Document byG0E35rOy0xmQpEngEzj5m21
FILE NAME: Oil Industry and American Petroleum Institute (API) DATE: 1955 Oct 1
DOC#: API129
DOCUMENT DESCRIPTION: API Research Project MC-1 - Tabular Summary of Current and Completed Biological Experiments - The Kettering Lab
TABULAR SUMMARY ' OP
CURRENT AND COMPLETED BIOLOGICAL EXPERIMENTS
October 1, 195$
Department
The Kettering Laboratoryin the
of Preventive Medicine and Industrial Health College of Medicine
University of Cincinnati Cincinnati, Ohio API
06476
TA3LES
labi I
- Carcinogenic Potency of Various Fractions from the Refining of Petroleum
Table II - Control Experiments with Various Solvents
Table III - Experiments Involving the Application of Solutions of Methylcholanthrene in Various Solvents Upon the Skin of C3H Mice
Table IV
- Experiments Involving the Application of Solutions of 3enzopyrene in Non-accelerating Solvents to the Skin of C3H Mice
Table V
- Experiments to Determine the Potency of Mixtures of Polycyclic Hydrocarbons in Technical White Oil for the Skin of C3H Mice
Table VI
- Experiments Involving the Application of Solutions of Methylcholanthrene in Dodecylbenzene Upon the Skin of Mice
Table VII - Accelerating Activity of Various Solvents on Rate of Induction of Tumors by Dissolved Benzopyrene (BP) in C3H Mice
Table VIII- Effect of Early Exposure to Accelerating Solvents on Results of Subsequent Exposure to Carcinogen
Table II
- Experiments to Determine the Carcinogenic Promoting
Activity of Various Materials for the Skin of
C3H Mice
.
(
Table X
- Effect of Termination of Exposure of C3H Mice to Catalytically Cracked Oils at a Critical Phase of the Experiment
Table XI - Experiments to Determine the Potency of Certain Polycyclic Hydrocarbons for the Skin of C3H Mice
Table XII - Experiments on the Retardation of Tumor Formation by Washing
PI 06477
INDEX TO PPCCESSES
Process___ _ ^on_catalytic cracking of virgingas oil Non-catalytic cracking ofcatalytic gasoil Steam cracking Viscosity breaking pubbs coking gatch coking Delayed coking Naphtha reforming polyforming Hydroforming Thermofor catalytic cracking (T.C.C.) Fluid catalytic cracking (F.C.C.) Houdry Cycloversion Solvent extraction Straight run distillation Fractional distillation Lubricating oil Wax pressing Filtration dewaxing Desulfurization by catalytic hydrogenation Acid treating Viscosity effects Fuel oil blending Diels-Alder reaction Air oxidation
Solvent extraction with concentrated HgS04 Fractionation of API-12 Chromatography
Table I ya5
Number
1
1
3 3 3 3 3
[. 1;
6 3 3 9 9 10,13 11
11
11 11 12 12 12 13,15,16
II4.
16 16 17
-'* .- -'c* v
INDEX TO TABLE I Process
? D 7 9
3-3 3-1+
3-5 5-6 - 12
8-l2a
3-13 6-13& - i
9-11+ - 15
6-16
8-17 3-18
8-19 3-20
8-21 8-22
9-23a - h 3-21+
3-2 5 a
8-25b 8-26a - d
8-26e - n
fl-26n-l 3-26-2
8-26-3
9
10 11 12 12-2
12-7
12-8
13 lb
17
18
19
20 20-1 21 22
27
23-1 23-2 21+
25 25-1 26
27 23
29
'ion-catalytic cracking of virgin gas oil
Non-catalytic cracking of virgin gas oil
T. C. C.
P. C. C.
Filtration dewaxing
Dilution of API-8
Chromatograpny
Fractional distillation
Diels-Alder reaction
Fractional distillation Chromatography
Fractional distillation
Dilution of API-8
Chromatography Fractional distillation Solvent extraction with Solvent extraction with
Dilution of API-8
Chromatography
of API-8 of API-8 of API-8
of API-8 cone. HaS04 cone. HaS04
Diels-Alder reaction
Chromatography
Diels-Alder reaction
Diels-Alder reaction
Fractional distillation
Fractional distillation
Diels-Alder reaction
Chromatography
Chromt ography
To Co Co
To C Co
Koudry
F. C. C.
Chromatography
Fractionation
Fractionation
Polyforming
v
Solvent extraction
Solvent extraction
Viscosity
Naphtha reforming
Non-catalytic cracking of catalytic gas oil
Dilution of API-20
Desulfurization by catalytic hydrogenation
Cycloversion
F. C. C.
Solvent extraction with cone. HaS04 Solvent extraction with cone. HaS04
Non-catalytic cracking of catalytic gas oil
Distillation
Dilution of API-25
F. C. C.
Solvent extraction
Delayed coking
Catalytic feed to non-catalytic cracking
Tac le page
Number
1 1
5
6 11 6 6
13
13 13 17 13 b
6
13
16
16
6
+ 15 .
6
15 15 13
11+
15
11+ 11+
5 5
8
7 7
16
16
1+
9 9 3
1+ 1 1 20 8
1,7
16
16
1
7 7 7 9 3
1
API 06479
5c i?le 'lumber
3
31
32 33 3*+ 35
36
37 38 39
1*0 1*1 1*2
1+3 1+3-1 i+l+ i+5
1+6
1+7
1+8
1+9 50
51 52 53 51+ 55 56 57 58
59 60 61 62
63 61+ 65
66
67
68
69
70
71 71-1
71-2
72
73 7i+ 75 76
77 78
79
81
INDEX TC TAPIS I
Process
Non-catalytic cracking of catalytic gas T. C. C. Wax pressing Delayed coking Houdry Non-catalytic cracking of catalytic gas T. C. C. Polyforming Catalytic feed to non-icatalytic cracking Non-catalytic cracking of catalytic gas T. C. C. Delayed coking Fa Ce C a Fa C a C Dewaxing
F. C. C. Non-catalytic cracking of catalytic gas i F. C. C.
Non-catalytic cracking of catalytic gas 1
F. C. C. Hydroforming Houdry Houdry Dubbs coking Dubbs coking Catalytic feed to non-catalytic cracking Non-catalytic cracking of catalytic gas Straight run distillation Wax pressing Naphtha reforming Non-catalytic cracking of virgin gas oil T. C. C. Non-catalytic cracking of catalytic gas Acid treating Houdry
Non-catalytic cracking of catalytic gas 1
Non-catalytic cracking of virgin gas oil Viscosity breaking Viscosity breaking Fa C a C a Polyforming Solvent extraction T. C. C. Chromatography Chromatography Non-catalytic cracking of virgin gas oil Fa C a C Delayed coking Solvent extraction Naphtha reforming Hydroforming T. C. C. Straight run distillation Houdry
Table I
Page Number
1
5 11
3 1,8
1
5
k22
5 k 7 7 7 2.7 2
22.7
1
\
8
3
2 3 2
9,11 11 k 1
25
12
2.8
2
1
3 3 7
9 5 17 17
1
7 3 9 i+ k 5
98
API 06480
I . .noie mb er
82
63 n 8^-1
S3-2 81+
8 86
87
88
89
8999--1 2
89-3
90
91 92
93 9b
96 9978
99
100 100- 1 100-2 101 102 103 10I+ 10? 108 109 110- 1 111- I+ 111-l+a 111-l+b
111-5
111-6 111- 7 112- 1 112-3
113
111+
111+-1 115 117
118
119 120 120-1
INDEX TO TABLE I
_________________ tr o c o a a
T. C. C.
Air oxidation
Air oxidation
Chromatography-
Delayed coking
F C C
Steam cracking
Batch coking
F. C. C.
F C C
Diels-Alder reaction
Diels-Alder reaction
Chromatography
Delayed coking
Catalytic feed to non-catalytic cracking
Non-catalytic cracking of catalytic gas oil
Non-catalytic cracking of catalytic gas oil
Non-catalytic cracking of virgin gas oil
Delayed coking
Delayed coking
Delayed coking
Lubricating oil
Lubricating oil
Lubricating oil
Lubricating oil
F. C. C.
F. C. C.
Delayed coking
F. C. C.
Straight run distillation
Non-catalytic cracking of virgin gas oil
T. C. C.
Fractional distillation
Fractional distillation
Fractional distillation
--'
'
Fractional distillation
Fractional distillation
Dilution of API-111-1+ '
Dilution of API-111-1+
Fractional distillation
Fractional distillation
Fuel Oil blending
Straight run distillation
Viscosity effects
Straight run distillation
Straight run distillation
Fuel oil blending
Fuel oil blending
Straight run distillation
-
Diels-Alder reaction
Table I Page
Number
5
.11+
11+ 11+
3 7 3 3 7 7
16 16
7 3
2,8 2 2 1
13
+
1+ 11 11 11 11 8 8
6 9
1
5
10 10 10 10 10 10 10 10 10 12 9,12
12 10 10 12 12
9 16
API 06481
IMOGENI7 F!TENCY OP VARIOUS FRACTIONS FROM THE REFINING OF PETROLEUM
API HUMBER
DESCRIPTION OF
EXPERIMENT
1RAVITY
API]
FRACTION DISTIL LING <750F. {%)
SCHEDULE
OF
APPLICA
BENZO TIONS
PYRENE ]no./week
{%)
- mg.)
RELATIVE
INCIDENCI CARCINO
OF
GENIC
TUMORS POTENCY,
% - week] PMC
on-cat,alytic cracking
nf VIJgin gas oil
2 Cracked Side 21.2
stream
0.0002 1 - 100 0-75
-
6 Cracked residuum 5.2 33
0.013 3 - 100 72-30 rw 0.08
59 Cracked residuum 8.5
0.005 3 - 100 82-69
0.02X
65 Cracked residuum 6.6 1+3.8 0 .01+ 3 - 100 89-29
0.11X
72 Cracked residuum 9.6 35
0.06 3 - 100 73-18
0.21X
91+ Cracked residuum 10.1+ 35
0.02 3 - 100 80-39
0.09X
108 Cracked residuum 2.3 32
0.12 3 - 100 71-28
0.12X
108
3 - 5 100-52 o .o 5 .o i
Non-catsalytic cracking of cal;alytic gas oil
20 20
20-1
Cracked residuum 1+.7 50% oil No. 20,
50% dodecylberzen 9
23 FCC gas oil feed 26.7 23
21+ Cracked residuum 5.9
from No. 23
29 TCC gas oil feed 15.7
30 Cracked residuum 8.5 from No. 29
31+ Houdry gas oil 28.0
feed
35 Cracked residuun 2.7 from No. 3l+
51
78.5 32.3 73 36
35
0 .21+
3 - 100 3 - 100
3 - 100
100-22 90-21
100-25
ryj 0.18
0.17X
rJ 0.18
0 .01+3 0 .21+
3 - 100 2 - 100
3 - 100
100-19
91+-28
100-15
AJ 0.21+ 0 .22!;^
nJ 0.1+
0.10 0.23
0.011+
1 - 100 1 - 100
81+-30
100-33
3 - 100 81+-32
0 .3l.Oi+
- 26-.' 02
1
<0 o . l
0.18 3 - 100 100-20 A) 0.15
API 06482
TABLE I
e.)
'ccsEr:: f :t e n c y of v a r i o u s f r a c t i o n s f r o m t h e r e f i n i n g o f p e t r o l e u m
'-a _ '
' " --
1 ..... ----1-
.... ' -----------
____
API
SAlffg
ffirMBFR_
DESCRIPTION OF
EXPERIMENT
Total cracking 3S charge; combin
ation unit
1RAVITY
PAPl!
FRACTION DISTIL LING <75f .
(JO
SCHEDULE
OF
APPLICA
BENZO TIONS
PYRENE [no./week
(JO
- mg.)
RELATIVE
INCIDENCII CARCINO
OF
GENIC
TUMORS POTENCY,
- weeki ?MC
L6.1 32.2 J10.005 3 - 100 62-58 aJ 0.06
Cracked residuum) 7.8
from No. 38
31.0
0.03
3 - 100 56-21+ /'Z 0.15
FCC decanted oil]l5.2 feed
31.1
0.15
1 - 100 91+-1+0
0.22X
Cracked residuunj-1.7 from No. 1+1+
26.1+
0.38
1 - 100 88-1+1
0.18X
FCC gas oil feed
87.9 0.03 3 - 100 100-21+ ^ 0 . 1 5
Cracked residuum from No. 1+6
76 0.21 3 - 100 93-17 rJ 0.22
Total cracking charge
93.9 0.01+1 3 - 100 IOO-36 r J 0.09
Cracked residuum from No.
55.9 0.23 3 - 100 89-19 ro 0.21
Cracked residuum
Houdry gas oil feed
66.8
1+8.5
0.05 0.05
3 - 100
3 - 100
3 - 100 3 - 100 2 - 100 3-20
3 -5
88-26
89-26
100-19
89-28
100-33 100-1+5
86-37
f j 0.20
O0 -1TP2*- .0^12
0.184.03 0.21X
.3.51:82
0.11!o3 o.0 9 !;8 |
61+
from No. 63
52.5 0.11 3 - 100 100-23 0 .1 7-.0 2
FCC gas oil fe<
80.1 0.037 2 - 100 95-23
Cracked residua from No. 91
70.5 0.072 2 - 100 91-23 o.3i!;8|
93 Cracked residuumj 7*9 87 0.03 3 - 1 0 0 91+-1+0 0 .07-.01;
API 06483
AaJ3 --
i
V.'S"]"'"~ PnOnTENCY OP VARIOUS FRACTIONS FROM TRR REPINING O? PETROLEUM
API 06484
TA3LE I (page 5) :n c g e n i c p o t e n c y c f v a r i o u s f r a c t i o n s f r o m the r e f i n i n g cf p e t r o l e u m
API
sample
jjMBER
DESCRIPTION OF
EXPERIMENT
SCHEDULE
FRACTION
OF
DISTIL
1APPLICA- INCIDENCE
GRAV( LING BENZO TIONS
OF
ITY 750F. PYRENE (no./week TUMORS
APX (%)
(*) - mg.) (#-weeks)
RELATIVE CARCINO
GENIC POTENCY,
MC
jhermofor Catalytic tracking
'racked residuum 20.2 a ; lo o
9 Cracked residuum I8.i| 97 9
10 bracked residuum 11.6 56.7
10
31 bracked residuum 1 6 .0
63
36 Cracked residuum 21.9 N 50
UO Cracked residuum 19.8! 77.2
t
71 Cracked residuum 22.a 77
71
71 7U
71 71
78 Cracked residuum 16.1 45.7 82 Cracked residuum 13.6 25.7
82
0.019
0.07
0.23
0.65
0.18
0.09 0.10
o .4 r
0.53
1 - 100
3 100 3 100 1 100 1 100
1 100
1 100
1 - 100
l 100 1 20
2 20l
2 201
25 15 1 100
1 100 1 10
11-56
100-47
100-41
o .o 5 .o i /V 0.06
94-39
90-31 100-32
94-44 100-42
0 .3X
a ^o .5
u,J'-.09
0 `i1Q9-+.*o^5 0 .16X
90-22 0.52I .05
90-37 -36;g|
100-27 100-25
0.2.02
U0 'd2l1+-.*Q^2
94- 36 O.I9+ .05
.03
85-70 O.lOi.03
88-20 *60-.*
95- 34 o .3o !;8
100-50 o .2o !;i
60
Sidestream
109 Sidestream
;249 100 24*1
<.0004 3 - 100 0.35 3 - 100
57-48 93-25
r J 0.031 0.14.03
API-71 involved repeated application until death. API-71A involved
repeated application only until appearance of papilloma in each
mouse. No significant difference in the average time to the
appearance of gross carcinoma was noted.
______ __ ______
API 06486
TABLE I (page c) ^ RCliiOC'ENIC POTENCY OP VARIOUS FRACTIONS FROM THE REFINING OF PETROLEUM
sample
DESCRIPTION OF
EXPERIMENT
FRACTION
DISTIL GRAV LING
ITY <750F.
;a p i ' (%)
SCHEDULE
OF
IAPPLICA- INCIDENCE
BENZO TIONS
OF
PYRENE (no./week TUMORS
{%) - ag.) ({6-weeks )
RELATIVE CARCINO
GENIC POTENCY,
PMC
pMd Catalytic Cracking
Cracked residuum 11.:. 75
0 .1+2
i -i8-:26
- -\U y 0.6
0.2X
0.1+01.03 i-fiL
-57-:i3
91-1+0 100-32
884+8
100-18
O.ZlUos 0.23.05 o.37t;^ 0.20!;OJ
.25:;g|
8-1+
8-16
8-21
$ 0 % API-8, 50^ (white oil + W. Texas
residuum)
-
50# API-8,
sec .-amylbenzene
50% API-8, $ 0 % API-8-21+
Chromatography of API-8 :
Aromatics
8-21+ Colorless fraction
257 8-17
Solution of 0.239)6 BP in API-8-21+ Reblend of all fractions
3 - 100 1 - 100 1 - 100
1 - 100 1-100
3-50
1 - 100
90-23
100-52
87-i+3
79-28
92-22 0-86
100-1+3 91+-30
O.ll+X 0n.118ft"_*"*n0c1r
rJ 0.3 0.1+2X
0 .1 5 ^ .0 2
OD OD 11 VA VA H
1 v0n
i
- v - a~= . / VARIOUS FRACTIONS FROM THE RZFININ:- OF 'i t r c l i y m
ij
J
1 API sjaMPLE I \njf4BER
12 12 12-2
DESCRIPTION CRAV-
OF
ITY
EXPERIMENT
;api
Cracked residuum 18.1
Colorless fraction from chromatography
FRACTION DISTILLING <75o f . M)
5 700+ bottoms frcr+24.3 49
cracked residuum
5ENZ0PYRENE
[%)
O.42
0.09
SCHEDULE OF
APPLICATI0NS
|no./week - mg. )
1 - 100 3 - 100
3 - lOCf
3 - 100
INCIDENCE OF
TUMORS iC-weeks )
88-34
100-14
0-93
95-19
RELATIVE CARCINO-
GENIC POTENCY,
Fvip a '0.4
A/0 .4
-
0.24i.03
25.1 ZOfc API-25, 50# 21.1
(White oil + Vfest Texas residuum
3 - 100
92-4O
r\ ' r- f O.UV-
,0021
2b
Tracked residuum 7.3 0I .3
0.63 1 - 100 100-20
O.oX
42 Cracked residuum 14.2 28.6
0.36 1 - 100 94-34
43 Cracked residuum 24.; 24.5 0.27 1 - 100 100-37 0#l8-.02
43-1 Dewaxed API-43 12. C 29.5
1--1 1
1+3-U (1+4) Cracked residuum 15.2 1+3 Cracked residuum 6.C
08 Cracked residuum 9.8
73 Cracked residuum 17.8 73
31.1
47.1 43.3
21
0.47
1 - 100 2 - 201 2 - 201
0.15 1 - 100 0.32 1 - 100 0.52 1 - 100 0.35..: 1 -,.100
1 - 100
95-25 94-17
100-19
94-40
100-36
100-17 83-22
100-31
0.37*.04 0.36i;gI -32i;8|
0.22X
0.19X
0.59!;^
0 .41X
o .27 *.85
35 Cracked residuum 8.1 42.6 0.42 1 - 100 100-25 .u4;g|
23 Sidestream 23 46 Sidestream
26.7 78.5
23.8 87.9
0.027 0.033
3 - 100 2 - 100
3 - 100
100-19
94-28
100-24
^0.24 o-22-!o^ AVO.15
88 Sidestream
22.5 69.3 0.029 2 - 100 94-26 o.25;g|
89 jSide stream
2 7 .c 100
0.001 3 - 100 89-21 0.26! ; ^
39-3 }+-rineed ^ornati cs of API-89, jLl.0% solution in benzene
3-20
0-1
-
API-i+3~l involved repeated application until death. API-43-1A in
volved repeated application only until appearance of papilloma In each mouse. No significant difference in the average time to the appearance of gross carcinoma was noted.
Painting discontinued after I4.I weeks._____________
API 06488
IC a i ,
TA.
texcy cf various fractions from th:
FINING CF PETROLEUM
API
sample
^JMBER
DESCRIPTION CF
EXPERIMENT
r"~
91 ic:
Sidestream Sidestream
1 102 ; 102
Sidestream
101+ 1i 101+ 1
j"oudry
Sidestream
FRACTION DISTIL-
JRAV- LING ITY <750F. "API) (*)
SCHEDULE
OF
APPLICA-
BENZ0- TIONS
PYRENE `no./week
(%)
- mg.)
RELATIVE
INCIDENCE CARCINC-
OF
GENIC
TUMORS POTENCY,
(-weeks) PMC
20 J+ 80.1 0.037 2 - 100 95-23 0.26!;"
21+o8 89.7 0,007 3 - 100 100-121 0.33X
23 o5 99
0.015 2 - 2 0 2 - 100
69-U-3 1 93-321
0,1 :X 0.16X
25.8
0,011 2 - 2 0
75-531 . 0.03X
2 - 100 89-2c1 0 0iO aU*
II Cracked residuum if.3 81+
0.21 3 - 100 9h-l9
0 .19X
31+ Cracked residuum 23.0 90
0.011+ 3 - 100 84-32 Ay 0,1
So
Cracked residuum 21o3
85
0.07 3 - 1 0 0 100-21 aj 0,2
51 Cracked residuum 25.7 83
0,06 3 - 100 83-19 a/ 0.2
63
Cracked residuum 25.6 i+8.5
0.05
3 - 100
89-26
,, ,> .0 2 0 1 2 - ,0 1
63
3 - 100 100-19 0.l9i.03
63
3 - 100 90-26
0.21X
3
2 - 100 100-33 ,15-l|
63
3 - 2 0 100-1+5 o . u i . 0 3
63
3 -5
88-37
31 Cracked residuum 22.7 1+0.8 81
91
lycloversion
22 Cracked residuum 25.6
i+9.5
0.20 1 - 100 100-36
1 - 100 91-I+I
1-20
97-52
0.091 3 - 100 100-17
o.20;g^ o .2 ix 0 . 11+x 1
i
!1
a/0,3X | l
1
! The pattern of response to the irritational effects of this oil was similar to that observed with dodecylbenzene.
API 06489
TABLE I (?a?e C) potency cf various fractions from the refininc- of petroleum
API gAMPLE tjUJER
description of
EXPERIMENT
FRACTION DISTIL
GRAV LING ITY <750F.
V I ) (*)
SCHEDULE
OF
APPLICA INCIDENCE
BENZO TIONS
OF
PYRENE 1no./week TUMORS
{%)
- mg.) [%-weeks)
RELATIVE CARCINO
GENIC POTENCY,
PMC
solvent extraction
lb Phenol extract 9.7 from Coastal
16 900-X
Duosol extract 7.1 3
V
from California
waxy residuum,
5Of? in sec.-amyl
benzene
Phenol extract 11.0 80 from San Joaquin naphthenic dis tillate
70 Nitro-benzene ex15.7 5 tract from Barbers
Hill 60/80
75 S0a extract from +.1+ 100 TCC gas oil
.003
^.006
3 - 100 3 - 100
3 - 100
67-73 i+3-70
87-62
/V 0.01
ny 0.01
s-J o.ix
S .002 3 - 100 89-17 ^ 0.3 0.007 3 - 100 93-1+1+ 0.06.01 .001 3 - 100 77-51 /\j 0.05
Straight; run distillatici r
5b Waxy Midcontin 29.9 ent distillate
5b
5b 1
79 San Joaquin naphj-16.6 thenic lube dls-j tillate, narrow cut
52.1+ r j 13
0.003
.
3 - 100 3 - 100
3-20
88-22 65-1+2 81+-51+
/v 0.16
0.09X
0 .06X
<.005 2 - 100 86-57
(
1
!
O.lOX '
120 Ditto, wider cutil9.5 r J $ 2 X ?.003 3 - 5 0 1 65-60 o.o7+- ; ^
105 iWest Texas par 28.9, 72.9 '0.0003 3 - 100
!affin distillate
i
1
,
i
88-33" 1 0.ill*03
111+ Gulf Coastal ;distillate
111+
I21+.61 rv 501
i1
! 4 .002! 3 - 2 0 51+-83 ; 0.Ol.01
1
3 - 100 ! 55-71
0.02X
1 A.S.T.M. distillation.
a The pattern of response to the irrltational effects of this oil was
m
similar to that observed with dodecylbenzene.
API 06490
" ---
API
sample
DUMBER
DESCRIPTION OF
EXPERIMENT
;s t r a c t i o n s ef.c m t :e r e f i n i n :
PETROLEUM
,
FRACTION DISTIL-
GRAY LING ITY <750F. a p i : ($)
SCHEDULE
OF
APPLICA INCIDENCE
BENZO TIONS
OF .
PYRENE (no,/week TUMORS
($)
- mg.) \% -weeks)
RELATIVE CARCINO
GENIC POTENCY,
PMC
ii5 Blend of Gulf 23.2 50 `
Coastal distil U 5 lates
117 Gulf Coastal distillate
30.s r j 90 1
.002
3 - 20 3-50
0.000 3 - 50
77-80
63-66
75-04
0.02X -
pr a c t i c >nal distillation ( S r i t i s h Medical Re sear *ch Council)
110-1 Kuwait Naphtha 61.0 100
l l l - k Lagunillas dis 23.0
tillate 111-1+
111--i+a 75$ API-lll-U,
25$ benzene
22.7
lll-l+b Lagunillas dis tillate b. 650 690
1 Solution of .16$ BP in API-lll-i+b
in-5 75$ Lagunillas
residuum, 25$
benzene
I5.il
111-6 50$ API-110-1, 50$ API-lll-U
111-7 50$ API-111-1+ 50$ API-112-1
112-1 Oklahoma naphtha 65.9 100
112-3 Oklahoma
' 39.7
distillate
3-20 3-20 3 -5 3 -5
2 - 15
0-55 88-22 614.-75 51-82
- '
o.o4;^ 0U.oU?B+_a002i
0-1+7
3 - 50 100-16 u0.t3Ob_o017-
3'- 5 3-20
56-71+ 0.02.01
. 77-31
i
0.09 .01 ;
3-20
76-104
3-20
3-20
0-50
-
o-56a
3
a A.S.T.M. distillation. 8 Two papillomas appeared at 20 weeks but regressed.
The pattern of response to the irritations! effects of this oil was similar to that observed with dodecylbenzene.
API 06491
TA-LE I (page
. .. -ycGENIC p o t e n c y c p v a r i o u s f r a c t i o n s f r o m t h e r e f i n i n g c f p e t r o l e u m
API
sample
DUMBER
DESCRIPTION CP
EXPERIMENT
RAV ITY API
FRACTION DISTIL
LING <750F.
(*)
SCHEDULE
OF
RELATIVE
APPLICA [NCIDENCE CARCINO
BENZO TIONS
OF
GENIC
PYRENE [no./week TUMORS POTENCY, (*) - "g.) [% - weekj* PMC
y.nbrieating oil
99 Naphthenic dis- 20.0 ^v/38
tillate contain ing antioxidant
100 Solvent extract-29.5 rJ 0 ed, no additives
100-1 0.2^ Antioxidant1 in API-100
<.001 3 - 100 94-47 0.061.01
<.001 3 - 100 0-80
-
3 - 100 O-78
-
100-2 0.5* Antioxidant, 2,6-ditert.-butyl4-methylphenol in API-100
3 - 100 0-88 ;
fax pressing
32 Dewaxed paraffin distillate frac tion from Lima
crude
0.000 (3-6)-100 50-32
-
100-40
56 Feed to^presses 29.9 52.4 0.003 6 - 100 50-15
-
87-22
57 Dewaxed oil from API-56
28.7 80
.002 .6 - 100 50-17
100-25
Filtration dewaxing of JLPI-8
3-3 Filtrate oil, 11.3 65
85* of original
(.94* S)
3 - 100
90-17
n+.06 *30_.o 4
!Desulfurization of 8-3 by catalytic hydrogen ation
Hydrogenated heavy gas oil M 5 * S)
J Same type additive Three applications thereafter.
18.1 74
O .23 3 - 100 100-13
as that contained in API-99. per week for 14 weeks, six applications
1 n -/+.07
*36_.oi+
i
per week
API 06492
M 3 LE I (page ~~) 'pjtCTBOG10 PCTENCY 0P VARIOUS FRACTIONS FROM THE REFINING OF PETROLEUM
A?1 js^lpBSER
DESCRIPTION OF
EXPERIMENT
GRAV ITY i"API
FRACTION DISTIL LING <750F.
(JO
BENZO
PYRENE
(JO
SCHEDULE
OF
APPLICA-tNCIDENCE
TIONS
OF
no./week TUMORS
- mg.) 56-weeks)
RELATIVE CARCINO
GENIC POTENCY,
MC
Hydrolyzed acid 14.2
sludge
effect of viscosity on ^ - induction_______
Gulf Coastal distillate. 35 Sbo/xOO
21*.6
N 50
95Ji A P I-Ill*, $i l25.il alkylpolystyrene 17b U/Iuu -
jvusl oil Blending
113 Industrial fuel 6.3 1*3 oil
118 Catalytically
cracked residuum
component of
API-119
35.2
10* a p i -118, 90^ 3,3
light catalytic
cycle oil b. 1+50-600
S.002 3 - 100 25-79
'.002
3-20 3 - 100
3-20
3 - 100
67-83
8O-7 I
86-71* 75-71*
0.Oli.01 ' 0.02X i
0.03.01 : -l*-*.02 i
0.10
1.1
3 - 20
3 - 20a
3 - 20S
2 - 203
1 - 20*
3 100
a 3-5
3 20 s
3-
20
2/month100
77-27
0.11X ,
88-28 IOO-25
*li+ - ! o i .
91- 1*0 0,ll*i.02 ^
95-1*5
n i 7 + *01 '17-.02
100-25 I o-is*:8!
92- 31* ! 0 .1 S i ; 8 f
100-27 0.13X '
100-26 1 -11*-'.02 1
100-50 0.32-.0? ;
2/month100
2 - 100
81-85
96-30
. u * - 01* ! *12-.03 1 n i a + *02 ' *16-.01 .
_L
Approximate age of mice at start of experiment, 27 weeks,
* Approximate age of mice at start of experiment, 23 weeks,
* Approximate age of mice at start of experiment, 20 weeks, * Approximate age of mice at start of experiment, 11* weeks.
TABLE I
M - potency op various fractions from the REFINING OF PETROLEUM
API ,,
sample
VIJMBER *
FRACTION
pr&ctic nal distillation (30
Alunni
--
Fraction from API-8
3-6 0-9.3^ X
c^7 9.3-19.^ 1
plate
ESTIMATED SCHEDULE CORRECTED OF BOILING APPLICA-
RANGE p TIONS (in F.at )no./week
760nun. ) - mg.)
INCIDENCE OF
TUMORS (Ji-weeks]
1+35-560
560-630
2 - 100
2 - 100
O-06
0-71+
RELATIVE CARCINO
GENIC POTENCY,
PMC
-
5-8 19.U-30.3#1
3-9 .30*3-39.8^ X
3-10 39.8-4.9 ,6#1
3-11 1+9.6-59.2X .
8-12 59.2-69.I#1
630-695
695-710 710-765
765-800 800-830
2 - 100 2 - 100 2 - 100 2 - 100 2 - 100
0-71+ 56-o2
91+-1+1+
90-33
93-28
-
^ 0.07
0,10-.02 0 *li+-.02
0 .21 .03
Diels-Alder Reaction
fl-12a Non-adduct from reaction (95.W of API-9-12)1
2 - 100 100-26 0.23-.01+
Hractional distillation (30 plate
column) `Fraction from API-8
3-13 69.1-79. SfBl
6-11+ 78.5-80.Qf*
3-15 Residue; 80.8-100ji5
8-18 !Proportionate reblend of distillation fractions,
8-6 through 8-15
830-650 850-875 >875
2 - 100 2 - 100 2 - 100 1 - 100
79-25
92-35 87-39
0 .1 7 - .02
X
8-26a *26b
1Aromatics from API-8 j26.5-3O.85i 1 j3O.8-3 2 .O5i a
61+1-61+6 3 - 10
0-76
-
61+6-651 3 - 1 0
0-76
-
8 - 2 6 c |32.0-3J+.li 1
651-656 3 - 1 0
0-76
-
8-26d 31+.1-36.0J 1
656-662 3 - 1 0
0-76
-
j
, $Qfz solution in benzene.
, 33-3^ solution in benzene. Analysis indicated a content of .85# BP. $0% solution in benzene. Analysis indicated a content of 2.0^ BP.
API 06494
1
. -'ICGSIC POTENCY OP VARIOUS FRACTIONS FROM THE REFINING OF PETROLEUM *`________________________ _______ _______ _______________
sampi-b hjmber
DESCRIPTION
OF EXPERIMENT
ESTIMATED SCHEDULE
CORRECTED OF
BOILING APPLICA
RANGE
TIONS
;in F.at 'no./week
76O mm.) - mg.)
INCIDENCE OF
TUMORS ($-weeks)
RELATIVE CARCINO
GENIC POTENCY,
PMC
8-26 8-2M 3-26g 0-26h 8-261
3-26 j
0-26k
36.0-33.0$ X 3 8 .0-U0 .051 U0.0-U3.95i1 U39-U6.0$ 1 U 6 .O-5 0 .35i1
50.3-52. Sfc1
52.5-5U8$a
0-261 5U.8-57.3^1
0-26m
8-26n
57.3-6o .U^S 60.U-62.U5i1
662-668 3 - 1 0
O-76
-
668-67U 3 - 1 0
7-U2
-
_ 67U-686 3 - 1 0
20-72
-
686-693 3 - 10 12-25
-
693-709 3 - 1 0 36-61
-
709-717 717-727 727-736
3 - 10 3 - UO 3 - 10
25-U1
83-19 55-38
0.21X
-
736-7U7 7U7-759
3 - UO* 3-10
93-35 100-39
O-^-ioy -17-:o 7
Contribution of accelerators to above fractions
8-26-2 0.17$ BP in 80$ saturates through alkynaphthalenes fraction of 8-26g, h, and i, and 20$ benzene
0-26-3 0.17$ BP in 80$ 3-ringed aromatic
fraction of 8-26g, h, and i , and
20$ benzene
'
3 - 50 3 - 50
100-19
100-26
-i9i:S2
Air 0x3.dation (cobalt naphthenate catalyst)
8 FCC cracked residuum (prior to oxidation
83
83-1
Product of 2 hour oxidation of API-8 Product of U hour oxidation of API-8
2 - 100
2 - 100 2 - 100
9U-14
100-17
9U-17
.95-1^3
O.39X
o .U 5 x
8-22 69$ aromatics of API-8, 31$ sec.-
amylbenzene
83-2 69$ aromatics of API-83, 31$ sec.-
amylbenzene
1 50$ solution in benzene. * 50$ solution In dodecylbenzene. * Painting discontinued after 10 weeks;
1 - 100* 1 - 100*
63-39 79-U5
20 weeks.
0 .20X
u* ^ -.0 7
TABLE I (page 15) _NCGENIC POTENCY OF VARIOUS FRACTIONS FROM THE REFINING OF PETROLEUM
API * 3A|iPLE kuSber
DESCRIPTION OF FRACTION
wftterials regenerated from Diels-Alder fttions (Maleic anhydride extraction)
SCHEDULE
OF
APPLICA-] INCIDENCE
TIONS
OF
[no./week TUMORS
- mg.) ($-weeks]
RELATIVE CARCINO
GENIC POTENCY,
?MC
Material from 1st adduct formed
(2.7$ of API-8), 1$ In benzene
Material from 2nd adduct formed
(1.8$ of API-8), 1$ In benzene
Material from total Class B 1 adduct
(1.6$ of API-8 ), 1.5$ in benzene
Material from total Class A 1 adduct
(3*5$ of API-8), 2.2$ in benzene
Chromatographic fractionation of extract similar to 8-23h________
Crystalline material from 1st frac
tion (.15$ of API-8), .34$ in benzene
Crystalline material from 2nd frac tion (.17$ of API-8), .34$ in benzene
Material in mother liquor from 8-23a
and 8-23c (1.5$ of API-8), 1.5$ in
benzene .
Third fraction (.4$ of API-8), .8$ in benzene
Fourth fraction (.33$ of API-8),
.57$ in benzene -
Fifth fraction (.37$ of API-8),
.57$ in.benzene.
26n-l Total material from 8-26n, 2$ in
50$ benzene, 50$ dodecylbenzene
3-50
0-8
[lClass A adduct was that normally soluble in 5$ aqueous NaOH; Class B
adduct was not soluble in either 5$ aqueous NaOH or benzene after
hydrolysis.
fainting discontinued after 30 weeks;
37 weeks; * 32 weeks.
API 06496
TABLE I (page l)
.
jOGSNi: POTENCY OF VARIOUS FRACTIONS FROM THE REFINING- OF PETROLEUM
API
sample
fljMBER
DESCRIPTION OF FRACTION
SCHEDULE OF
APPLICA TIONS
no./week - mg.)
RELATIVE
INCIDENCE 'CARCINO
OF
GENIC
TUMORS POTENCY,
(-weeks) PMC
89-1
Anthracenic chromatographic fraction
(1.6^ of API-89) of material from
total adduct, 2% in benzene
89-2
Remainder of chromatographic frac
tions (mixed anthracenes, benzanth
racenes, etc., 0.2% of API-89),
.5$ in benzene
j
3 - 15
3-10
0-71+1 <0.02 100-68 0.03t. 01
120-1 Material from naphthenic distillate, 3 - 2 0
0-1+
-
API-120, corresponding to API-89-2,
2;% in benzene
jolvent extraction with cone. HBSOft 8-19 $0% extract* from API-8-10 and 8-11,
50% benzene
s 2 - 100
22-32
8-20 $0% raffinate* from API-8-10 and 8-11, $0% benzene
2 - 100* 83-25
23-1 Q0% extract from API-23, 20% benzem . 2 - 100* 90-26
23-2 Q0% raffinate* from API-23, 20%
benzene
2 - 100* 100-1+1+
<0.09 A-'O.I
0.2l4:o 0.13.02
Fractio nation of API-12
12-7
3Off non-adduct of Diels-Alder
reaction on raffinate from sulfuric extraction of aromatic fraction b. 'v 680-780*, 7 0 % benzene
12-8 Ditto from fraction b . ^ 780-950 70% benzene
2 - 20* 2-15
77-65 90-58
0l+-.02 0.071
* Accelerators removed prior to extraction and reblended proportionately in extract and raffinate.
* Painting discontinued after 21+ weeks; 4 1+3 weeks. ii
API 06497
TABLE I (page 17) ..-^ISOGENIC POTENCY OF VARIOUS FRACTIONS FROM THE REFINING OF PETROLEUM
A?I ,, SAMPLE ! jfljjtBER
DESCRIPTION OF FRACTION
SCHEDULE OF
APPLICA TIONS
no./week - mg.)
RELATIVE
INCIDENC]: CARCINO
OF
GENIC
TUMORS POTENCY,
(-weeks) PMC
osraphy l .a
8-13 First aromatic fraction, 2% of API-8-13
3 - 20* 9-36 c o . 05
8-13b Second aromatic fraction, 2.1+J of API-8-13
_ ,* 8-13C Third aromatic fraction, 0 . 7 % of
API-8-13
3 - 20* 1U-58 3 - 2 0 100-1+2
C O . 03
0.07X
8-13d 8-13 8-13f
Fourth aromatic fraction, $ . 6 ) ( * of API-8-13
J| Fifth aromatic fraction, 56$6 of API-8-13
g Sixth aromatic fraction, 2% of API-8-13
8-13g Seventh aromatic fraction, 16.9J6* of
API-8-13
.
3-20 3-20 3 - 20* 3-20
IOO-29 86-1+0
83-1+5
100-27
0 .10.02
0.07X
0.11X
B-l3h Eighth aromatic fraction, 2.1+j6*of
API-8-I3
g 8-131 Ninth aromatic fraction, 6.9/6 of
API-8-13
3-20 3 - 20
100-37 73-36
0.09X
0 0 .1 .+ 00
U> M
71-2 Proportionate reblend of all frac tions from API-71
71-1 Reblend of all fractions except 71-1 dark resin proceeding aromatics
1-20
93-59
1-20
03-61+
1 - 100 IOO-15
0*22i3+-.*0062 n*i16A"-*".G01l+
O.9OX
i
Proceeding colorless non-aromatic fraction, l+8j6 of API-8-13, proved to be a non-accelerating solvent when diluted 5Oj6 with benzene. See API-266 on page 3 of Table VII. Tested at this percentage in benzene. Painting discontinued after 35 weeks; * 1+1 weeks,
API 06498
TABLE II CONTROL EXPERIMENTS WITH VARIOUS SOLVENTS
API EXPERI MENT
number
80 95
221 221a
22k 22 8
22 8
214-1 29k 29k*
639
SOLVENT
SCHEDULE OP
APPLICA TIONS
Cno./week
- mg.)
STRAIN OP
MICE
MAXIMUM INCIDENCE
OP TUMORS
()6 - weeks)
INCIDENCE OP
OR OSS CARCINOMA
- weeks)
White oil (95SSU)
3 - loo1 C3H
White oil (95SSU)
3 - 100* CPW
Dodecylbenzene
3 - 100 C3H
mm0
8-81;% fraction b.
1
C3H
5U8-572 from dis
tillation of API-22]
Sec.-amylbenzene Benzene Benzene Distilled water
3 - 100 CFW 3 - 100 C3H 3 - 100 CFW 3 - 1004 C3H
m0
Dodecane
1
C3H
Dodecane for 12
3-50
C3H
weeks followed by
70^ dodecane, 30% 3I4QSSU white oil
75/6 dodecylbenzene
1
mO
C3H
2$% benzene
0-80 0-80
33-37
0-52
18-59*
0-100
0-62 7-78
0-80 0-82
0-80 0-80 0-52 0-52
0-82 0-100
0-62 7-78
5
0-80
0-82
U-15
0-I9
a Painting discontinued after 60 weeks; 31 weeks; 61 weeks. Histopathologieal examination confirmed only one of the four gross
k lesions as a papilloma; the others were termed hyperkeratosis,
5 Histopathologieal examination showed one fibrosarcoma in 70 weeks.
API 06499
TABLE III
1
^ H lffiN TS INVOLVING THE APPLICATION OP SOLUTIONS OF METHYLCHOLANTHRENE
IN VARIOUS SOLVENTS UPON THE SKIN OP C3E NICE --
API gXPERl" ItENT
gtJHBER
SOLVENT
SCHEDULE OP
CONCEN APPLICA TRATION TIONS ( % by (no./week
weight) - mg.)
MAXIMUM
INCIDENCE OF
TUMORS (-weeks)
RELATIVE CARCINO
GENIC POTENCY,
PMC
218 Crude residuum,
API-5
625 API-80, 95 SSU white oil
0.31
0.10
621+ API-80
0.20
293 31+0 SSU white oil 0.50
607 5056 benzene, $0% 0.10
31+0 SSU white oil
281 Cottonseed oil
0,0i+
291 Cottonseed oil
0.50
21+6 Naphtha, API-1124 0.21
21+6
21+8 Naphtha,API-110-1 0.21
223 Sec.-amylben^ene, 0.09
API-221+
222 API-221+
0.18
231+ API-221+
0.35
235 API-221+
0.70
608 Decalin
0.08
609 Dinonylnaphthalene 0.08
3 - 100 100-30 0.09i.01
3 - 1 0 100-32 0 .lot. 01
2-10 3-20
3-10
95-32
100-20
93-38
3 - 100 3-20 3-20 3-20 3-20 3 - 100
89-69
95-23
100-22 100-21 100-22
81-1+6
0 ,1 5-.02
0.16X
U0 ,U0Q'-+.*0 ^2
0.03t .01 n*1177^-".*0 6 0.19.02 0 .19 1.0 2 n )l+.02
0 ,lb - .o i
0 .01+1 . 01
3 -~100 2 - 100 2 - 100
3 - 50 3 - 50
100-1+1+
100-27
100-19
92-1+51 88-56
o . o9 !: 2
0 .27! ; ^ 0 .28 1.03
o.ol+x
0 .0 5 1 .0 1
1
The pattern of response to the irritational effects of this solution was similar to that observed with dodecylbenzene.
API 06500
TABLE IV
IMENTS INVOLVING THE APPLICATION OF SOLUTIONS OF 3ENZ0PYRENE IN NON-ACCELERATING SOLVENTS UPON THE SKIN OF C3H MICE
A fl ^NT HtjNBER
602 6014 299
296
282 21*14
2I4I4
252 252 252
252
613 613 28$
286
SOLVENT n-octane Isooctane
3I4.O SSU white
oil 31+0 SSU white oil Benzene Benzene
Benzene
85/S b-methylnaphthalene,
15^ benzene
Cottonseed oil Cottonseed oil
SCHEDULE
OF
MAXIMUM
CONCEN APPLICA INCIDENCE
TRATION TIONS
OF
( f b y (no./week TUMORS
-weight) - mg.) | jf-weeks)
0.21 0.15
0.08
3 - 100 3 - 100
3-5
100-36 100-31
96-14-3
RELATIVE CARCINO
GENIC POTENCY,
PMC
o .o e t;!
0.10.01
0.0l*.01
0.20
0.08 0.17
0.32 0.32 0.32
0.32
0.20
0.50 1.0
3 - 50 100-36
3-20
3 - 100 3-20 3 - 100 3-20
2-20 1-20
2 - 15
2-50
3-20 3-20
100-50
100-33 91+-37
100-26 100-27
9l4-51l 96-1*3 100-1+0
-100-37 100-32
95-25
0.081*02
0.07-.01
0 .09.01
0.07X
0,13-,02 0.10X 0.10X
0.15X
0.08.01 o .io x
0.09X
.0.12.01
T
] f1
TABLE V EXPERIMENTS TO DETERMINE THE POTENCY OF MIXTURES OF POLYCYCLIC
HBYDROCARBONS IN TECHNICAL NHITE OIL FOR THE SKIN OF MICE
API EXPERI MENT MEMBER
"
HYDROCARBON
b2k Me thylcholanthrene control
623 Me thylcholanthrene Benzopyrene
625 Methylcholanthrene control
626 Methylcholanthrene Benz anthracene
CONCEN TRATION
by weight)
SCHEDULE OF
APPLICA TIONS
(no./week - mg)
0.20
2 - 10
0.10 0.20
0.10
2-10 3-10
0.10 0.20
3-10
MAXIMUM INCIDENCE
OF TUMORS
- weeks)
RELATIVE CARCINO
GENIC POTENCY,
PMC
95-32
0,15-.02
100-26
0.17*.02
100-32
0.10*.01
IOO-3I4.
0.08X
TABLE VI
-gjjiENTS INVOLVING TEE APPLICATION OF SOLUTIONS OF METHYLCHOLANTHRENE (MC)
IN DODECYLBENZENE* UPON THE SKIN OF MICE
.
API gjCPSRl*ENT
DUMBER
CONCEN TRATION ( i fey
weight)
STRAIN OF
MICE
SCHEDULE OF
APPLICA TIONS
(no./week
- mg)
MAXIMUM INCIDENCE
OF TUMORS (jf - weeks)
RELATIVE CARCINO
GENIC POTENCY,
___PMC
fmc
OF
MC
221
0
C3H
221a
0
C3H
226
0.006
C3H
226
0.006
CFW
225
0.012
C3H
225
0.012
CFW
213
0.05
CFW
211
0.12
C3H
211
0.12
CFW
208
0.15
C3H
21*9
0.17
C3H
21*9
0.17
C3H
212
0.35
C3H
3 - 100
3 - 508
3 - 100 3 - 100 3 - 100 3 - 100 3 - 100 3 - 100 3 - 100 3 - 100 3 - 100 3-20 3 - 100
33-37
0-52 50-1*0
1*1-51*
81-1*3 100-51* 100-18 100-22 100-17 100-15 100-12
89-11*
"100-18
s
-
0.05X A/0.03 SiS 0.30
U.36-.12 A^0.30
0.33 .03
0 )i7+08
u,43-.07
0 7c+06
*35-.oi*
0 7+*06
u *35_.o9
m 1*17 /v250 a/600
292
^250 220
252
206 100
--
___________ 1
Product obtained by alkylation of benzene with the propylene tetramer
(aluminum chloride catalyst).
Painting discontinued after 31 weeks.
"
` ivldence of invasive mallgnaQpT,
API 06503
TABLE VII
n
ACCELERATING a c t i v i t y o p v a r i o u s s o l v e n t s o n r a t e o p i n d u c t i o n OF TUMORS BY DISSOLVED BENZOPYRENE (BP) IN C3H MICE
API gjCPSBliNT
SOLVENT
CONCEN TRATION
(% by weight)
SCHEDUIE OF
APPLICA TIONS
(no./week
- ag.)
MAXIMUM INCIDENCE
OF TUMORS % - weeks)
RELATIVE CARCINO
GENIC POTENCY,
__ Im c ____
n-octane n-decane dodecane
0.08+ ..0023
o i10 - .0012
cetane (chromato graphed- on siile gel)
n0 .1114+- ,0032
70
n-hexadecene-1
rVHLOPARAFFINS Decalin
Cyc1ohexylde cane
7 -cyclohexyltri-
decane, PSC-504
3-40
100-25 0.19'+..0043 100
0.04X * 22-!o 4
n 1 02
, -,
0 . 1 5 - ,oi
^5
0.09*.01 o.09.oi 0.09.02
0.1U
0.Ili.01
Carcinogen in this case was methylcholanthrene. * The pattern of response to the irritational effects of this solution
API 06504
TABLE VII (page 2) ACCELERATING ACTIVITY OP VARIOUS SOLVENTS ON RATE OF INDUCTION
OF TUMORS BY DISSOLVED BENZOPYRENE (BP) IN C3H MICE
API gXPERl-
IftjMBgL
SOLVENT
A ctions from 2
rjgmTT.rJtTIONS OF API-80
Percent Boiling API-80 Range
O-3 .5
SCHEDULE OF
CONCEN APPLICA TRATION TIONS ( % by (no./week weight) - mg.)
0.17 3 - 5 0
MAXIMUM INCIDENCE
OF TUMORS [% -weeks)
100-22
0.17 3 - 5 0
100-22
0.17 3 - 5 0
100-22
0.17 3 - 50 100-32
8.7-16.7 625-614.5' 0 .1 7 3 - 100 91+-21+
276-Q U . 7 -19.5 61+5-655' 0.17 3 - 100 100-28
^5.7-36.3 61+0-685' 0.17 3 - 100 100-30
L9.5-30.3 655-675' 0.17 3 - 100 100- 21+
276-10 )0.3-1+0.5 675-700' 0.17 3 - 100 100- 21+
276-6
276-6
36-IOO > 700 0 .17
(residue purifiei by percolation
through silica ge )
3 - 100
3 - 50 j
100-29
92-29
RELATIVE CARCINO
GENIC POTENCY,
PMC
o .i6!;o J
0.15*.03 0.08.01
0 . 1i+.02
0.11X
0. 10*.01
0-l4i:o3
00 # 1H1 -+.*012
o.ioi.oi
0.09X
P *MC
OF BP
88 88 i|7 82 65 59
82
65 59 53
FRACTIONS FROM DISTIL LATION OF SATURATED COM PONENTS OF TCC RESIDUUM, API-71
Percent Range 0-2.9 4-30-500'
6.1-7.1+ 550-565' 7 .+-11.3 580-600' Ll.3-i5 .l4. 600-620'
0.18 0.18 0.18 0.18
3-30
3-20 3 - 1+0
3-50
88-17 83-I8 100-25 100-27
+ .06 22-.01+
122
0,i2iR3+-.*1^0 128
- ,-+.06
*17-.o5
9k
0 T2+*^2
67
TABLE VII (page 3)
a c c e l e r a t i n g ACTIVITY OP VARIOUS SOLVENTS ON RATE OP INDUCTION OF TUMORS BY DISSOLVED BENZOPYRENE (BP) IN C3H MICE
r------
API SXERIHSNT HUMBER
' SOLVENT
CONCENTRATION
by .weight)
SCHEDULE OP
APPLICATIONS (no/week
- g.)
MAXIMUM INCIDENCE
OP TUMORS
(j6-weeks)
RELATIVE CARCINO-
GENIC POTENCY,
PMC
0 PMC OP BP
1 9 AlPesIs-8-f2r1a+,cticoonlor 0.21+ 1 - 5 0 100-1+3 0.15*.02 63
from chromatog
raphy of API-8
2b6 50ji colorless
fraction from
0.15 3 - 100 100-31+ 0.07*.01
1+7
chromatography of
API-3-13, $0%
benzene
aleylbeiJZENES
605 Diisopropylbenze i 0.17 3 - 5 0
100-1+7 0.05t . 01
29
275 Triisopropylbenzene
275
606 t-octyltoluene
0.17 0.17 0.17
3-50 3-30 3-50
100-18 0 22+,(^
130
* 03
100-30 0.12*.02
71
100-21
0.17X
100
262 1-phenyldecane
629 Dode cylbenzene (DDB)
21+5 DDB
0.18 0.08
0.17
3-20
3-20
--
3 - 100
95-16
75-30
100-19
-33;3 183
o.ii+t!o \
180
. ->+.08
*30-.o 6 176
21+5
3-20
100-31 0.16*.05
91+
21+5
3 -5
100-23 0.19*.01+ 112
LAB DIS:'ILLATION OP COMMERC:CAL ALKYLATES
Distillation of
Alkylbenzene1
271+-8 Fraction b. 1+50 0.17 3 - 1+0 100-22 o.lSt-.ofc
88
500*
271+-13 Fraction b. 555560
0.17
3-50
100-12
o.UoYo l 236
L x Product of alkylation of benzene with polypropylene
TABLE VII (page k)
ACCELERATING ACTIVITY OF VARIOUS SOLVENTS ON RATE OF INDUCTION OF TUMORS BY DISSOLVED BENZOPYRENE (BP) IN C3H MICE
API gjCPSRl-
hsnt
JIUMBER
SOLVENT
267-1
Distillation of
PDDB1
Fraction b,60361+2
267-3 267-5
Fraction b.655-
683
Fraction b.661j.730
267-8 Fraction b.659-
76O0
SCHEDULE OF
CONCEN APPLICA TRATION TIONS ( i by ^no./week weight) - mg.)
MAXIMUM INCIDENCE
OF
TUMORS \$ - weeks)
0.17 0.17 0.17 0.17
3-20 3-20 3-20 3-20
100-31 100-33
IOO-38 IOO- 3 6
RELATIVE CARCINO
GENIC POTENCY,
PMC____
. . n+.02 0.1 0 - ,0 1
0 .0 7 .0 1
0.06*.01
0 .07**01
PMC OF
BP
59
1+1
35
1+1
alkylna:HTHALENES
613 85/6 b-methylnaphthalene, l5j?
benzene
0.20
265 Butyl-dimethylnaphthalene
0.16
272 Monoamylnaphthalenes,b.570
0.16
273 Dlamylnaphthalene s 0.16 b.b30-690o
09 Dlnonylnaphthalene 0,08*
2-50 3-20 3 - 1+0
3-50 3-50
IOO- 3 7
100-25 100-19
100-19 88-56
0.10X
oau!;gI
0 .1 7 .03 n0 .23A8+-.*018^ 0.05*.01
50
88 106
175 a
63
MIXTURE 3 OF ACCELERATORS
WITH V!HETE OILS
260 5* DDB, 95*
API-80
0.17 3 - 100 100-33 0.07*.01
1+1
259 2 0 $ DDB, 8 0 $ API-80
0.17 3 - 100 100-32 .o8t;2
1+7
33 5 0 $ DDB, $ 0 $ API-80
0.08 3 - 5 0
61+-37 rsj 0.06
75
637
l--
50# DDB, 50$ AFI-80
0.17
3-50
100-27 0.10*.01
59
Alkylbenzene, residual by-product of commercial alkylation of
, benzene with propylene tetramer. Carclnoeen In this case was methylcholanthrene,
TABLE VII (page $)
a c c e l e r a t i n g activity of various solvents on rate of induction OF TUMORS BY DISSOLVED BENZOPYRENE (BP) IN C3H MICE
r"'---
API gjrpERl'
uent
SOMBER
SOLVENT
CONCENTRATION
( * by weight]
SCHEDULE OF
APPLICATIONS
(no./week - mg.)
MAXIMUM INCIDENCE
OF TUMORS (*-weeks)
636
75* DDB,
25* API-80
0.08 3 - 5 0
100-27
638
75* DDB,
25* API-80
0.17
50* DDB,50* 31+0
SSU white oil
0.08
3 - 50 3-50
100-29 1+2-36
297 50* dodecane, 50* 0.20
3i+0 SSU white oil 297
297
611+ 75* dodecane, 25* 0.20
3i+0 SSU white oil 611+
611+
3 - 100 3-50
3-20
3 - 50
2-50
1-50
100-21+ 100-29 IOO-33
100-28
100-26 100-31+
RELATIVE CARCINO-
GENIC POTENCY,
Pm c
0.-+3- no
n -P+.02 0.12-01
/VO.05
0.13.01
u *13-.o 3 0 .08.01 0.12t. 01 0 .1 5 ^ .0 1
n pn"*"*02 *0 -.01
O *MC
OF BP
163
71
r j 63
65 65
i+0
60 75 100
MIXTURES OF DDB WITH aromatic HYDROCARBONS
628 50* DDB, 50* b- 0.08 3 - l+o . 93-32 0 .lit. 02 138
me thylnaphthalene
'
31+ 50* DDB,
50* benzene
0.08 3 - 5 0
95-23 o.n+i|oi 175
1+1+ 50* DDB,
0.09 3 - 5 0
68-13
-
-
50* benzene
6I+3 50* DDB,
50* benzene
0.17 3 - 50
30-13
>-- API 06508
TABLE VII (page 6)
ACCELERATING a c t i v i t y of v a r i o u s s o l v e n t s on r a t e of i n d u c t i o n OF TUMORS BY DISSOLVED BENZOPYRENE (BP) IN C3H MICE
API EXPERI MENT
number
S0LVENT
CONCEN TRATION ( % by weight)
SCHEDULE
OF
MAXIMUM
APPLICA INCIDENCE
TIONS
OF
(no./week TUMORS - mg.) \% -weeks)
i\ -O\ Vn-3 1\
IF
**603
M E S FROM VARI0US GENIC 0ILS
Fraction of TCC residuum, API-9,
b. 01+0-600
0.16
3-50
100-30
RELATIVE CARCINO
GENIC POTENCY,
PMC
bl5
Lagunillas dis
tillate. b.550-
650
616 Lagunillas dis tillate, b. 650
690
0.16
0.16
3 - 50 3 - 50
100-16
100-16
0.35! : $
distill/ITES FROM CRUDE ASSAYS
by BURE/ITT OF MINES'1
Corre 1Boiling Specific ation
Range Dispersion Index
617 1+80-660 li+1
26
618 1+80-660 186
U9
619 1+80-660 161+ . 5k
630 1+80-660 151+
31
631 1+80-660 190
53
d32 1+80-660 11+5
37
632a
50 PI-632, diluted $0%
with benzene
3 - 50 3-50
3 - 50 .
3-50 3-50 3 - 50 3-50
100-21+
100-19 100-19
92-19
100-18
95-19 5-13
0 .1i+.01 0.20.02
*20-.*02 0 .18.02
0.23*. 01+
0.20-.8!
-
61+0 1+80-660 11+1
21+
3-50
26-13
-
Diluted 50j6 with benzene
61+1 1+80-570 130
21
3-50
10-10
-
Diluted $0% with benzene
61+2 570-660 138
23
3-50
Diluted 50 with benzene
11-10
PMC OF BP
88
169
219
78
118 118 106
135 116
-
Experiments run at a concentration of 0.17^ BP.
API 06509
TABLE VIII
effect of early exposure to accelerating solvents on results OF SUBSEQUENT EXPOSURE TO CARCINOGENS
----- -
API SXPER10KT SM3ER
DESCRIPTION
MATERIALS APPLIED TO MICE IDURING
FIRST SIX WEEKS OF EXPERIMENT
SEVENTH WEEK TO END OF EXPERIMENT
STRAIN OF
MICE
SCHEDULE
OF APPLI
CATION
OF iINCIDENCE
CARCINOGBf
OF
(no./week TUMORS a
- mg.) (Jf-weeks)
AVERAGE LATENT PERIOD
FOR TUMOR INDUCTION
(5J F.L. in weeks)
EdJki
221 DDB*
DDB
9
TCC resid API-9
uum,API-9
221-9 221-9 253-9
DDB
PDB3
API-9 API-9
57 API-57*
API-57
221-57 DDB
API-57
208 API-208^ 221-208 DDB
API-208 API-208
82 TCC resid API-82 uum, API-82
600 Dodecane
API-82
601 3^0 SSU
API-82
white oil
C3H
3 - 100 33-37
C3H
3 - 100 100-1+7 36.23.9
C3H
3 - 100 100-21 11+.5-1.8
C3H
3 - 100 100-22 12.82.i+
C3H
3 - 100 91+-26
13
CFW
6 - 100 50-I6
-
IOO-25
CFW
6 - 100 50-13
-
100-16
C3H
3 - 100 100-15 10.1+4.6
C3H
3 - 100 100-11+ 8.11 .1
C3H
1 -1 0
100-50
3!I
C3H
1 - J.0 100-1+2 30.741+.0
C3H
1 -1 0
100-1+1 30.2*5.1+
76 Reformer API-76 tar,API-76
620
Dodecane
API-76
621 95 SSU
API-76
white oil
C3H
3 - 50
83-52 ^31+
C3H
3-50
C3H
3-50
67-1+8
55-1+5
,n/33 1+3
622 31+0 SSU
API-76
white oil
C3H
3-50
60-1+7
35
Schedule of application of accelerator was the same as that of the
carcinogen except In experiments 600 and 601 In which case $ 0 mg.
was applied three times each week.
Time measured from date of initial painting with carcinogenic material.
Dodecylbenzenes obtained by DDB obtained with propylene
alkylation of benzene with tetramer; 2-phenyldodecane
12-carbon olefins (PDB) obtained
;
with 1-dodecene.
Filtrate oil from pressing of Midcontinent paraffinic distillate.
Solution of 0,l5ji methylcholanthrene_Jja_dodecjlbaaaan______
AP! 06510
TABLE IX
EXPERIMENTS to determine the carcinogenic promoting activity
OP VARIOUS MATERIALS FOR THE SKIN OP C3H MICE
CARCINOINCIDENCE TIME
GENIC OP TUMORS OP 2nd PROMOTER
INITIA PROM APPLICA USED
API
TOR, SINGLE TION PROM 3rd
jgCPERl" SINGLE APPLICA(if appli-' Hk RK
jfiSNT APPLICA TION cable) TO
HUMBER __ TION (Jf-weeks)(wks.-mg.l END
SCHEDULE OF APPLI
CATION OP
PROMOTER |no./week
- mg.)
MAXIMUM
INCIDENCE OP
TUMORS (-weeka)
AVERAGE LATENT PERIOD FOR TUMOR INDUCTION
{5jC P.L. in weeks)
229 100 mg. 13-13 none
none
-
API-229'
1 3 -61+
-
23O 100 mg.
API-229
none
Dodecylbenzene, DDB
3 - 100
92-31+ 1 1 .8^2.8
231 100 mg. API-8,
O-63 none
FCC res
iduum
none
O-63
232 100 mg. API-8
239 100 mg. API-8
none DDB
3 - 100 50-26
21+X
none Distillei 3 - 1 0 0
0-76
-
water
21+0 100 mg. API-8
none API-80, 3 - 100
0-76
--
95 SSU
white oi]
29O 100 mg.
k -2 b 28-100 none
. -
API-290
95-59 . rO 1+6
287 100 mg.
API-290
288 100 mg.
API-290
0-28
none
28-100
Alkylbenzwne, partly DDB
API-80
3 - 100 3 - 100
79-30 96-57
17^
1+8
289 100 mg.
API-290
0-28 28-100 31+0 SSU 3 - 100
white oil
89-72 /x/ 50
292 100 mg. API-290
292
292
none
Dodecane
3-50 2-50 1-50
91+-26 94-53 81-59
u!2 . aC i
1+1+.0+3 . 9
Solution of 0.5 g. dimethylbenzanthracene in 100 ml. aec.-amylbenzene. Solution of 0,5 g. dimethylbenzanthracene in 100 ml. 3l+0 SSU white oil.
API 06511
TABLE X EFFECT OF TERMINATION OF EXPOSURE OF C3H MICE TO CATALYTICALLY
CRACKED OILS AT A CRITICAL PHASE OF THE EXPERIMENT
API gXPSR1" jffiNT UMBER...
W-l
DESCRIPTION OF
EXPERIMENT
Dewaxed oil from catalytic ally cracked re s iduum
SCHEDULE OF
APPLICATIONS
TOTAL (no./week NUMBER
- mg.) OF WEEKS
2-20 1
W -1A Ditto 43-IB Ditto
2-20 2-20
10-19*
9
1
71 TCC residuum 2-20
71A Ditto `
7IB Ditto
2-20 2-20
lil-25* 12
MAXIMUM
INCIDENCE OF
TUMORS {%-weeks)
AVERAGE LATENT PERIOD FOR TUMOR INDUCTION
(5* F.L. in weeks)
AVERAGE TIME FROM
PAPILLOMA TO GROSS CARCINOMA
(weeks)
914-- 17 12.7-1.14
114
100-19 1 3 .8-1.2
16
16-12*
-
-
100-27 18.5-1.3
15
100-25 18.3-1.5
16
53-18*
Painting continued in each mouse until gross evidence of malignancy in that mouse. Painting of each mouse discontinued at time of appearance of papilloma in the individual mouse. No additional tumors developed up to the 23rd week at which time appli cations were resumed. They were terminated in the 28th week after the appearance of a papilloma in an additional animal. All survivors had developed tumors by the 58th week.
* Procedure similar to API-I4.3 -IB. Painting resumed at 30 weeks, discon
tinued after 32 weeks. By the 61|.th week all but one of the survivors had developed tumors. Gross malignancy was evident in 58% of the mice.
API 06512
TABLE XI
EXPERIMENTS TO DETERMINE TEE POTENCY OF CERTAIN POLYCYCLIC HYDROCARBONS FOR THE SKIN OF C3H MICE
API CPSRI0ST mJMBER
HYDROCARBON
261
1;,5-dime thyl-
phenanthrene
SOLVENT Benzene
627
Benz Ca]anthracene Dodecane
CONCEN TRATION ( % by weight)
SCHEDULE
OF'
APPLICA TIONS
(no./week
- m g .)
MAXIMUM INCIDENCE
OF TUMORS (J? - weeks)
0.86
m
1
0-814.
CoVJ
0.50
ion
53-1*5
'
API 06513
TABLE XII
EXPERIMENTS ON THE RETARDATION OF TUMOR FORMATION BY WASHING CFW MICE
PERIOD OF
EXPOSURE
TO OIL HATERIAL
CPBRI- CARCINOGENIC BEFORE RE USED FOI ;AGENT
ggNT
OIL MOVAL BY INITIAL FOR
DUMBER APPLIED WASHING RINSE WASHING
"U3 113
Industrial fuel oil, API-113
control (no -washing)
none
none
AVERAGE
SCHEDULE
LATENT
OF MAXIMUM PERIOD
APPLICA INCIDENCE ?QR TUMOR
TIONS OF
[EDUCTION
(no/week TUMORS f(5* F.L.
- mg.) $-weeks) -in wks. 1
3 - 100 ' 94-36 A/ 16
3 - 1001 97-25 17.3*1.2
309 API-113
1 hour none 1letergenl 3 - 100 40-67
X
solutior
31O API-113
4 hours none 1letergenl 3 - 100 54-57 56x
solutior
311 API-113
4 hours 95 s s u .Letergenl 3 - 100 83-52 45x
white o .solutior
API-95
31* API-113
7 hours none 1Letergenl 3 - 1001 94-46 a /35
solution
12 FCC residuum ,control none
API-12
(no
-washing)
303 API-12
1 hour none
}0k API-12
9 hours none
8 FCC residuum , control none
API-8
(no
washing)
300 API-8
10 min. none
301 API-8
1 hour none
302 API-8
4 hours none
none 3 - 100 100-14 A/ 10.5
soap 3 - 100
solution
soap . 3 -.100
solution
'
100-40 100-21
a/ 27
- V 17
none 1-100 100-26 12X
soap 1 - 1 0 0
solution
soap 1 - 100
solution
soap 1 - 100
solutior
0-80
-
20-80
-
100-70 a/ 6 0
| !
1 j
Strain of mice used for this experiment was C3H.
API 06514
TABLE XII (page 2)
EXPERIMENTS ON THE RETARDATION OF TUMOR FORMATION BY WASHING CFW MICE
API iYPERI" jCJNT nM3ER
t
8
PERIOD OF
EXPOSURE
TO OIL
CARCINOGENIC BEFORE RE
OIL
MOVAL BY
APPLIED WASHING
API-8
control (no -washing)
MATERIAL USED
FOR INITIAL
RINSE
none
AGENT FOR
WASHING
none
SCHEDUIE
1AVERAGE LATENT
OF MAXIMUM PERIOD
APPLICA- INCIDENCE ?0R TUMOR
TIONS
OF
INDUCTION
(no /weok TUMORS (5* F.L.
- mg.)
weeks) -in weeks'
3 - 100 100-9 ^ 8X
305 API-0
20 min. none <Letergent 3 - 100
solution
93-51 /vuo
CO Or*~\
API-8 306 a p i -8
20 min. 1 hour
API-95 none
none
<.etergent solution
3 - 100 3-100
IOO-52
9U-UU
^32 r J 33
307 a p i -8
1 hour API-95 letergent 3 - 100 85-33
5
solution
312 Barrier cream applied API-8 applied Removal of 0il by washing
with detergent solution
313 ABParIr-8ierappclrieeadm applied API-8 applied
Removal of oil by washing with detergent solut ion
9:00 AM 11:00 AM
12:00 AM
3 - 100
71-U5 a A O X
9:00 AM 11:00 AM
2:00 PM
1+t30 PM
3 - 100
100-31
v 25
' API 06515
TABLE XII (page 3) EXPERIMENTS ON THE RETARDATION OP TUMOR FORMATION
BY WASHING C3H' MICE
ERIOD OP
EXPOSURE
API
TO OIL MATERIAL
gXPERI- CARCINOGENIC 3EFORE REUSED FOR AGENT
jENT
OIL
MOVAL BY INITIAL FOR
DUMBER APPLIED
WASHING RINSE WASHING
AVERAGE
SCHEDULI
LATENT
OF MAXIMUM PERIOD
APPLICAINCIDENCI FOR TUMOR
TIONS
OF INDUCTION
]no./weel TUMORS (S% F.L.
- mg.) (jf-weeks) -in weeks
8 API-8 8 316 none 317 none 320 API-8
318 API-8
319 API-8
control none (no .washing]
none none
none 3 - 15 3 - 100
ietergen1;3 solutioi L
100-18 89-9 O-72
12.1+11.2 5.2.6
none
a p i -95 ietergen- 3 solution
O-72
95 min. 95 s s u ietergen-;3 - 100 white oi] solutioi L
API-80
95-16 10.011.2
75 min. 3*4-0 SSU ietergen-3 - 100
white oi] solutioi 1 85 min. refined ietergen-;3 - 100
kerosene solutioi 1
100-21 91+-21
16.6*1.1+ 16X
56 ?eed to Wax control none
none 3 - 2 0
84-51+
32X
?ressing,
(no
56 a p i -56
-washing]
3 - 100 65-1+2
21+X
311+ a p i -56
7 hours none ietergen-3 - 100 67-7*+
55x
solution
-