/0007-B
A240/0270-A

A240/0270-B
A254/0037-A

A254/0037-B

A254/0191-A

A254/0191-B

LL . 0.0740.02 0,060.01 0.0140.0004 trace 0.0240.0002 . 0.170.002 ’ 0.0240.001  Na,Mg,A1,SI,Ti,Fe

LLI 1.70.5 * 0.1340.01 0.070.003 0.0440.001 0.460.001 trace 0.0240.01 0.1140.01 4.1540.01 Mg,Al,Si,K,Ti,Fe,Ce

LL2 0.4440.04 ——0,0640.03 0,060.01 0.0240.002 0.0240.0003 0.070.003 0.010.003, * 0.1340.004 0.440.002 NajMg,ALSLTLFe,Ce

LL3 0.1140,05 0.0840.02 ——_0.0640.01 0,0140.002 0.0140.0003 -0.0340.0003 0.010.003, * 0.100.003 0.190.002 Fe

LL . 0.0640.02 0.0440.01 0,0140.0005 trace 0.0240.0002 . 0.1520.004 ° 0.7440.002 nena Si,Ti,Fe

LL 2.0140,05 0,130.03 ~——0,0340.01 0.1340.003 ——0.0240.0004 0.6340.001 0.0140.004 * 0.0820.01 0.312.003 —_Na,Mg,Al,Si,K,Ti,Fe,Ce
Lue 0.4120,06 —0.0620.03 ~——0.0840.01 0,0240.001 0.0140.0003 —0.0740.0004 —_0.0140,002 0,0840.003 0.040.001 Na,Mg,Al,SI,K,Ti,Fe,Ce
LL3 0.194005 0.1740.02 0.020.002 trace 0.0540.0003 0,010.03 * 0.140.003 0.010.001‘ Na,Mg, Al,Si,K,Ti,Fe,Ba,Ce
LL trace 0.1620.02 * * 0.1120,0002 * 0.39£0.002 —0.0120.003 -0.2020.001 —Na,Mg,AI,Si,K,TI,Fe

m1 1 sito ng e.c2t0.003 25028.c32 5.3525.002 20.01 v.vozu.uus .0420.01 2.3820.01 —_Na,Mg, Al,Si,K,TI,Fe,Ba,Ce
LL2 0.6620,04 0.0140,003 2.0280.001 0.0440.001 0.0240.01 0.0520.01 0.0440.01 0.360.003 Mg,Al,Si,K,TI,Fe,Ba,Ce
LL3 0.1420,05 trace 1.6140,001 0,0420.001 0.0240.01 0,050.01 0.0440.004 —0,1140.002 Na, Mg,A1,Si,K,Ti,Fe,Ba,Ce
Lt 0.1420.03 0,150.02 0. 1040.01 0.0140.0004 0.010.002 0.0140. 0002 . 0.0140,001 0.170.002 0.180.001 Na, Mg, Al,Si,Ti,Fe

LL 1.6120.04 0.1820.04 0.2420.02 0.0240.002 0.0540.0004 0,5240.001 trace 0.0540.001 0.610.003 Na,Mg,Al,Si,K,Ti,Fe,Ce
LL2 0.474005 —0.0720.03 ——0.0740.02 trace 0.0240.0003 —0.0340.0003 0.010.003 0.050.003 0.1120,003 0.030.002 Na,Mg, Ti,Fe,Ce
LL 1340.05 0,1240.03 0,050.02 * 0.0340,0003 —0,0240.0003 —0.0240.003 © 0.0540.004 0.110.002 .0340.002 Mg,AlSI,K,Ti,Fe,Ce
ae trace 0.1740.03 -0.0840.02 . 0.010.003 0.0240.0004 —0.0240.002 —0.0640.003 0.160.003 0.040.002 Mg, ALSLTHFe,Ce

LL 0.1420.04 0.1740.02 0.1040.02 ° 0.0140.0004 0.0340.0004 0.0340.001 0.0920.004 0.2040.003 0.0140.002 Na,Mg,Al,Si,TI,Fe,Ce

Lu 1.4540.04 —0.4640.03 —(0.0640.01 0.0340.003 1,960,001 0,1240.001 0.0240.008 0.040.004 0.0820.01 0.732001 NasMg/ALSLIGTHFesBasCe
Luz 0.3640.08 —0,5840.02 —0.0440.01 trace 2,6040,001 0.0240.001 0.0340.001 0,0540.002 © 0.1140.004 0, 140.001 M )K,Ti,Fe,Ba,Ce
LL 0.1240.04 0,640.02 ©——_0.050.01 3.1340.002 0.0240.001 0.0340.01 0.060.003 0.130.005 —_0.0640.003 Name, A1,SI,K,TI,Fe,Ba,Ce
LL trace 0.7420.02 -0.0640.01 —0.0140.001 —0.0240.0003 0.0140. 0003 * 0,0420.002 0.2920.002 0.0420.001 Na, Mg,Al,Si,Ti,Fe,Ba

LL 2.3340.05 —0.8740.03 © 0.0540.02 0.040.003 2.140.001 0.2a+0.001 0.0340.01 . 0.1120.01 0.3840,004 —_Na,Mg,AL,Si,K,TI,Fe,Ba,Ce
LL2 0.8740.05 —0.4940.03-—0.0440.01 0.0240.002 1.75#0.001 0.0640.001 0.02% 0.01 . 0.08%0.004 0.090.002 Na, Mg, Al,S1,K,Ti,Fe,Ba,Ce
LL3 0.1740.05, 0.2640.03 0.0440.01 0.0140.001 0.7040.0004 0.0140.0004 0.0140.002 . 0.0440.002 0.0140.001 Na,Mg,Al,S1,K,Ti,Fe,Ba,Ce
LL 0.2540.04 0.5640.02 0.0740.01 0.0140.002 0.2040.0003 0.0940.0004 . 0.07£0.0007 0.1240.004 0.0840.002 Na,Mg,Al,Si,Ti,Fe,Ce

LL 2,0240.05 —0.2040.030.1320.02 0.080.003, 2.6140,001 0.520.001 0,0240.005 ’ 0,0740.02 0.8420.01  —-Na,Mg,Al,SI,K,Ti,Fe,Ce
LL 1.2520.08 —0.1720.03 ——0.0840.02 0.050.004 4.92£0.002 0.16%0.002 0.030.004 0.1340.01 0,320.01 Na,Mg,Al,Si,K,Tl,Fe,Ce
LL3 0,460.05 —0,0940.03 —0.0720.02 0.020.002 2.0240.001 0.0520.001 0.0140.004 * 0.0540.01 0.100.003 Na,Mg,Al,Si,K,Ti,Fe,Ce
LL 0.1640.04 -0.1440.02 © 0.0540.01 0.010.001 0.070.002 ——-0.0340.0003 ° 0.0440,002 0.050.002 —0.0540.001 Na, Mg,AI,SI,Ti,Fe,Ce

uu 1.7540,.04 —0.3540,03——0.1540.01 0.1240.004 ——_0.0120,0004 0.2140,001 0,05¢0.004 . 0.2440.01 0.4140.003 —_Na,Mg,Al,Si,K,TI,Fe,Ba,Ce
LL2 0.3420.04 0.860.03 0.0840.02 0,010,005 0,0140,0004 0.0240.0004 0.0340,005 . 0.2440.004 0.0640.002 Na, Mg, AL,S1,K,Ti,Fe,Ba,Ce
LL3 0,1640.05 0.8340.03 0.0840.02 0.010.004 0.0140.0004 0.0240.0004 0.0340.004 . 0,2240,004 0.0320.002 Na, Mg, Al,Si,K,TI,Fe,Ba,Ce
Lt trace 1.490.030. 1020.02 * ° 0.0340.0001 0,079.01 . 0.4240.004 0.040.002 Na, Mg, Al,SI,K,Fe,Ba,Ce
LL 1.45%0.04 —1,0640.04 ——-0.0940.02 0.0440.01 0.0240.001 0.2140.001 0,0340.01 * 0.2540.01 0.8740.01 —_Na,Mg,Al,SI,K,Ti,Fe,Ba,Ce
Liz 034¢0.08 0.8940.03 —-0.0740.02 ry trace 0.0340.005 0.0340.01 . 0.2240.004 (0.180.003 Mg, Al,SI,K,Ti,Fe,Ba,Ce
LL3 0.12#0.05 1.0140.03 —0.0740.02 * trace 0.0140.0004 0.020.004 . 0.2040.003 —-0.0640.002 Mg, Al,Si,K,Ti,Fe,Ba,Ce
LL . 1.4040.03 0.0940.02 . . 0.04t0.0007 0.050.007 . 0.5340.01 0.0940.003 Mg,Al,S1,K,Fe,Ba,Ce

below the detection mit
trace - at the detection mit

€T


PAGE 4 CONVERTER SURFACE AREA ANALYSIS AQ54/0191-A  (LL-3)

F+ecvetoceat Fecccteceet + + +

058
2052
048

/V(1-x)
0.

2032
2028

+
+
+
.
+
049 +
+
:
+
x

2075 085 2085 2105
080 030 100 2110

Ne 3
COR .9996 p/P

MEAN ST.DEV. REGRESSION LINE RES.MS.
X 08481 = .03484 X= 2,3359*Y-,01176 173E-8
Y ,04134 01491 Y= ,42779%X+ 00508 316E-9

VARIABLE 1 /PO VERSUS VARIABLE 2 X/V SYMBOL=X

Figure B-51. Plot of BET equation versus relative pressure for
Converter A254/0191-LL3

B-52

eacetoccetsvceteace

etecccteccctoanctaccctocscteccctocceteccetoccstoscoteses

Brees

SS


RUN DESCRIPTION: AUIATL - AUTO CATALYST =WRI
BATE GF XRAY ANALY'S13: 04/30/35

SAMPLE TYPE? JBRIGUETTE

SITE ID: N/A

MISCELLANEGIIS INFO? NONE

SAMPLE SECUENHE NO
‘PAMPLE IDk ADL /OR10-B-LL

ELEMENT DETN LIM

NA OD +
MG ne
AL +
a1 . ae +>
Pp | 282689 +-
3 »1S1lL02E + 164057 +7
CL Xx + 105726E-02 ~.161345E-02 +7
K + L409S6E-08 »DSO8S1E-O1 +-
cA - 197394E-03 + TISOIFE-OL +-
TI 21S9796E-O3 2115718 +
v - 545 244E-03 22795 1E-92 +
CR 2 VIS BIAE-OS ~ 52201 2E-0L +-
MN » SLSSO%E-03 « 7L9SS5E-02 +-
FE »447821E-03 + 348564 +-
m9 xX 31: 191E-03 -.127671E-"9 +-
NI +-
cu +
ZN 23141 27E-01 +-
3E XxX + 296731E 03 7 R47 668 3E-O2

BR X + E47 9G7E-O8

SR OX

mo Xx

co Xx

SN XxX

SB OX

HA X

TE

rt Xx

HG xX

PE Bebe 03

TOTAL DETECTED BY XRF = 45,2124


Conversely, a normal surface area does not necessarily indicate a normal catalyst,
because the depos ts can increase the apparent surface area while covering the
surface and preventing contact with the exhaust gases. In this work assignment, the
surface area of 0.5 inch pieces from the front, middle, and rear of the upstream
biscuit and the surface area from the front and rear pieces of the downstream
biscuit were analyzed. These large wedges were placed in a large sample tube and
analyzed whole. The sample tube consisted of a large tube with a ground glass joint
in the middle, or the sample was entirely sealed in glass. Either method was equally
effective, except the tube with the ground glass joint experienced a problem with
breakage. In order to eliminate this problem, all subsequent samples were sealed in
glass.

Upon completion of the analysis of the LL1 piece, the sample was ground to a
coarse powder (approximately 100 mesh). This sample was also analyzed for surface
area. The results for the specific surface areas are presented in Table 4. The plots
for the BET equaticn versus the relative pressure for each converter are included in
Appendix B.

F. X-Ray Diffraction

X-ray diffraction analysis of the samples was used to determine the crystal
structure of the alumina. Gamma-alumina and several other very similar alumina
structures are the criginal crystal structures used in the alumina washcoat. Whena
catalyst containing these types of alumina is overheated (temperatures greater than
1000°C), the crystal structure changes to the alpha-alumina form. This conversion
in crystal structure can trap the active metals and change the active surface area of
the catalyst. The Debye-Scherrer powder x-ray diffraction technique was used to
determine the alumina crystal structure. This technique is well suited for the
analysis of monolith catalysts because of the small quantities of sample required. In
the case of monolith catalysts, the alumina is deposited as a thin wash-coat on the
surface of the ceramic substrate. The alumina can be scraped off carefully and
analyzed, The x-rays are diffracted by the various crystalline compounds within the
sample, Each crvstalline compound has a characteristic diffraction pattern.
Amorphous compounds do not result in a diffraction pattern. These patterns are
compared to known compounds in a Powder Data File for identification. Table 5
lists the alumina crystal structure of each sample and any other crystalline
compounds observed in the samples.

G. ‘Proton Induced X-Ray Emission

Proton induced x-ray emission (PIXE) was used to determine the
concentrations of noble metals and the accumulation of poisons. This technique
utilized protons to "knock" electrons from the inner orbital shells. The electron
removal causes the element to fluoresce x-rays at characteristic wavelengths.
These fluoresced x-rays are detected, and they represent the quantity of each
element present in the sample.

The elements of concern were phosphorus (P), sulfur (S), calcium (Ca),
manganese (Mn), zirc (Zn), lead (Pb), platinum (Pt), palladium (Pd), rhodium (Rh),
and nickel (Ni). The elements P, S, Ca, Mn, Zn, and Pb are poisons or contaminants.
They are derived from engine wear, dirt deposits, oil, fuel, and other sources. The
noble metals are Pt, Pd, and Rh, and they perform the function of "cleaning up" the
exhaust. Nickel was found in some converters, and is reportedly present to enhance


PAGE 4 CONVERTER SURFACE AREA ANALYSIS = A1S5/0941-2-A SAMPLE 8

wewotennetassetrecatecsetecceteccntrccstessatessatesvetossetessetaccetoas
. Y
45 + fi
. x.
40 + +
35 + +
: :
xviI=x) | :
30 + L
28 + +
. x .
. :
20 + +
: x :
13+ / :
10 Y +
Y :
lesctececteccetsccstecsetecseteccetsccstescstsssstessetesestsseatessetecs
104g 1078 ‘108 1138 1165 1198 1228
.080 080 120 .150 180 .210 .240
we 4
cor .s9g8 pvea

MEAN ST.DEV. REGRESSION LINE RES.NS,
xX  .12179 = .07988 X= .S3748*Y~.00838 3726-8
Y 23848 .14823 Y= 1,88SB°X+ .01198 1296-7

VARIABLE 1 P/PO VERSUS VARIABLE 2 X/V SYMBOL=X

Figure E-8. Flot of BET Equation Versus Relative Pressure for
Converter A155/0941-2-A (Powder Sample)

E-9


APPENDIX C

ELEMENTAL CONCENTRATIONS OF METALS AND POISONS
FOR REAR BISCUITS BY X-RAY FLUORESCENCE


PAGE 4 CONVERTER SURFACE AREA ANALYSIS-A220/D81C 1-8
ca cateccats rooteccetecsetescetecsetevcetecseteccetessstecsetevcetsseetecs
150+ +
. Y
: .
. x .
135 + ;
120 + t
105 + ¢
xVU-K) :
aso + I
075 + +
: x :
ost + +
: :
Q x :
045 + / +
35 +X, +
Vhetecoctecsatesscteccetecectecsete cect aeetecceteccetecsetes :
104s ‘078 $108 1138 1168 1198
.080 .os0 120 .180 .180 .240
m4
cor .9987 P/Po

MEAN ST.DEV. REGRESSION LINE RES.MS,

X= = 12177 ,07887 X= 1,8936*Y-,00117 2806-7
Y 07258 04888 Y= ,S88S90°X+ S79E-8 s8BE-8
VARIABLE 1 P/PO VERSUS VARIABLE 2 X/V ‘SYMBOL=X

Figure E-4. Plot of BET Equation Versus Relative Pressure for
Converter A220/0810~1-B (Powder Sample)


RUN DESCRIPTION: AUCATI - AUTO CATALYST SWRI
DATE GF XRAY ANALYSIS: 04/30/37

‘AMPLE TYFE: BRIQUETTE

SITE Its N/A

MISCELLANELH INF NONE

SAMPLE WAER MU. St aa

SAMPLE ID: Al:¢4/017)-B

ELEMENT DETN LIM

NAL
MG
AL
=]
FP
CL Xx

+ 7O7276E
+77 B53E-

»23845E-072

+ 10747

> >K >

KOS 2 KK KOE OK

HG x
PE

TOTAL DETECTED BY XRF = 40.0731


PAGE 4 CONVIERTER SURFACE AREA ANALYSIS A240/0007A, LL-1 (100 MESH)

+

0350

20325

0300

0275

X/V(1-X)

20250

20225

20175

0150

MRF ee He ee He ee te we te wee tee ew tee ew tee we te

*
+

ee ee oars

ete cectooucteccetosvatscccteccetoccctecseteccstocsetessntessatsssstesents

2042 054 088 .078 080 102 2114
+048 2080 2072 084 096 108
Ne 3
COR= .9336 P/PO

MEAN ST.DEV.. REGRESSION LINE RES,MS.
X 08482 = .03514 3,9137*Y-,01458 = 315E-7
Y 02535 00892 Y= ,25225°X+ 00400 203E-8

VARIABLE = 1-P/PL VERSUS VARIABLE 2 X/V SYMBOL=X

Figure B-34. Plot of BET equation versus relative pressure for
Coaverter A240/0007-A-LL1 (Powder)

B-35

0126


PAGE 4 CONVERTER SURFACE AREA ANALYSIS A246/0092-8 9 (UR-2)}

Heeeet

085 + xv
060 + i
105s + +
.0s0 + +
WVUI-X} 2 :
: x :
045 + +
oa + :
035 + ;
.o30 + t
x :
.028 i
watecsetecaetconteccateccetecsatecastesaetessetencctsssetescstecsstecses
2055 .065 075 085 085 105 115
.050 -000 .070 +080 +090 100 110
Lhd 3
con= .9992 p/po

MEAN ST.DEV. REGRESSION LINE RES.MS,
xX 08482 03484 1,7999"Y+ .00244 383E-8
Y  ,04577 01934 »55471°X-,00128 = 118E-8

VARIABLE 1 P/PO VERSUS VARIABLE 2 X/V ‘SYMBOL=X

Figure B-30. Plot of BET equation versus relative pressure for
Converter A246/0092-B-UR2

B-31


RUN DESCRIPTION? AUCATL ~ ALI
BATE OF XRAY ANALYSIS: 04/30/37
‘SAMPLE TYFE: SRIGUETTE

CATALYST SWI

INFO: RE- Ri. WoO OLD SAMPLE AS CA CUNTROL

ELEMENT ETN LIM
MA
Mc.

~LBOOOFEL-O1
«45077 3E-03 41 26936 - al +
. 430305

x OO Ke oe x

TOTAL DETECTED BY XRF = 44,740

FIGURE 4. ELEMENTAL CONCENTRATIONS OF METALS AND POISONS FOR
BULK SAMPLE BY X-RAY FLUORESCENCE

22


PAGE 4 CONVERTER SURFACE AREA ANALYSIS A230/0849-A-LL3

Fecaateceatecnetancetaccateccatacacteseatsssetecentacsatescatscnstesseks

+057

x

teen

054
051
048
X/V(A-X)
2042
039
2036

+
+
+
i
045 +
+
+
+
033 +

Dee ec te ee te ee te ee te ww te ew te ee te ee

ies

11

08° 120"
Ne 3
COR= .9718

MEAN ST.DEV. AEGRESSION LINE RESUS,
xX 08482 03514 X= 2,8408%Y-,03767 197E-6
Y .04305 01202 Y= .33247*X+ 01491 160E-7

VARIABLE 1 P/PO VERSUS VARIABLE 2 X/V SYMBOL=X

Figure B-21. Plot of BET equation versus relative pressure for
Converter A230/0649-A-LL3

B-22


PAGE 4 CONVERTER SURFACE AREA ANALYSIS A248/0092-A-LL1

+

+ + + +

070 +
.06s +
.0s0 +
: x
05s +
VIX)
.os0 +
,0a5 +
.oag +
.oa5 +
:

+030 iy"

WK ewecteccctersetesseteccetocsstaasetvcastescetecestescctoees
«042 2054 086 078 080 2102 114
2048 060 072 084 096 108

+

N= 3
CoR= .9903 P/PO

MEAN ST.DEV, REGRESSION LINE RES.MS,
xX 08462 03514 -7726%Y- 00763 476E-7
Y 05204 01963 55327°X+ .00522 149E-7

VARIABLE 1 P/PO VERSUS VARIABLE 2 X/V SYMBOL=X

Figure B-25. Plot of BET equation versus relative pressure for
Converter A246/0092-A-LL1

B-26

ee ae

ce ee ee er

ete nee

a eeeteeeete

126


PAGE 4 CONVEHTER SURFACE AREA ANALYSIS A254/0191-8 9 (UR-2]

aotacsetaccctecceteccctescetscsetescstsccetecsetecsctessetecsetssentecses
: :
060 + Y
. x,
.055 + :
.050 + +
VX) :
045 + x +
. .
040 + +
: :
035 + +
030 + :
. .
025 YX +
vetevcetecastascateccetecseteccetecsetscsctaccstsssateacstescstesseteases
1085 1085 1078 ‘088 1088 1108 45
.050 .080 .070 080 .090 -100 110
Ne 3
CoR= .9888 P/Po

MEAN ST. DEV. REGRESSION LINE RES.MS.
xX 08482 .09484 X= 2,0231%Y-,00224 1966-8
Y 04303 «007721 Y= .48388*X+ .00114 © 479E-9

VARIABLE 1 P/PO VERSUS VARIABLE 2 X/V SYMBOL=X

Figure B-54. Plot of BET equation versus relative pressure for
Converter A254/0191-B-UR2

B-55


TABLE 9. PRIECISION, ACCURACY, AND COMPLETENESS OBJECTIVES

Analytical Precision Coeff. Completeness
Procedures _ of Variation, % Accuracy %
Whole catalyst X-ray NA@ 0.026 >95
2-2T¢
X-ray fluorescence 1-3 415% >95
X-ray diffraction 5 25% >95
BET surface area 7 B% >95
PIXE +5 15% 95

NA = not applicable
bgeometric unsharpness
Csensitivity


PAGE 4

CONVERTER SURFACE AREA ANALYSIS  A246/0092-8 (UR-1)

: Y
: Xx
.04g0 + ;
.0455 + i
.0420 + +
VEX) :
.0385 + x +
.0350 + +
.0315 + L
: :
.0280 + :
0245 + ;
* :
woteccetocsotecsstecsotesseteccetscseteccctsscetsssatessetssentecsstessss
1058 108s 1078 1088 108s 1105 is
.050 .060 .070 .080 .090 100 110
m3
cor .9984 P/O
MEAN ‘ST.DEV. REGRESSION LINE RES.MS.
X 09082 03484 X= 2,4945"Y-.00474 7825-8
Y {03879 <014a9 Y= ,40ga2"x+",00208 1916-8
VARIABLE 1 P/PQ ‘VERSUS VARIABLE 2 X/V syMBOL=x

Figure B-29. Plot of BET equation versus relative pressure for

Converter A246/0092-B-UR1

B-30


also designated with respect to their locations in the biscuit. The location along
the length of the quarter section was labeled 1, 2, or 3, respectively, for the
upstream, middle, or downstream position. The exception to this rule was for the B
biscuit; no middle sample was taken for the BET surface area analysis. In this case,
"2" indicated the downstream location. The labeling designations are listed in Table
2. The term "biscuit" is used to refer to each individual piece of ceramic
honeycomb material in a converter.

B. Whole Catalyst X-Ray

Two of the converters were examined by whole catalyst x-ray (A280/0005L
and A246/0092). The other two whole converters in this work assignment
(A254/0037 and A254/0191) were examined by whole catalyst x-ray in Work
Assignment No. 20 of EPA Contract 68-03-3192. The radiographs taken in this work
assignment are included in Appendix A. Both converters appear normal. Converter
A246/0092 had several couplings welded to the outside of the case with
thermocouple connectors. Upon careful examination, the positions of the holes
drilled for the thermocouples can be observed in the radiographs.

C. Sample Weighing

The weights of the various samples were determined 1n several stages. All of
the whole converters were weighed whole, and each biscuit was weighed after
opening. All of the partial samples were weighed, but these weights are only a
determination of the amount of sample received. In order to do additional
calculations on these converters, the weights of the biscuits before the samples
were taken must be known or estimated. All of the weights are presented in Table
3.

D. Visual Inspection

Each whole converter and biscuit was inspected for visual signs of overheating
or damage. Catalyst A230/0734-A was severely melted. A large void had developed
about two inches from the front face. This was the only visible example of melting
in this work assignment. Several samples had developed cracks. They were:
A221/0310-A, A220/0400-B, A230/0649-A&B, A230/0734-B, A246/0092-A&B, and
A240/0270, Catalyst A246/0092 had been drilled in an effort to place
thermocouples into the center of the biscuit. All of the catalysts showed typical
signs of usage (dark front faces with rust on outer surfaces).

E. Specific Surface Area

The specific surface areas of the whole length of all biscuits were measured
with a Micromeritics Flowsorb II dynamic surface area analyzer using the multipoint
analysis technique. This analysis was conducted "in-house" during this Work
Assignment. The advantages for "in-house" analysis include a stricter control of the
analytical procedures, ease of repeating questionable samples, and assurance that
the analysis is performed on a sample that represents the entire length of the
biscuit. Losses in surface area are due to thermal degradation and/or plugging of
the sub-microscopic pores with metals and other deposits. A loss in the active
surface area results in the reduction of contact between exhaust gases and the
catalyst material. A low surface area generally indicates converter overheating.


PAGE 4 CONVERTER SURFACE AREA ANALYSIS ASS4/0037-A = (LL-1)

+,

+ t+eoect

ccetecceteccntecccteccstecscteccctecsetvccstecceteccetescotosest

-1250
21125
-1000
XWV(1-K)
0875
.0750
«0825

:
+
.0500 + J
:
Y

0375

78 1625, 21875

Ne 4
COR= .9883

MEAN ‘ST.DEV. REGRESSION LINE AES.NS.
X = 41175107132 <= 1,7936*Y-,01359 111-7
Y 07308 .03973 Y= .SS88B*X+ .00787 343E-8

VARIABLE 14 P/PO VERSUS VARIABLE 2 X/V syMBOL=x

Figure B-46. Plot of BET equation versus relative pressure for
Converter A254/0037-A-LL1 (Powder)

B-47

+

«1500 21750 2000

x

wcctoccatercstecvetevcctscnetescetsccstoseatece

62125

4.

+
.

te

ee ee ee ee ee ey


PAGE 4 CONVERTER SURFACE AREA ANALYSIS A221/0310-A [LL-1!

22275

+2100

01925

YMIHK)

21756

+1875

+1400

#1225

«1050

ateenateceet

a eeeteneeteceeteeee”

seta cnateceeTeceeteccatenceteaaetecneTeseaten
2075 .085 .095 2105 «115
.050 060 .070 «080 .290 +100 4119
Ne 3
COR= .9996 P/PO
MEAN ST.DEV, REGRESSION LINE RES.HS.

x 08462 = .03484 52270°Y-.001G6 1728-3

Y 16545 06663 68116°X+ .00330  S31E-3

VARTABLE 1 P/PO VERSUS VARIABLE 2 X/V SYHBOL=X

Figure B-1. Plot of BET equation versus relative pressure for
Converter A221/0310-A-LL1

saeeteeretenneteceatecsetenes sscetaesee

a ee rr 2c

a a rs

se tee


PAGE 4

070

060

2055

WV(1-X)

2045

040

Nw 3

CONVERTER SURFACE AREA ANALYSIS A254/0037-A = (LL~2)

coteccetsccatrcectasceteccetocveteccetoccsteccetoccetsccstescetsssete

%t

x
AVroccetocccteccetsccateccetocectoccetenecteccstessatecceteccatecsetecas
1058 1068 ‘075 108s 1038 2108 148
.080 -060 .070 .080 .080 100 190

Ce ee
x“
Ce

CoR= .9988 P/PO

MEAN

ST.DEV. REGRESSION LINE RES.HS,

xX 08482 §=,03484 X= 1,6984*Y-315E-6 S4SE-8
Y 05013 = ,02048 «Y= ,58747*X+ 297E-6 188E-8

VARIABLE

4 P/PO VERSUS VARIABLE 2 X/V SYMBOL=X

Figure B-44. Plot of BET equation versus relative pressure for

Converter A254/0037-A-LL2

B-45


(PAGE 4 CONVERTER SURFACE AREA ANALYSIS A240/0270-A LL-1

atevcatecnctacceteccetsccetacceteccetaccsetecsatocrsteccsteccctoscateaXY ts

m4 + +
toa + ;
102, + i
XVUA-X) :
098 + +
.oso + ;
: x :
084 + i
07a + :
.o72 + ;
x :
ate anet Ke otocscteccctaccetecveteccstesseteccvtecceteneeteanetecsetescete
t0a2 1084 1088 1078 ‘os0 1102 ia” "Mee
.048 .060 .072 084 .038 108 120
Neg
CORE .9873 P/O

MEAN ST.DEV. REGRESSION LINE RES.MS.
X 08483 = ,03515 X= 1,3838*Y-,04078 6236-7
Y 09063 02508 Y= .70442*X+ .03101 317E-7

VARIABLE 4 P/PO VERSUS VARIABLE 2 X/V ‘SYMBOL=X

Figure B-37. Plot of BET equation versus relative pressure for
Converter A240/0270-A-LL1

B-38


APPENDIX A

WHOLE CATALYST X-RAY RADIOGRAPHS


IDLE
PAGE 4 CONVERTER SURFACE AREA ANALYSIS A280/000SL-B UR-1

ateceeteccctucsetavcctoccetecseteosetocsetacsatioast

+1350
21275
21200
x/V[1-X)
01125
1050
«0875

0900

20825
x

/

Ce

+ + + + +. + +

AAV ec etecceteceetaccstoceetecectoccetocsetesseteccetasenteseatecceteces

120

+
2042 2054 066 .078 080 102 -114
048 060 072 084 2096 +108
te 3
COR ,9998 P/PO

MEAN ST.DEV. REGRESSION LINE RES.MS,
X 08483 03515 X= 1,2399°Y-.05198  106E-8
Y  .11017_.02834 Y= ,80618*X+ .04195 687E-9

VARIABLE 1 P/PO VERSUS VARIABLE 2 X/V SYMBOL=X

Figure B-11. Plot of BET equation versus relative pressure for
Converter A280/0005L-B-UR1

B-12

“\

ee te ee te ee te ee te we ee te we te ee tee

+

te
F

+.

2126


IDLE
IPAGE 4 CONVERTER SURFACE AREA ANALYSIS A240/0007-A LL-1

20425

ee ray

+0400

0375

TYV(1-X)

0350

20325

20300

0275

0250

x

be te te ee te ee te ee tee

tee ae

re

Ce en a a

+
2126

ateceeMXeccteasetecceteccctucceteccctsccstevsctecasterestassstssceteccate
042 054 066 .078 090 102 114
048 080 .072 084 098 -108 120
ue 3
COR= .9859 p/po

MEAN ST DEV, REGRESSION LINE RES.HS.
x 08463 -.03515 X= 3,5148*¥-,03189 694E-7
Y 03315 00988 Y= .27652°%+ .00975 S48E-8

VARTABLE 4 P/PO VERSUS VARIABLE 2 X/V SYMNBOL=X

Figure B-31. Plot of BET equation versus relative pressure for
Converter A240/0007-A-LL1

B-32


APPENDIX A

WHOLE CATALYST X-RAY RADIOGRAPHS


RUN DESCRIFTICN: ALICATL — Alt CATALYST SWRI
DATE OF XRAY ANALYSIS: 94/30
SAMPLE TYPE: BRIOUETTE

SITE ID: N/A

MISCELLANE INFO: NONE
SAMPLE ‘SEO NO.E 2
SAMPLE ID ALGO/O070-B-LL

ELEMENT DETN LIM

NA bee
MiG ae
AL be
SI tn
P to
4 +-
cL XxX +
t +
cA +
3 _
+o
11204E-02 +
~S7L2132E-03 +7
»S8°731E-03 +e
x . 2461 25E-03 Ei . 172 3196-03 +7
. 1l7741 +
. 24236 1E-o2
x .
x . ac
x »S20237E-02
x »7ZA1L72E- Os =
Xx
x
x

1140846

FE

TOTAL DETECTED BY XRF = 7.44tl

C-10


PAGE 4 CONVERTER SURFACE AREA ANALYSIS = A220/0400-8-UR2

wots Fececter coteeneteceete

ataceotece

2072

066

XWV(1-x)

054

048

2042

Ce ee eS a a
Se i ee i ee re he

030
+

teres atecoete

2102
098 108 «120
t= 3
CORF .9997 P/PO

MEAN ST.DEV. REGRESSION LINE RES.MS.
xX 08482 =.03574 X= 1,8406*Y~,00527 147E-8
Y 05479 02141 Y= ,60919°X+ .00924 S546E-9

VARIABLE 1 P/PO VERSUS VARIABLE 2 X/V ‘SYMBOL=X
°

Figure B-18. Plot of BET equation versus relative pressure for
Converter A220/0400-B-UR2

B-19


RUN DESCRIFTION: AUCAT1L — ALITO CATALYST 2WRL
DATE OF XRAY ANALYSIS: 94/20/27

SAMPLE TYPE: BRICUETTE

TE ID: N/A

MISCELLANECUWIS INFOS NONE

MPLE SECUENCE Nu.e tt
SAMPLE ID: A4220/0400-8

ELEMENT DETN LIM

NA SIIE-OL te
MG 4. a
Al. a +-
1 +-
FP . tm
a R477 2E— o ++
CL xX —.204375E-02 +
+ + 210317E-0 +-
cA «L7OIS6E-1 +
TI »16093E-0% +-
v SS50421E-02 ZE-O2 +-
1 SUNBOSE-OS 2 PVE SE +
47952 1E-O2 »4746136E-02 +
»424651E-038 2348747 +
x + SOUL USE-03 2631 3E-03 +
~ 4e
+
b +
x -.147185E-028 +-
x -.271857E~
x
x
x
x
x
HG X
PRE «741 671E-0%

TOTAL DETECTED BY XRF = 44.3731

C-5


PAGE 4  CONVIERTER SURFACE AREA ANALYSIS  A240/0007B = UR-2
Foe eoeete
: Y
.1080 + x +
.0975 + i
.ogo0 + +
WVUI-X) :
.0825 + +
: x :
.0750 + i
.0875 + +
.ogo0 + :
525+ x * +
WKicsctecectesectescstescetscsctesssteccstecsetecsstescatecsetecssteceets
043 1058 ‘088 1078 {080 1102 mia” 26
048 .060 .072 084 .096 108 .120
ne 3
COR= .9951 P/PO
MEAN ST.DEV, REGRESSION LINE —_AES.MS.

X 08482 03514 X= 1,3492°y-,0208B 2406-7
Y 07827 02592 Y= .73398°X+ .01616 131E-7

VARIABLE

1 P/PO VERSUS VARIABLE 2 X/V SYMBOL=K

Figure B-36. P.ot of BET equation versus relative pressure for

Converter A240/0007-B-UR2

B-37


RUN DESCRIPTION: AUCATL - AITO CATALYST SWRI

DIATE GF XRAY ANALYS 04/30/87
SAMPLE TYPE? BRICUETTE
“ITE ID: N/A

SCELLANEOUS INFO? NONE

SAMPLE SECUENCE
DAMPLE ID ALSO/04&

&

ELEMENT DETN LIM
NA X 2263216
MG
AL
“a1
Pp

CL Xx . I7SOVSE-O3
k ner IE-OZ
cA 3
TI
uv
CR 1o93296- -02
MN 1235344603
FE
co x
NI

cu oD
ZN

SE

BR

hans %

x

x
3 x
ma x
co x
‘oN OX
SB Xx
BA
ce
FT
HG xX
FPR cop aaze- Oz

TOTAL DETECTED BY XRF = 45,0714

Cc-6


PAGE 4 CONVERTEA SURFACE AREA ANALYSIS A221/0310-A [LL-2)

ateaeteeeateeeeTensetonseteccetessctasceTeccatasnstessetescatucestasess

1050 + L
.0973 + +
.o500 + +
wi | :
0825 + i
.0750 + +
.0975 + +
.o600 + i
.0s25 + i
mx :

.050 060 .070 080 .090 «109 146
we 3
COR= 9990 P/PO
EAH ST.DEV. RES.IS.
x 08482 8 =,03484 103E-8

x
Y 07073 «.03077| Y= .80298*X+ .00383 © S40E-3

VARIABLE 1 P/PO VERSUS VARIABLE 2 X/V SVHBOL=X

Figure B-5. Plot of BET equation versus relative pressure for
Converter A221/0310-B-UR1



Biscuit
Numbers

A221/0198-A

A221/0198-B

A221/0310-A

A221/0310-B

A280/0005L-A

A280/0005L-B

A220/0400-A

A220/0400-B

A230/0649-A

A230/0649-B
A230/0734-A
A230/0734-B
A246/0092-A
A246/0092-B

A240/0007-A

A240/0007-B

A240/0270-A

A240/0270-B

A254/0037-A,

A254/0037-B

A254/0191-A

A254/0191-B

TABLE 5. ALUMINA CRYSTAL STRUCTURE BY X-RAY DIFFRACTION

Alumina Crystal Structure and Other Crystalline Structures Found

Front Face (URI)

intermediate alumina (gamma, delta, or theta) with
trace of CeOz or ZnS and AIPO4

intermediate alumina (gamma, delta, or theta)

mostly alpha alumina with some theta, possible
unidentified phosphate phases and CeQ2 or ZnS

intermediate alumina (probably theta)

mostly theta alumina with CeOz

intermediate alumina (gamma or delta)
intermediate alumina (probably gamma) with NiO
and CeQ2 or ZnS, trace of AIPO4 and Ni,
possible spinel cubic NiAl2Oq

intermediate alumina (prrobably theta)

intermediate alumina (probably gamma or mixture
of gamma and delta)

intermediate alumina (gamma) with CeOz
mostly gamma alumina with possible AIPO4
mostly alpha alumina

mostly gamma alumina with NiO

mostly theta alumina

intermediate alumina (gamma, delta, or theta) with
NiO and possible Ni

intermediate alumina (gamma, delta, or theta) with
possible CeOz

intermediate alumina with spinel cubic NiAlzO4,
possible NiO and trace of AIPO,

intermediate alumina with CeO,

mostly delta alumina with CeQ2 or ZnS, possible NiO

mostly delta alumina with CeO2

mostly delta alumina with CeO2 or ZnS

mostly delta alumina with CeOz, possible CeAlO3

Middle Outer Edge (UR2)

intermediate alumina (gamma, delta, or theta) with
CeQz2 or ZnS

intermediate alumina (probably theta) with CeOz

mostly theta alumina with trace of alpha with
CeO7

intermediate alumina (probably gamma) with NiO and
CeQa, possible spinel cuble NIAlz04

intermediate alumina (probably gamma or mixture
of gamma and delta)

mostly alpha alumina

mostly gamma alumina with NiO

intermediate alumina (gamma, delta, or theta) with
NiO and possible Ni

intermediate alumina with spinel cuble NIAIZ04,
possible NiO and CeQ2 or ZnS

mostly delta alumina with CeQz, possible NiO
and CeAlO3

mostly delta alumina with CeO2, possible NiO
and CeAlO3

Rear Face (UR3)_

intermediate alumina (gamma, delta, or theta) with
CeQg or ZnS

intermediate alumina (probably theta) with CeOz

intermediate alumina (gamma or delta) with CeO?

intermediate alumina (probably gamma) with NiO
and Cea, possible spinel cubic NiAl204

intermediate alumina (probably gamma or mixture
of gamma and delta)

mostly alpha alumina

mostly gamma alumina with NiO

intermediate alumina (gamma, delta, or theta) with
NIO and possible Ni

intermediate alumina with spinel cubic NiAlz0q,
possible NiO and CeOz

mostly delta alumina with CeO2, possible NiO
and CeAlO3

mostly delta alumina with CeQz, possible NiO
and CeAlO3


PAGE 4 CONVERTER SURFACE AREA ANALYSIS = A230,/0849~A-LL2

068 +
.063 +
.o60 +
: x
1057 +
xviiex) |
asa +
051 +
.o4a +
100s +
a2 + /x
y
Kereatecertocaetascstescatansatescataccetsccetecseteccctescctsceet
Yoa2 1066 1078 ‘oso {102 44
.048 .060 .072 .084 .098 108
Ne 3
cor .9709 P/ea

MEAN ST.DEV, REGRESSION LINE RES.MS.
X 08481 = 03514 X= 2,9115*Y-.07527 142E-8
Y 05494 = 01172 Y= ,32375*X+ .02752 1S8E-7

VARIABLE 4 P/PO VERSUS VARIABLE 2 X/V SYMBOL=X

Figure B-20. Plot of BET equation versus relative pressure for
Converter A230/0649-A-LL2

B-21

tee ee tee ee tee ne te

ee ee

+

2126


lo

TABLE 4, CATALYST SPECIFIC SURFACE AREA

Total Surface

Specific Surface Area, m2/g Area for Whole
Front Biscuit(A) Rear Biscuit(B) Biscuit,* m2

Biscuit No. LL1 = LL2 LL3) Powder URL UR2 Front Rear
A221/0310 2.3 2.7 3.5 3.8 4.9 5.1 2800 2300
A280/0005L 6.6 3.6 3.0 7.8 5.1 6.6 4900 2700
A220/0400 10.5 15.4 9.2 12.0 7.0 7.1 10600 4300
A230/0649 5.0 12.4 12.5 8.6 9.8 9.1 7700 5500
A246/0092 7.8 15.4 15.7 8.9 10.6 7.9 11200 6800
A240/0007 15.2 14.2 22.8 17.0 3.9 5.8 7400 2800
A240/0270 5.9 8.1 10.9 8.7 5.0 5.7 3400 3100
A254/0037 6.4 7.4 6.5 7.7 7.4 7.0 5400 6000
A254/0191 9.7 8.5 10.1 11.3 8.1 8.8 7500 6700

*Total biscuit surface area based on average of surface area and total weight of biscuit.
For partial samples, the total weight of the biscuit was estimated based on the amount
of sample received. The partial samples were A221/0310, A220/0400, A240/0007, and
A240/0270.


PAGE 4 CONVERTER SURFACE AREA ANALYSIS A220/0400-A [LL-2)

+ +

seeeteceeteces

watecvatenastecnetescetoccstoccatecessccetousetesen eens

0350
xX.

20325

tee tee

-0300

bees

20275

X/VU1-X)

0250

0225

0200

ee re rs

20175

tenes

0150

ee cc

Died 3

COR= .9993 P/PO
MEAN ST.OEV. REGRESSION LINE RESIS,

X 08481 = 03484 _ X= 3,5407*Y-,00323 796E-S

Y 02486 = .00984 Y= .28234%%+ 919E-5 83E-9

VARIABLE 41 P/PO VERSUS VARIABLE 2 X/V SYNBOL=x

Figure B-14. Plot of BET equation versus relative pressure for
Converter A220/0400-A-LL2

B-15


23

We hope that the results from these catalyst evaluations will help to answer some of
the EPA questions about relationships concening the catalyst condition. Please
contact us if there are additional questions, or if we can be of further assistance.

Prepared by: Reviewed by:
a
= ail
E kbar é Clade? po
E. Robert Fanick Charles T, Hare
Research Scientist Director

Department of Em'ssions Research Department of Emissions Research


PAGE 4 CONVERTER SURFACE AREA ANALYSIS

: x
125 + .
* Equation for Line
+ y= A+BX + Cx?
420 + Where:
. A = 83.4527
. B = 0.649277
: C_ = 0.051388
15 + R2 = 0.999711
30 :
& .
3 .
Q 10 +
‘2 .
[-} .
GI .
x .
8 105 +
Ss .
s
4 .
3 .
6 100 * x
95, +
: x
30, + A
tox
ceatVeeteccatessstecssteasetecseteseatessatecsstessstecsetecsstessetoce
4.50 7.50 10.5- 13.5 16.5 19.5 22.5
6.00 9.00 12.0 15.0 18.0 21.0 24,0
m4
CoRs .9929 Carrier Gas Concentration, % Nitrogen

MEAN ST.DEV. REGRESSION LINE RES.MS,
X 12,425 8.12818 = X= ,45073*Y-33 549 1.3978
Y 102,00 17,9017 Y= 2,1874°X+ 74,822 6,7824

VARIABLE 14 P/F VERSUS VARIABLE 2 X/V ‘SYMBOL=X

FIGURE 3. CALIBRATION KNOB SETTING FOR BET INSTRUMENT

setacerteccetececteccatesccteccstaccetavcctecectoccetoasetacestonsete XY

So

18


TABLE 2. LABELING PROCEDURE CODE

Code
A

B

UL
UR
LL

LR

Description

Upstream biscuit
Downstream biscuit

Upper left portion of biscuit
Upper right portion of biscuit
Lower left portion of biscuit
Lower right portion of biscuit
Upstream piece of section

Middle piece of section or downstream
when no middle piece taken

Downstream piece of section


PAGE 4 CONVERTER SURFACE AREA ANALYSIS A155/0841-1-A

weatancatoccetoveeteccet,

saveteccctoccatevcetecsetescetos

\

1730

e tee
od

21575,

1400

WV(I-X)

21225,

1050

20875

0700

Tree tee ee tee ee tee ee tee ee tee ee tee

20525
x

+
+
+
+
+
+
+
+

Govssstrssstessstessstessstessstessstec ataccataccetecceteccetoceetes
045 075 105 0135 0165 0195 225
.060 .0s0 120 150 2180 6210 240

Ne 4
CORS .9877 P/PO

MEAN ST.DEV. REGRESSION LINE RES.MS.
xX = .12177,—_ ,07987 X= 1.3907*Y-.00850 4305-7
Y .08387 05718 Y= .74681°X+ .00851 2236-7

VARIABLE 1 P/PO VERSUS VARIABLE 2 X/V ‘SYMBOL=X

Figure E-7. Plot of BET Equation Versus Relative Pressure for
Converter A155/0941-1-A (Powder Sample)

E-8


PAGE 4 CONVERTER SURFACE AREA ANALYSIS A254/0037A LL~1

+

. Y
102 + +
. x.
. :
.08g + i
oso + +
: x :
084 + +
WVit-x) :
: :
078 + +
. :
072 + :
088 + :
oso + :
x :
054 + +
aoteccetancetecsatoscctecsatesccteccetacestacestassetacsetucestessetecces
1088 1085 1078 1088 1098 $108 48
-050 .060 .070 .080 .0s0 109 110
Ne 3
Cons .9819 P/O
MEAN ST.DEV, REGRESSION LINE RES. HS,

x ,08482 .03484 X= 1,5055*Y~,03713 390E-7
Y .08100 02296 Y= .65358*°X+ .02557 169E-7

VARIABLE

1 P/PO VERSUS VARIABLE 2 X/V SYMBOL=K

Figure B-43. Plot of BET equation versus relative pressure for
Converter A254/0037-A-LL1

B-44


INLET

wR
317

OUTLET

Figure A-1. X-Ray Radiograph of A280/0005L


TABLE 7. ELEMENTAL ANALYSIS OF CATALYST POISONS BY X-RAY FLUORESCENCE

Biscuit Number P s Ca Mn Ni Zn Pb Others

ALzi/o “Li Otsu. 0.1520.01 0.2440.01 trace trace 0.02+0.001 0.040.002 Mg, AI,S1,K,Ti,Fe,Ce,Pt
A221/0310-B-LL_ 0.070.004 0.1640.01 0.080.004 0.0140.001 trace 0.0340. 002 1.2440.06 Mg, Al,S1,K,Ti,Fe,Ce,Pt
A280/0005L-B-LL 0.08*0.005 0.1340.01 0.090.005 0.0240.001 trace 0.0640.003 0.1340.01 = Na,Mg,Al,Si,K,Ti,Fe,Ba,Ce,Pt
A220/0400-B-LL 0.060.004 0.0940. 01 0.0840.004 trace 0.0140.0004 0.0440. 002 0.1140.01  Na,Mg,Al,Si,K,Ti,Fe,Ba,Ce,Pt
A230/0649-B-LL — 0.0440.003 0.1320.01 0.0840.004 trace 0.0140.001 0.0140.001 0.020.001  Mg,Al,Si,K,Ti,Fe,Ba,Ce,Pt
A230/0734-B-LL 0. 0540.03 0. 1040.01 0.0940,004 trace 0.0140.0005 0. 02+0.001 0.0140.001  Mg,Al,Si,K,TI,Fe,Ba,Ce,Pt
A246/0092-B-LL 0.0240. 002 0.5640.03 0.0540.003 0.0140.001 0.0140.001 0.0140.001 0.0240.001 — Mg,Al,Si,K,Ti,Fe,Ba,Ce,Pt
A240/0007-B-LL_ 0. 1040.01 0.3640.02 0.0740.004 0.0140.001 0.1040.001 0.0540.003 0.0440.002 Mg, Al,Si,K,Ti,Fe,Ba,Ce,Pt
A240/0270-B-LL —0.2240.01 0.3020.02 0.10%0.005 0.0240.002 0.1340.01 0.0720.004 0.1440,01 — Mg,Al,Si,K,T1,Fe,Ba,Ce,Pt
A254/0037-B-LL —0..0340.002 1.0140.05 0.070.004 0.010.001 * 0.0140.001 0.0140.001 Mg, Al,Si,K,T1,Fe,Ce,Pt
A254/0191-B-LL —0.0340..002 0.9140.05 0.050.003 trace * 0.0140.001 0.0240.001 Mg, Al,Si,K,Ti,Fe,Ce,Pt

trace - at detection limit
* - below detection mit

vas


PAGE 4 CONVERTER SUAFACE AREA ANALYSIS A221/0310-A = (LL-3}

1625

1500

ere rr a

21375

wee dee

«1250
HAN(1-K)

01125

bee ee tee

+1000

0875

re ee ee oe or

a rr

0750

&

.0625

see Ke ee

ate ceeteceeteceeteces Tense eens Tene abeweateneeTecceteceeteeeetone

2055 365 2075 5 2095 2105 2115
2050 «060 .070 JE «090 +100 2110

ie 3

COR= ,9993 P/PO
HEAR ST.DEV. REGRESSION LINE RESIS.

Xx ,08482 0.03484 X= .79438"Y- 00251 3325-8

Y 210994 .04383 Y= 1,2571°X+ .00331 52GE-a

VARIABLE 41 P/PO VERSUS VARIABLE 2 X/V SYMBOL=X

Figure B-3. Plot of BET equation versus relative pressure for
Converter A221/0310-A-LL3

Bt


PAGE 4 CONVERTER SURFACE AREA ANALYSIS TITANIUM DIOZIDE 7.05 + 0.7 M2/G

eteccctecnetsccsteccetocceteccetocssteccateccateccetecsetascetecestecvete
.084 + Y
: x :
.078 + +
072 + +
068 + t
XIX) :
.oso + +
: x :
: :
056. + +
04g + +
042 + :
38 + xX :
TeV te ccatecsctocactecsctecsctecsctecsctecsctecsctecsctecnctscseteasets
toad ‘0s 1086 ‘07a ‘oso 2102 wa” Tes
3 .048 .060 .072 .084 .098 .108 120
Ne
cOR= 9974 p/po

MEAN ST.OEV. REGRESSION LINE RES.MS.
X 08482 03514 X= 1,6081*Y-,00884 1286-7
Y .05811 = .02179 Y= ,81851"X+ .00577  492E-8

VARIABLE 1 P/PO VERSUS VARIABLE 2 Xv SYMBOL=K

Figure D-5. Plot of BET equation versus relative pressure for
Titanium Dioxide 7.0540.7

D-6


RUN DESCRIPTION:

ALITATA

- AUTO CATALYST

DATE OF XRAY ANALYSIS! 04/30/37
SAMPLE TYPE: BRIQUETTE

SITE IDs N/A

MISCELLANEOUS “NFO NONE

SAMPLE ‘ECIUEN' Ni Le

DAMPLE ID ALS4/0027-H

ELEMENT DETN LIM

Na oO «L321 26E-01

MG 1 216244E-00

AL »2544.31E-01

a1 7364S LE-O2

° -248131E-03

= »160233E-02

CL Xx VL7ISLE-O3 -.A7FLS4E-02
F «210467E-03 2046475

CA + 172297E-03 2068959

TI + 265C52E-03 ~24552

v x + 748457E-03 -.100272E-02
CR »1435902E-02 . .148187E-01
MN + 636156E-03 -6146519E-02
FE - 7445 9SE-03 2114499

co oO . 2835736 - + 308914E-03
NI Oo 7ESE-O3 «7O4516E-03
cu x « 232864E-03 —. S79 264E-04
ZN 2297 S5E-03 »105716E-a1
BE OX + 244432E-03

BR X »lOS321E-02

= Xx + 462.224E-02

Mo Xx - 64073E-02

co oo » LES50RE-03

SN OX + 1041'53E-02

3B OX » S007 75E-€

RA X 747 225E-

Te « 33594 E-€

PT . 1O03E-0

HG X + 643 109E-03

FR » 667627E-O8

TOTAL DETECTED BY XRF

= 40,2821

C11


TABLE 8 SURFACE WEIGHT PERCENT OF ELEMENTS
NORMALIZED TO ALUMINUM

Biscuit .. Normalized Weight Percent
Number _P Ss Ca Mn Pb Si Zn
A180/0094 17.40 0.21 3.61 1.24 82.64 0.25 26.13
A193/0908 3.09 2.80 0.54 0.36 1.55 2.84 3.75
A218/0045 15.06 2.04 4.08 0.91 42.56 2.26 = 26.03
A218/0045X 15.65 10.17 2.48 0.75 34.38 11.44 32.53
A218/0045X* 0.20 0.01 0.04 ND 0.09 0.02 0.07
A218/0068 49.54 2.89 11.04 1.23 155.73 3.42 97.31
A220/0392 3.34 2.09 0.77 0.08 5.17 2.23 3.80
A220/0392* 0.12 0.02 0.01 ND 0.03 0.02 0.02
A220/0810 11.45 0.68 2.95 0.10 8.15 0.80 18.44
A221/0152 10.90 24.96 2.58 5.20 19.51 24.36 20.65
A221/0204 12.64 1.55 2.41 0.24 14.88 1.94 37.71
A221/0447 2.03 2.94 0.28 0.12 13.07 3.14 2.82
A221/0447* 0.03 0.04 0.003 ND 0.02 0.06 0.002
A230/0177X 0.56 0.37 0.09 0.05 0.27 0.42 0.45
A230/0177X* 0.05 0.03 0.01 ND 0.02 0.05 0.03
A230/0636X 1.68 0.23 0.23 0.08 3.09 0.27 1.60
A240/0016L. 2.40 0.61 0.35 ND 8.58 0.72 3.62
A240/0016L* 2.45 0.10 0.04 ND 0.87 0.12 0.14
A240/0102 3.47 1.20 1.01 0.08 3.42 1.33 3.93
A240/0141L 9.12 37.62 0.85 4.03 6.20 30.63 7.17
A240/0153 1.71 0.10 0.13 0.27 1.15 0.11 1.02
A240/0334L 1.74 0.41 0.03 0.03 1.46 0.45 0.31
A249/0169-1 1.48 0.58 0.08 0.05 1.08 0.54 0.18
A249/0169-1* 0.05 0.01 0.01 ND 0.04 0.02 0.02
A249/0169-2 1.76 4.04 0.10 0.12 1.83 3.56 0.39
A249/0169-3 1.29 0.41 0.87 ND 14.60 0.56 0.73
A280/0001L 9.04 2.19 2.27 1.68 3.60 2.49 13.21
A155/0941-1 1.64 0.60 0.67 0.51 0.70 0.64 2.15
A155/0941-2 0.72 0.52 0.21 0.07 2.26 0.52 1.32
A207/0101 0.35 0.07 0.01 0.07 0.03 0.08 0.05

*Rear Face of A biscuit for comparison within each engine family
ND - none detected

15


PAGE 4 CONVERTER SURFACE AREA ANALYSIS ALUMINA PART. 3,04 + 0.25

+, +

ctoccetecceteccoteccetsccetecceteccetocee

1780
01625,

«1500

XWV(1-X)
01378

«1250
1128
1000

0875

/

x

/

Yrvccctessatesccteccotessetace

042 054 088 .078 oso 102 114
048 060 072 084 2096 108
Ne 3

CoR= .9979 P/PO
MEAN ST .DE¥. REGRESSION LINE RES.MS,

X 08482 9.036514 X= .74554°Y-,01459 105E-7

Y .13308 04708 Y= 1,3358°X+ 02008 187E-7

@
VARIABLE 1 P/P) VERSUS VARIABLE 2 X/V SYMBOL=X

Se te ee tee ee tee ee tee ee tee ee tee ee tee ee tees

Figure D-4. Plot of BET equation versus relative pressure for
Alumina 3.0440.25

D-5

atececteccetescstesectsccctecseteseet,

soveteccctoncetassestonvctesvots

rs

ete ee te eee tee ee te eee tee

a ar

eats

2128


PAGE 4 CONVERTER SURFACE AREA ANALYSIS ALUMINA PARTICLES (285 + 11 12/G]
ceectecsctaccctesceteccstecsstecssteccetecestecsctessstessetecsstecset ead
00s + .
: qt
: :
005 + +
004 + +
.004 + :
UX) :
003 + +
: :
: x :
00g + +
: :
002 + }
. x .
.ooz + :
Dx :
.09t vA :
y :
we caPecnetaccetecnetocceteccetessctesactscceteccatesectecsetecsetescetees
1048 {078 1108 1135 1165 1198 1238
080 .o80 120 .180 180 210 240
Ne 4
cor .9997 Peo

MEAN

ST.DEV. REGRESSION LINE RES.MS.

X =  .12179 07988) X= 51,135*Y-,01014 602E-8
Y ,00258 .00156 Y= .01SS4°X+ 200E-6 23-10

VARIABLE

41 P/PO VERSUS VARIABLE 2 X/V SY¥MBOL=X

Figure D-9. Plot of BET equation versus relative pressure for

Alumina 265411

D-10


PAGE 4 CONVERTER SURFACE AREA ANALYSIS A240/0270-1-LL = (LL-3)

+

0830

20585,

0560

0525

X/V(1-X)

0480

0455

0420

20385

x

/

AAV coteccetecsctocceteccateccatscsetessetocceteccetessetecceteces
2042 054 066 2078 030 102 0114
048 060 2072 «084 036 108 2120

Ne 2
COR= 1,000 P/PO

Se

20350

MEAN ST, DEV, REGRESSION LINE RES.MS,
X 08351 .04962 X= 2,8177%Y-.04702 0.0000
Y 04886 01896 Y= ,38202*X+ .01796 0.0000

VARIABLE 1 P/PO VERSUS VARIABLE 2 X/V ‘SYMBOL=X

Figure B-39. Plot of BET equation versus relative pressure for
Converter A240/0270-A-LL3

B~40

%
‘+

De te ee ee ee te ee te te eee te ee te ee te ee tee

Dy



PAGE 4 CONVERTER SURFACE AREA ANALYSIS  A254/0037A {LL-3)

+
:
:
¢
%
H
H
>
+
;
:

2078

072

VAX}

048

2042

036

ee oe ci ee ce acc

.<

ateceetsvcctoscetescetovcctecestecantecceteccetsces

055 085 1075 088 098 +105
+060 .060 -070 .080 030 -100 110
te 4
Cons .98e4 P/PO

MEAN = ST, DEV, REGRESSION LINE RES.MS,
X 08482 9.03484 X= 1,5041*Y~,00297 314E-8
Y 05637 02315 Y= .68996°X+ .00205 13SE-8

VARIABLE 1 P/PO VERSUS VARIABLE 2 X/V SYMBOL=X

Figure B-45. Plot of BET equation versus relative pressure for
Converter A254/0037-A-LL3

HaeneteceeTeneeteses

Fevcatevcatecsetocsateccuteccetscsatoccutevses
+

%

i ee ee a


TABLE 11. SPECIFIC: SURFACE AREA OF SELECTED POWDER SAMPLES

Specific Surface Total Surface Percent
Converter Area, m2/g Area, m2 Difference?
_Core Powder Core Powder
A221/0447-A 4.8 5.8 5300 6400 20.8
A221/0447-B 8.0 6.0 3800 2800 -25.0
A220/0810-A 4,7 9.4 4200 8500 100.0
A220/0810-B 4 7.4 5900 4600 21.3
A230/0177X-A =. 21.4 14.9 17,100 = 11,900 30.4
A230/0117X-B 14,3 12.0 9400 7900 -16.1
A155/0941-1A 346 6.0 45004 76004 66.7
A155/0941-2-A 3,1 2.3 15008 =. 11004 -25.8
A240/0141L-B o.7 8.8 4900 4400 -9.3
A240/0334L-A 13.9 12.7 8000 5100 -36.2

atotal surface area lhased on biscuit weights of converter A155/0926
bbased on specific surface areas


PAGE 4 CONVERTER SURFACE AREA ANALYSIS ALUMINA POWER 14,0 + .6

soenteccetscvoteccotecvotoccetos

: 7

0675

Pr ee ee

wv(1-x)
0525

20375

0225

:
:
:
:

ee ce ee ee ee ce 2 ae

ateceets

180
Ne 4
Cone .9994 P/PO

MEAN ST.DEV. REGRESSION LINE RES.MS.
X 12179 07988 «X= 3,2683°Y-,01722 1185-7
Y 04253 .02437 Y= .30560*X+ ,00531  108E-8

VARIABLE 1 -P/PO VERSUS VARIABLE 2 X/V SYMBOL=X

Figure D-6. Plot of BET equation versus relative pressure for
Alumina 14.010.6

D-7


INLET

SWR
317

OUTLET

Figure A-l. X-Ray Radiograph of A280/0005L


PAGE 4 CONVERTER SURFACE AREA ANALYSIS A230/0649-R = UR-2

056

«052

wv(1-x)

048

2044

2040

ee a ee a ae are er ay

x
ateVKatancatasectensetescstessatassetecretaccstessetesnatassetecest
042 054 056 078 030 102

2048 060 072 2084 086 2108

.
032 +

Nw 3
COR= .9849 P/PO

MEAN ST.DEV. REGRESSION LINE RES.MS.
X 08462 = =.03514 X= 2,0812*¥-.01410 740-7
Y ,04789 01679 Y= .47062*X+ ,00807 189E-7

VARIABLE 4 P/FO VERSUS VARIABLE 2 X/V SYMBOL=X

Figure B-24. Plot of BET equation versus relative pressure for
Converter A230/0649-B-UR2

B-25

x

2120

FH eeeeteceet, ateccetenceteneete XY teceete

ce Ceres

ate
2126


PAGE 4

1.50

1,35

1,20

CONVERTER SURFACE AREA ANALYSIS ~ ALUMINA (0,780 12/G)

acccteccetieceteccstecceteccetoccstascetacsotsccetoccstecesteccetavceteey

x“

+ +
+ +
+ +
1.05 + i
xVUG-X) .
900 + +
: x :
730 + +
: x :
.soo + :
480 + +
. .
was :
.300 Y +
seeateasetoccatesectsccetaccstocsatencetescatescatasentensetessstssestacs
1048 1078 1168 1138 1165 1198 1238
.083 .o90 .120 .180 180 .210 240
te 4
COR .9984 P/PO
WEAN ST.DEV, REGRESSION LINE —AES.NS,

X 12178 = 607987 X= .17000"Y-.01924  305E-7
Y 82955 .48792 Y= 5,.8837*X+ .11548 00105

VARIABLE

4 P/PO VERSUS VARIABLE 2 X/V SYMBOL=X

Figure D-2. Plot of BET equation versus relative pressure for

Alpha Alumina 0.78 NBS

D-3


PAGE 4 CONVERTER SURFACE AREA ANALYSIS A280/CO05L-A {[LL-1}

seteecctecccteccetencaTesceteccatesceteccetovcatscsastorveteacsTesneTevees

.034 Y
. x
.o7a + :
.o72 + ‘
.ogs + i
WV) .
.o60 + :
1054 + i
.oag + i
042 + +
x :
1036 Y :
ey to : :
.950 .030 .079 1230 .090 108 110
od 3
con= 1.000 °/PO

EAI ST.DEV. REGRESSION LINE RESUS,
X 08482 .03484 X= 1,5195*Y-,00692 216-9
Y  .06037 .02293 Y= .65810*X+ ,00455 935-10

VARIABLE 1 P/PO VERSUS VARIABLE 2 X/V SYMBOL=K

Figure B-7. Plot of BET equation versus relative pressure for
Converter A280/0005L-A-LL1

B-8


TABLE 12. QUALITY ASSURANCE FOR XRF (SAMPLE A220/0810-B)

Work Assignment Percent

Element 20a gb Difference
P 0.4840,02 0.5040.03 4.2
Ss 1.15£0,06 1.0940.05 -5.2
Ca 0.2040.01 0.2040.01 0.0
Mn 0.0140.001 0.010.001 0.0
Ni 0.020.001 0.0140.001 -50.0¢
Zn 0.2540.01 0.2540.01 0.0
Pt 0.3740.02 0.36*0.02 -2.7
Pb 0.1720.01 0.1840.01 5.9
Others Na,Mg,Al,Si, Na,Mg,Al,Si,

K,Ti,Fe,Ba,Ce K,Ti,Fe,Ce

4EPA Contract 68-03-3192, Work Assignment No, 20
bEPA Contract 68-03-3353, Work Assignment No. 8
CLarge percent difference due to low value. Probably not
significent

21


PAGE 4 CONVERTER SURFACE AREA ANALYSIS A240/0078 = UR-1

eteccateccctecnctavcctoccetacsetesccteccntsccetacsatacsetossateaseteeVete

: x :
0130+ +
. .
124 +
wat i
X/VEA-X) | :
. + +
: x :
08 + i
08 + ;
07 + :
og + pa
tx :
ltasVeteseeteceatesssteccetesseteccetecsetecsetecestasseteceet :
1043 1054 1068 1078 tosa {102 M4
.048 .060 .072 084 .096 108
Ne 3
COR= .9897 P/PO

MEAN ST.DEV. REGRESSION LINE RES.MS,
xX 08462 =,03514 X= ,88857*Y+ ,00107 163E-8
Y 09402 = ,03854 Y= 1,1247*X-,00115 206E-8

VARIABLE 4 P/PO VERSUS VARIABLE 2 X/V SYMBOL=X

Figure B-35. Plot of BET equation versus relative pressure for
Converter A240/0007-B-UR1

B-36



TABLE 3, CONVERTER WEIGHTS

Converter Whole Biscuit Weights, 2
Number Coaverter, Ibs. Upstream (A) Downstream (B)
A221/0198 -- 264.4/277.8 112.4/108.3
A221/0310 -- 257.3/229.0 116.3/110.4
A280/0005L 10.00 1121.6 463.1
A220/0400 - 216,3/237.7 155.6/149.0
A230/0649 - 188.4/197.5 145,5/144.0
A230/0734 - 189.0/192.2 138.5/155.5
A246/0092 11.37 865.7 731.0
A240/0007 - 106.9/104.9 144.6/144.5
A240/0270 - 99.9/103.5 135,4/152.0
A254/0037 9.65 797.5 838.6
A254/0191 11.58 794.0 790.00

Note: Converters A280/0005L, A246/0092, A254/0037, and A254/0191 where
whole converters. All others represent lengthwise quarters. The first listed
weight represents the lower left portion and the second weight represents the
upper right portion.


APPENDIX D

BET EQUATION VERSUS RELATIVE PRESSURE
FOR QUALITY ASSURANCE STANDARDS


PAGE 4 CONVERTER SURFACE AREA ANALYSIS 280/000!
a etewns eeeetesectessatesasTassetesnatesnetas
.o7a +
1072 +
066 +
.oso +
XOX).
: x
05g >
04g +
042 +
03g > /
ix
Y
2030 +
woteecetasnatacsetscsstecseteccstecsetenasteseatesent
1085 1085 1075 2985
+050 .060 1970 .080 .ogo
Ne 3
CoR= .9987 7/0
WEAN ST,DEV, REGRESSION LINE —AES.IS.
X 08482 .d3aB4 .5223Y+ 1116-3 355E-3
Y 05584 (02283 Y= .65513°X+ 773E-7 2826-8
VARIABLE 1 P/P2 VERSUS VARIABLE 2 X/V

SL-B

weteeeet

2095
«100

SY'iBOL=K

(UR-2]

+

+.
105

Figure B-12. Plot of BET equation versus relative pressure for

Converter A280/0005L-B-UR2

B-13

+

sataceetonnes

2110

2115,

x
tenes Fe

tee

tee tee

Ce ee a


PAGE 4 CONVERTER SURFACE AREA ANALYSIS GRAPHITIZED CARBON BLACK 71.3 + 2.7

cvcteccatavcctavcctecsctensetescataccctescotercetacsstessatessetacsstoce

20135
0120
20105
XW/V(1=X)
.00s0
20075
.0080

0045

-0030

:
:

ate ccctecceteccetecceteccoteccetocest

eaetonnet

090 2120 «180 180 2210
Ne 4
COR= 1.000 P/PO
MEAN ST.DEV. REGRESSION LINE RES.MS.
X 12178 = ,07887 X= 16,791*Y+ SOSE-6 S80E-9
Y 00722 00474 Y= .05955*X-299E-7 21-10

VARIABLE 4 P/PO VERSUS VARIABLE 2 X/V SYMBOL=X

Figure D-7. Plot of BET equation versus relative pressure for
Graphitized Carbon Black 71.3 NBS

seeetooes

105 2135 +165 2195 +225

+

/

tee

2240

tee

tenes

ee ee ey

+
+


PAGE 4 CONVERTER SURFACE AREA ANALYSIS = A220/0400-A~-LL3

+ +eeect,

atecnetescetacnetaccatesestscsctascotesesteccetacsetocsstesvet

x

0300

0625

+0750

wWVUI-X)

0875

+0525

0450

20375

*

ee ee ee ee ee ce rd

~~

Gast oteveatoccetecccteccetes
«042 2054 066 .078
048 080 2072
N= 3
COR= .9893 P/PO

MEAN ST.DEV. REGRESSION LINE RES.MS.
X 08462 «= .03514 X= 1,2771°Y+ 00345 334E-8
Y 06355 02750 Y= .78198*X-.00262 20SE-8

VARIABLE 4 P/PO VERSUS VARIABLE 2 X/V SYMBOL=X

Figure B-15. Plot of BET equation versus relative pressure for
Converter A220/0400-A-LL3

B-16

senate

‘+
&

ee