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Organic Coatings for the Interior of Gasoline Drums

(2)

NATIONAL

RESEAHCH C O U N C I L CAilADA

O R G A N I C COAllI;L'GS F O R TiiG I N T E l i I O H

O F G A S O L I N C DRUMS

by D. Dennis, B.S, S t a f f o r d , and

J,

Harris

R e p o r t No,

51

of t h e

D i v i s i o n o f B u i l d i n g R e s e a r c h

OTTAWA

(3)

The s a t i s f a c t o r y s t o r a g e of a v i a t i o n and motor f u e l s i s a v i t a l need i n Canada, e s p e c i a l l y i n a l l n o r t h e r n a r e a s . The problems i n v o l v e d have been u n d e r s t u d y f o r sornc t i m e under t h e d i r e c t i o n of t h e Group on Drum S t o r a g e of F u e l ,

The D i v i s i o n of B u i l d i n g Research h a s been p r i v i l e g e d t o p a r t i c i p a t e i n t h i s work t h r o u g h t h e P a i n % R e s e a r c h

L a b o r a t o r y of i t s B u i l d i n g M a t e r i a l s F e c t i o n , i n c o l l a l ~ o r a t i o n w i t h t h e D i v i s i o n of Mechanical E n g i n e e r i n g : t h e Royal

Canadian A i r F o r c e and t h e o i l companies,

The P a i n t R e s e a r c h L a b o r a t o r y h a s u n d e r t a k e n t o c a r r y o u t a l l n e c e s s a r y l a b o r a t o r y work on t h e e v a l u a t i o n of c o a t i n g f o r m u l a t i o n s f o r i n t e r i o r and e x t e r i o r a p p l i c a t i o n t o s t e e l drums. T h i s f i r s t r e p o r t d e a l s w i t h t h e work done on i n t e r i o r c o a t i n g s ,

Ottawa,

(4)

O H G A N I C COATINGS FOR THL INTERIOR OF GASOLINE DRUMS by

D.

G e n n i s , B. S o S t a f f o r d and J, H a r r i s

I n t r o d u c t i o n

The P a i n t R e s e a r c h L a b o r a t o r y u n d e r t o o k , f o l l o w i n g a d e c i s i o n rnade by t h e Group o n t h e Drum S t o r a g e o f F u e l on F e b r u a r y 1 0 , 191;3,

t o e v a l u a z e v a r i o u s c o a t i n s f o r m c l a t i o n s f o r i n t e r i o r and e x t e r i . 9 ~ a p p l i c a t i o n t o s t e e l drums, T h i s r e p o r t d e a l s w i t h t h e work t o d a t e on i n t e r i o r c o a t i n g s , An i n t e r i o r c o a t i n g , t o be e f f e c t i v e , must . ? r e v e n t c o r r o s i o n of t h e s t e e l drum and h e n c e i n c r e a s e t h e s t o r a g e l i f e of t h e f u e l b T h i s p r o t e c t i o n may b e needed f o r p e r i o d s a s l o n g a s t e n y e a r s dependfng upon t h e t y p e o f f u e l b e i n g s t o r e d . C o a t i n g s must h a v e good r e s i s t a n c e t o t h e f o l l o w i n g f o r c e s : 1) s o l u t i o n b y t h e f u e l b e i n g s t o r e d ; 2 ) c o r r o s i o n ;

3 )

f r a c t u r e by impact a t low t e m p e r a t u r e s , I n view of t h e c o n s i d e r a b l amount o f r e s e a r c h c a r r i e d o u t

f

on t h i s p r o b l e m by t h e U.S. ~ r m ~ ( l s t u d i e s i n t h i s p r o j e c t were l i m i t e d t o t h o s e c l a s s e s of c o a t f n g s which showed most praornise f r o m t h e work c a r r i e d o u t i n t h e U,S.A, These i n c l u d e a v a r i e t y of

m o d i f i c a t i o n s o f p h e n o l i c r e s i n s w i t h v i n y l , a l k y d and epoxy r e s i n s and a l l r e q u i r e b a k i n g , A number o f a i r - d r y i n g v i n y l b a s e form- u l a t i o n s were t r i e d a s w e l l a s s e v e r a l commercial m a t e r i a l s ,

Two s e r i e s of f o r m u l a e were p r e p a r e d and e v a l u a t e d , The f i r s t s e r i e s was e x p l o r a t o r y ; t h e second s e r i e s was a n e x ~ e n s i o n and e l a b o r a t i o n o f t h e f i r s t , F o r m u l a t i o n s f o r a l l t h e c o a t i n g s p r e p a r e d i n t h e l a b o r a t o r y a r e g f v e n i n Appendix A , p a g e s A : t o A l l ,

E l e v e n f o r m u l a t i o n s were o r i p i n a l l y p r e p a r e d . These were a s s i g n e d t h e l a b o r a t o r y numbers 1101L t o 1 1 0 2 4 i n c l u s i v e . The f o r m u l a t i o n s a r e g i v e n i n Appendix A , p a g e s All t o

AS

These c o a t i n g s were t e s t e d on 2

3/4-

b y 6 - i n c h , t w e n t y gauge, S.A,E, 1 0 1 0 , c o l d r o l l e d s t e e l p a n e l s , The P a n e l s were f i r s t c l e a n e d a c c o r d i n g t o t h e p r o c e d u r e o u t l i n e d i n method 1 0 0 . 1 o f t h e C a n a d i a n Government S p e c i f i c a t i o n Board'sf'Schedule o f Methods of T e s t i n g P a i n t s and pigments", 1-GP-71. The C o a ~ i n g s were

a p p l i e d by d i p p i n g t o a d r i e d f i l m t h i c k n e s s o f a p p r o x i m a t e l y

5

r n i ~ r o n s ,

(1) R e f e r e n c e : l e t t e r and r e p o r t frorn Q u a r t e r m a s t e r - G e n e r a l , W G R T 400, December 22, 1 9 5 2 , N O R O C , f i l e number M2-17-135-6,

(5)

The p a n e l s were s u b j e c t e d t o t h e t e s t s d e s c r i b e d below a f t e r t h e r e q u i r e d b a k i n g s c h e d u l e o r i n t h e c a s e o f t h e a i r - d r y i n g c o a t i n g s , a f t e r d r y i n g f o r one week a t 7 3 ' ~

+

3 . 5 " ~

and 5 0 p e r c e n t

+ 5

p e r c e n t r e l a t i v e h u m i d i t y . A l l t e s t s w e r e - c a r r i e d o u t i n d u p l i c a t e .

A

-

G a s o l i n e R e s i s t a n c e

Coated p a n e l s were immersed t o a d e p t h o f two i n c h e s i n a v i a t i o n g a s o l i n e a t 7 3 ' ~ t

3 . 5 ' ~

f o r one h u n d r e d d a y s . They were

t h e n removed and a f t e r a r e c o v e r y p e r i o d of two h o u r s , were e x a n i n e d f o r any c h a n g e s which may have o c c u r r e d .

B

-

Heverse Impact a t Low T e m p e r a t u r e s

Coated p a n e l s were t e s t e d a t - 2 5 ' ~ and

-SOOc

w i t h a Gardner Impact T e s t e r u s i n 2 t w e n t y . - e i g h t i n c h pounds imi3act, The p a n e l s were a l l o w e d t o r e g a i n room t e m p e r a t u r e t h e n examined f o r c r a c k s o r l o s s of a d h e s i o n on t h e convex s u r f a c e u s i n g a m i c r o s c o p e o f t e n power m a g n i f i c a t i o n , Any change i n t h e c o a t i n g by c r a c k i n g o r l o s s

of a d h e s i o n was c o n s i d e r e d a f a i l u r e ,

C

-

C o r r 3 0 s i o n R e s i s t a n c e

Coated p a n e l s were t e s t e d f o r r e s i s t a n c e t o s a l t f o g a c c o r d - i n g t o t h e A,S,T,M. method B l l 7 , " T e n t a t i v e Method o f S a l t S p r a y

( F o g ) ~ e s t i n g " u s i n g a 20 p e r c e n t s a l t s o l u t i o n , The e d g e s o f t h e p a n e l s were d i p p e d i n a n a i r - d r y i n g enamel b e f o r e e x p o s u r e t o f o r m a 1 / 4 - i n c h b o r d e r around t h e p a n e l ,

D

-

Steam R e s i s t a n c e

---

Coated p a n e l . ~ were suspended i n a s t e m b a t h f o r

4-8

h o u r s , The p a n e l s were removed and examined f o r any c h a n g e s which may h a v e o c c u r r e d ,

E

-

A l k a l i R e s i s t a n c e

C o s t e d g a n e l s were immersed i n 1 0 p e r c e n t sodium h y d r o x i d e s o l u t i o n a t 1 0 0 F f o r t h i r t y m i n u t e s , The p a n e l s were removed and examined f o r any c h a n g e s which may have o c c u r r e d ,

3 ,

---- Obsepvat+ o n s ----

(6)

TABLE

I

GASOLINE, IMPACT, STEAM

AND

ALIUiLI RESISTATICE OF COATEE PANELS

-

-

Laboratory

Gasoline

Reverse Impact

Steam

Alkali

Number

Panel Resistance

Resistance

Resistance desistanc

-2s0c

-soOc

CoRo

C.R.

C o R e

C.R.

C.R.

CeX*

NoCe

NoCa

N.

C,

N.C.

No

C

0

N.C.

NoCo

N. C

,. N o C e

N.C.

NoCo

N.Ce

N.Co

NoCo

MeC.

N.C.

LEGEND:

P

denotes pass;

F

denotes failure;

-

denotes test not done;

N,C,

-

No Change

(7)

TABLE I1

CORROSIOTJ RESISTAKCE OF COATED PANELS

L a b o r a t o r y

N-mb e r C o n d i t i o n

11014

Rust s p o t s a p p e a r e d a f t e r one day 11015 R u s t s p o t s a p p e a r e d a f t e r one day 11016 Rust s p o t s a p p e a r e d a f t e r t h r e e days 11017 S e v e r e r u s t i n g and s t r e a k i n g a f t e r t h r e e days A few b l i s t e r s a p p e a r e d a f t e r t h r e e d a y s , b u t no r u s t i n g t i l l n i n e d a y s 11020 Rust s p o t s a p p e a r e d a f t e r t h r e e d a y s 11021 S e v e r e r u s t i n g and s t r e a k i n g a f t e r t h r e e d a y s 11022 S e v e r e r u s t i n g and s t r e a k i n g a f t e r t h r e e days 11023 Rust s p o t s a p p e a r e d a f t e r f o u r t e e n d a y s 11024 Rust s p o t s and s t r e a k i n g a p p e a r e d a f t e r t h r e e d a y s

k.

Summarv of R e s u l t s on F i r s t G r o w o f F o r m u l a t i o n s I n t h i s s e r i e s :

a ) samples 11015, 11017 and 11023 were t h e most r e s i s t a n t t o f r a c t u r e by impact a t low t e m p e r a t u r e ;

b ) samples 11016, 11019, 11020 and 11023 gave t h e b e s t c o r r o s i o n p r o t e c t i o n t o s t e e l , Sample 11023 was t h e b e s t i n t h i s r e s p e c t ;

c ) a l l f o r m u l a t i o n s t e s t e d were u n a f f e c t e d by steam;

d ) samples 11015, 11019, 11020, 11023 and 11024 had s a t i s f a c t o r y r e s i s t a n c e t o a l k a l i .

5.

P r e p a r a t i o n of and T e s t s on t h e Second Group o f F o r m u l a t i o n s

On t h e b a s i s of t h e f o r e g o i n g r e s u l t s , i t was d e c i d e d t o p r e - p a r e a more comprehensive group o f f o r m u l a t i o n s t o b e t e s t e d i n a

(8)

p h e n o l i c - p o l y v t n y l b u t y r a . 1 and s e v e r a l y l a s t i c i zed ~ ~ i n y l c h l o r i d e -,

v i n y l - a c e t a t e copolymer f o r m u l a t i o n s which Report; TvTumber 1 7 8 1 o f t h e N a t i o n a l Bureau o f S t a n d a r d s had shown t o p o s s e s s des?.ral::le c h a r a c t e r a i s t i c s .

The f o r m u l a e a r e g i v e n i n Appendix A , p a g e s

AS

t o A l l , T:I a d d i b i o n , c o a t i n g s numbers 11015, 11017, 11020, and 11023 o f the p r e v i g u s s e t and 10956, 10965, 10968 and 10969 which a r e cornmerc-:.A cpoxy c o a t i n g s were i n c l u d e d i n t h f s s e r i e s .

T e s t s on t h e s e samples were c a r r i e d o u t a c c o r d i n g t o t h e metehods d e s c r i b e d on page 2

.

The ~ o s t i m p o r t a n t c h a r a c t e r i s t i c s o f t h e s e c o a t i n g s were r e s i s t a n c e t o c o r r o s i o n by s a l t f o g , r e s i s t a n c e t o f r a c t u r e by r e v e r s e impact a t low t e m p e r a t u r e , and r e s i s t a n c e t o g a s o l i n e , It was d e c i d e d n o t t o t e s t t h e s e c o a t i n g s f o r a l k a l i and s t e a m r e s i s t a n c e s i n c e t h e s e p r o p e r t i e s werc a l r e a d y showri t o be v e r y good f o r these t y p e s o f c o m p o s f t i o n s ,

The c o a t i n g s were t e s t e d on

4-

by 6 - , i n c h , t w e n t y , f o u r gauge,

SAE

1020, c o l d r o l l e d s t e e l p a n e l s . They were a n p l i e d a t a d r i e d f i l m t h i c k n e s s o f 1 2 , s

+

2.5 m i c r o n s . A f t e r t h e s u i t a b l e b a k i n g s c h e d u l e , o r a f t e r a i r - d F Y i n g f o r one week a t

7 3 ' ~

+

3 e 5 0 ~

and 50 p e r c e n t

-

+ 5

p e r c e n t r e l a t i v e h u m i d i t y i n t h e caseRof a i r - d r y i n g . f i n i s h e s , t h e p a n e l s were t e s t e d i n t h e same manner a s t h o s e of t h e p r e v i o u s s e r i e s e x c e p t t h a t t h e r e v e r s e Impact t e s t s were p e r f o r m e d a t O'C,

-

20°C and -25OC.

These t e s t s were c a r r i e d o u t i n d u p l i c a t e and t h e r e s u l t s a r e g i v e n i n T a b l e s I11 and. I V ,

(9)

TAGLE

I11

lILSISTATTCL OF'

COATEL

PklJEL? TO SALT SPliAY COHILO SIOI'J

L a b o r a t o r y Cays 3umb e

r

P a n e l Exposed C o n d i t i o n No change Few

/#?I

b l i s t e r f n g Kedium

#8

b l i s t e r i n ~ Complete l o s s o f a d h e s i o n o v e r t o p h a l f o r t h e p a n e l

-

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~ ~ e d i u r n . chan#e

8

o l i s t e r i n e o v e r

SO:,

or tile p a n e l

R l i s t e r f n . ~ s i z e and d e n s i - t y hiis i n - c r e a s e d and c a u s e d col;tlpl;.3f;e loss

of . a d h e s i o n o v e r 50:;; of t h e pane7'

-. F'ii 1 LzTJ

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$8

b i i s t e r i n f : o v e r p a n e l

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a l l a r e r u s t in:, and trios t of a r e st.realiin,y

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No chanpe Piedium

#8

b l i s t e r i n g o v e r p a n e l and two l a r y e ( $ ' I d i a a , ) r u s t b l i s t e r s 30'" , .I of b l i s t e r s a r e rus-bin[< anrl. s t r e a k . i n : -

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F A I L 3 9 No cLiin2:e K O c h a n : ~ e No clianr1.e Few

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776

b l l s t e r i n f i ;

-

fel-,J blisters a r e r u s t in,? and s t r e a k i n p - F A I L X I

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chanpe No chanple Fo c h a n ~ e

Few

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b P i s % e r i n ~ 25::. of b l i - s t e r s a r e r u s t streakin.::

--

FA

I

T.:XD No chanye No chznpe No chanp;e P'Iedium d e n s e

# 9

b l i s t e r i n g i 3 l . i ~ t e r i n . 5 i n c r e a s in?; i n d e n s i t y Dense

#q

b l i s t e r i n ? ;

-

n o s t o.f b l i s t e r s a r e r u s t i n c

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PJo change Few t o medium

#9

b l i s t e r a i n g

No

shancye Hediurn

89

b l i s t e r i n g

(10)

TA

.-!L;<

I1

I c o n t h u e d . --- Lalooratory Cays E:umL e r

--

---

--

P a n e l Exposed

-

---

C o n d i t i o n

,,

, , , , . i ~ n i p. F! t o medium d.ense

#9 51

i s t e r l r r i , - P ~ ~ e n s e

# a

S l i s - t e r i n r r <-,

-

most 0:;' 5 l i s t e r s a r c r u s t i n $ ;

-

F H P ~ ~ ~ ~ . ~ No chanqe 1:ediurn

k'9

b l i s t e r i n 5

-

1 0 a r e r u s t i n p : anti

streak in^

-

FAILED Few t o r i : e d i ~ l n

#9

listeri in^

F!Ted4.um

# q

b l i s t e r i n r p

-

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-

FAILED Yo chanrre Few

#8

b l i s e r i n m o v e r t o p 20::: of p a n e l

-

a l l a r e r u s t i n g 2 0 ' of b l i s e r s have s t a r t e d t o s t r e a l ;

-

FAILFT; Fo chang;e P;edfum d e n s e

H 8

b l i s t e r i n g over t o p 2wL of p a n e l

-

most a r e r u s t i n g and s t r s a k i n s

-

F A I L I D No change One s m a l l

( l / q r '

d i a m . ) r u s t s p o t Kedium d e n s e

k8

b l i s t e i n g Kedium d e n s e t o d e n s e

$8

b l i s t e r i n e

-

30$ a r e r u s t iiig and s t r e a k i n g

-

?'AILED No change No chan,rl;e 1~umerou.s w h i t e s p o t s

(3/16"

diam. )

-

some a r s b l i s t e r i n g E l i s t e r i n g i n c r e a s i n g

No

chhn,.:e S e v e r e b l i s t e r i n g , r u s t i n ~ ~ n d . s t r e a k i n , y

-

FAILED FC) chanc;e R O change

About

1.2

a r e a s o f rnediurn ,dense

#

8

b l i s t e r i n p ; 257: of p a n e l a r e a a f f e c t e d l ~ ~ e d i u m d e n s e

$8

b l i s t e r i n p o v e r p a n e l No cban!;e P a n e l i s d a r k e n i n g b u t n o s u r f a c e r u s t P a n e l i s s t a r t i n s t o s t r e a k

-

FAILED

No c h a n ~ e No change No c h s n ~ e P m e l i s d a r k e n i n g No change No change

(11)

TA3LE I11 c o n t i n u e d L a b o r a t o r y Num is e r

---

Pane 1 Days Exposed C o n d i t i o n No change No change Median t o medium#

8

b l i s t e r i r ~ ~ Medium dense

#8

b l i s t e r i n g

-

vest

showinp r u s t

-

FAILED K O chanpe

P.?o chanSe

EIediurn

#8

b l i s t e r i n g

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few showing r u s t

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FAILED

K O

chanpe No change No chan e Medium

88

b l i s t e r i n g

-

501~

a r e r u s t i n g and s t r e a k i n p

-

FAILTJ One r u s t s p o t No change Medium dense #8 b l i s t e r i n g

50$

of b l i s t e r s a r e r u s t i n g and s t r e a k i n g

-

FAILED

Many w h i t e s p o t s (+I' d i a m , )

-

two

a r e showing r u s t S e v e r e r u s t i n g and s t r e a k i n g

-

FAILZD Many w h i t e s p o t s

-

3

a r e r u s t i n g and t h e o t h e r s a r e b l i s t e r i n g S e v e r e r u s t i n c and s t r e a k i n g

-

FBILZD No change Medium b l i s t e r i n g

-

257; of b l i s t e r s a r e r u s t i n p ;

-

FAILED No change Few v e r y s m a l l r u s t s p o t s Medium

#8

b l i s t e r i n g

-

257:

of b l i s t e r s a r e r u s t i n g

-

FAILED No change Few

#8

b l i s t e r i n g

-

a l l a r e r u s t i n g and s t r e a k i n g

-

FAILED Few

#8

b l i s t e r i n g

-

a l l a r e r u s t i n g and s t r e a k i n g

-

FAILEC No change About 50 s m a l l b l a c k s p o t s b e n e a t h s u r f a c e No change

Black s p o t s have s t a r t e d t o show s u r f a c e r u s t

-

FAILED No change Few s m a l l b l a c k s p o t s beneath s u r f a c e About 100 s p o t s now S p o t s i n c r e a s i n g i n a r e a

( 3 / 8 "

diam.) S e v e r e r u s t i n g b e n e a t h s u r f a c e

-

FAILED

(12)

TABLk I11 c o n t i n u e d Laboratory Days Number P a n e l hxposed C o n d i t i o n 11032 A

3

Few

#8

b l i s t e r i n g

7

No change 11 About 10 b l a c k s p o t s beneath s u r f a c e 1 8 No change

$2

No change Area of d a r k s p o t s i n c r e a s i n g but; no s u r f a c e r u s t i n g y e t

46

Severe r u s t i n g , b l i s t e r i n g and s t r e a k i n g

-

FAILbU B

3

No change

7

No change

11 A few b l a c k s p o t s

(l/ol'

diam.) beneath s u r f a c e

18

No change

t 2

No change No change

46

Severe r u s t i n g , m i s t e r i n g and s t r e a k i n g

-

FAILED A

3

No change

7

No change 11 No change 1 8 No change

$2

Panel i s s t a r t i n g t o darken No change

4-6

Severe darkening beneath s u r f a c e

-

FAILED B

3

No change

7

No change 11 No change 1 8 No change 25 Panel i s s t a r t i n g t o darken

8

No change

Severe darkening beneath s u r f a c e

-

FAILED A

3

No change

7

No change ' 11 Few #8 b l i s t e r i n g

18

B l i s t e r s a r e r c s t i n g and s t r e a k i n g

-

FAILED B

3

No change

7

Few

#8

b l i s t e r i n g 11 Few t o medium

#8

b l i s t e r s

18

Dense

#8

b l i s t e r i n g

-

FAIL%

(13)

L a ' r ~ o r a t o r y Xumb e r P a n e l TABLE 111 c o n t i n u e d Cays Exposed C o n d i t i o n

3

2 v e r y s m a l l (1/1011 diam. ) r u s t a r e a s

7

No change 11 About 30 w h i t e s p o t s

(it'

d i m , ) b e n e a t h s u r f a c e

18

White s p o t s have b l i s t e r e d and a r e s t a r t i n g t o r u s t

-

FAILED

3

No change

7

3

v e r y s m a l l (1/16" d i m . ) r u s t a r e a s

11 About 1 2 r u s t s p o t s

(if'

diam. ) FAILED

3

No change

7

Few v e r y s m a l l (1/16" d i m , ) r u s t a r e a s 11 Mediurn #8 b l i s t e r i n g

18

SO$

of r u s t s p o t s have s t a r t e d t o s t r e a k

-

Ff'iILED

3

No change

7

Few v e r y s m a l l (1/16" diam, ) r u s t a r e a s 11 No change

18

About 50% ,&, b l i s t e r s t h a t a r e r u s t i n g 40% a r e s t r e a k i n g

-

FAILEE

3

No change

7

Few v e r y s m a l l r u s t a r e a s

( l / l h t '

d i m . 11 Few

#8

b l i s t e r i n g

18

80;:

of b l i s t e r s a r e r u s t i n g

-

FAILED

3

No change

7

Few v e r y s m a l l r u s t a r e a s ( l / 1 6 ' t d i a m . ) 11 Few #8 b l i s t e r i n g

-

00;%

a r e r u s t i n g

-

FAILED

3

bout 1 2 r u s t a r e a s

(1,/0*

d i m , ) o v e r 25% of p a n e l

-

a l s o many w h i t e s p o t s b e n e a t h t h e s u r f a c e .

"7

S e v e r e r u s t i n g and s t r e a k i n g

-

FAILED

3

No change '7

I About 20 a r e a s

(in

diam.) of

r u s t

-

FA1LL.D

3

Medium

#8

b l i s t e r i n g

-

a l s o many r u s t a r e a s

(1/8"

d i m , ) - FAILED

3

No change

7

S e v e r e r u s t i n g and s t r e a k i n g

-

FAILEG

3

No change

7

About 20 a r e a s (3/16" d i a m , ) of s e v e r e r u s t i n g . and s t r e a k i n g

-

FAILED No change S e v e r e r u s t i n g o v e r t o p 255 of p a n e l

-

F'AILED

-

-

(14)

TAbLTi; I I I coiii;inued --

-

.-.- La-::.orat o r y Number Days P a n e l Exposed C o n d i t i o n ..-

3

r u s t a r e a s (1/:3" d i a m . ) Few r u s t a r e a s t h a t a r e s t ~ e a k i n g

-

FAILED No change Few r u s t a r e a s t h a t a r e s t r e a k i n g

-

FAILED S e v e r a l r u s t a r e a s t h a t a r e s t r e a k f n g

-

FAILED S e v e r a l r u s t a r e a s t h a t a r e s t r e a k i n g

-

FAILEG

Few t o mediim

#8

b l i s t e r i n g and

two s m a l l r u s t a r e a s ( l / f j l ' diam, ) S e v e r a l r u s t s p o t s a t t h e t o p o f p a n e l Tdllich a r e s t r e a k i r l g

-

FAILED No change About 1 0

#4

b l i s t e r s o v e r p a n e l -dhich a r e s t r e a k i n g ' - FAILEG Four l a r g e r u s t a r e a s (5/16" d i a r ~ , ) t h a t h a v e s t a r t e d t o s t r e a k

-

FA I USD C o a t i n g h a s l o s t a d h e s i o n - FAILED

3

S e v e r e r u s t i n g and s t r e a l r i n g o v e r p a n e l

-

FAILED

3

S e v e r e r u s t i n g and s t r e a l t i n s o v e r p a n e l

-

FAILED

3

Few r u s t a r e a s

(118"

d i a m . )

7

Complete l o s s of a d h e s i o n '== FAILE13

3

F i v e r u s t s p o t s o v e r p a n e l t h a t a r e s t r e a k i n g

-

FAILED

3

No change

7

S e v e r e s t r e a k i n g from medium j'8 b l i s t e r s *-= FAILil,L;

3

Plediurn

#8

b l i s t e r i ~ g r 9 30% a r e r u s t i n g and s t r e a k i n g

.-

FAILED Note: The

size

and d e n s i t y o f any b l i s t e r s a r e r e p o r t e d a c c o r d i n g

t o t h e A.S.T.M. method f o r E v a l u a t i n g Degree o f B l i s t e r i n g

(15)

T A B L E I V G A S O L I N E AND R E V E R S E I M P A C T R k , S I E T A N C E OF G O A T E E PAI'TITLS

---

L a b o r t a r y G a s o l i n e N u m b e r Panel R e s i s t a n c e R e v e r s e Impact R e s i s t a n c e 1 0 0 days 0 ° C -:2OUC - 2 5 ° C

-

10956

A No C N e C e C.R. COT!O N.C. N.C. i\To,Co N a C e NOC. C o R , N a C e N.C. C o R . C .I?, A N, C. C . R . C , H , C , R o C o R o C , R , C . R . C.Ii. B N.C. C O H O C o R o C a R o N o C o N oC 0 N o C e C o R e C . R o N o C o N e C o C o R o N o C o N o C . N o C e C 0 Ii, C , R o C.R. A N o C o m.3

-

B

N,

C.

-

-

-

-

(16)

T A B L E I V c o n t i n u e d L a b o r a t o r y G a s o l i n e N u m b e r P a n e l R e s i s t a n c e R e v e r s e I m p a c t R e s i s t a n c e -

---

100 days 0 ° C - 2 0 ° C

-..~sac

N o C e N o C e N.C. N o C e N.C. N e C o No C o N o C. N. C ,

PJ,

C , N , C . N o C o N o C a N, C. N.Co N o C e N o C e N.C. NQCO NoCo WOCO N.C. C e R e CUR. N.Co N o C o COHO C O H O C , R . C o R o C o R o C , R . C . R e C o R o C e H , C o R o C o R e C.H. C.R. C o H e C o R o C o R o C o R o C o R o No Co N.C. C o R o C , R , C OR0 C . H a C , R , C O H O C o R e C . R . C.R. C.Ro C .R, COHO C o R e C , R , L E G E N D : - d e n o t e s t e s t n o t done; N e C ,

-

N o C h a n g e ; C o R e C r a c k e d

(17)

TABLB I V continued L a b o r a t o r y G a s o l i n e Numb e r Panel R e s i s t a n c e R e v e r s e I m p a c t R e s i s t a n c e 1 0 0 d a y s O°C - 2 0 P C

-325"

C 11040 A N. C. N o C o N ,

c

.

N.C, B N . C o N. C . C O H O C U R .

11041

A

ram c o

C.R. C o R o C o H - B N e C a C e i i O C o H a C o R e 11042 A N o C o C - R , C , K . C , R . B N e C o C o R o C e

H e

C e R e

11044

A N o C. C e R e C o H o C o H o B N o C . C o R e C O H O C oHo

1104.5

A N e C e C e R o C o K O C OR, B N a C m C a R o C o R o C o R o

11046

A N o C e C

OH

o C o R o C o R o B N o C 0 C o R o Co Ro C o R o

11047

A N.C. C o R e C o R a C o R o B N o C o COHO C e R o C o R o

11048

A

N.

C , C , R , C . R . C o R . B No C a C o R e C * H o C o R o

11049

A N . C m N o C e N o C o i\i o C 0 B N.C. N.C.

N o

C , N.C. LEGEND: - d e n o t e s t e s t n o t done; N.C.

-

N o C h a n g e ; C o R o

-

C r a c k e d

(18)

S u m ~ a r y of t h e Second F e r i e s o f T e s t s The r e s u l t s o f t h e s e t e s t s show t h a t t h ~ c o a t i n g s

10968,

10969, 1 1 0 2 3 , 11032 and 11033 h a v e b e t t e r c o r p o s i o n - r e s i s t z n t p r o p e r t r i e s t h a n t h e r e r n a i n i n ~ f o r 7 - c ~ u l a t i o n s of t h e s e r i e s , S ' m p l e s 1 0 9 6 8 a ~ l ~ d 'C)969 a r e c o m m e r c i a l t t l e r m o - s e t t i n g epoxy f o r m u l a t i d ~ l s , s a m p l e s 11023 and 11033 a r e v i n g l i d e n e c h l o r i d e - a c r y l o n i t r i l e c o p o l g ~ ~ e r 1 o r m u l a t i o n s and 11032 i s a p h e n o l i c - v i n y l f o r r r . u l a t i o n . The t e s t s f o r r e s i s t a n c e t o f r a c t u r e

a t

low t e m p e r a t u r e s by i m p a c t were more s e v e r e i n t h i s s e r i e s s i n c e t h e f i l x thickness h a d b e e n i n c r e a s e d . Samples 10965, 10969 and 11049 showed b e s t

i m p a c t r e s i s t a n c e i n t h i s s e r i e s . Samples 10965 and 10969 a r e t h e r m o - s e t t i n g epoxy t y p e f o r m u l a t i o n s w h i l e 11049 i s a n a i r - d r y i n g v f n y l f o r m u l a t i o n . A l l t h e c o a t i n g s were u n a f f e c t e d by i m m e r s i o n in a v i a t i o n r a s o l i n e f o r 1 0 0 d a y s , 0

7. E f f e c t o f Using Wask-primed and P h o s p h a t i z e d

-

S t e e l

-

The e f f e c t o f u s i n g a wash-primed s u r f a c e and a p h o s p h a t i z e d s u r f a c e was a l s o s t u d i e d i n a n a d d i t i o n a l s e r i e s ,

S t e e l ~ a n e l s o f t h e same z a u g e and t y p e u s e d i n t h e f o r e - g o i n g s e r i e s were c l e a n e d a c c o r d i n g t o method 1 0 0 , l o f t h e C a n a d i a n Government S p e c i f i c a t i o n B o a r d ' s " S c h e d u l e o f Methods o f T e s t i n g P a i 2 t s and p i g m e n t s " , 1-GP-71. These p a n e l s were t h e n

di,.

a,oated w i t h a v i n y l - t y p e wash p r i m e r ( l a b o r a t o r y number 1 1 1 3 0 ) , The formulation of t h i s m a t e r i a l i s g i v e n i n p a s e

All

o f Appendix A,

The d r i e d f i l m t h i c k n e s s of t h i s m a t e r i a l w a s l e s s t h a n 2.5 m t c r o n s , The p r i n e r was a l l o w e d t o d r y f o r a p p r o x i m a t e l y one h o u r a t room t e m p e r a t u r e and t h e p a n e l s were t h e n d i r z o a t e d w i t h c o a t i n g s 1 1 0 2 3 , 1 1 0 3 5 , 11040, 1104.2 aqd 1104.6 t o a t o t a l d r i e d f i l m t h i c l i i l e s s b e -

t w e e n 1 0 and

15

m i c r o n s .

These c o a t i n g s were a l s o a p p l i e d t o p h o s p h a t i z e d s t e e l p a n e l s . These p a n e l s were o f 24-gauge s t e e l a n d h a d a z i n c p h o s p h a t e c o a t i n g of 200 m i l l i g r a m s p e r s q u a r e f o o t , The o r g a n i c c o a t i n g t h i c k n e s s was b e t w e e n 1 0 and

15

m i c r o n s .

A f t e r b a k i n g u n d e r t h e p r e s c r i b e d c o n d i t i o n s o r a f t e r d r y i n g f o r one week a t 7 3 ' ~

+

3.5'F and 50 p e r c e n t

+ 5

p e r c e n t r e l a t i v e h u m i d i t y f o r t h e a i r - T r y c o m p o s i t i o n s , t h e p a n e l s were s u b j e c t e d t o t h e c o r r o s i o n and t h e r e v e r s e i m p a c t t e s t s a s d e s c r i b e d f o r t h e p r e v i o u s s e r i e s , A l l t e s t s were c a r r i e d o u t i n d u p l i c a t e ,

8,

O b s e r v a t f o n s

(19)

TABLE; V H E S I S T A X C E O F C O A T I N G S ON P H L T R Z A T E D P A N E L S T O F H A C T U R E BY I M P A C T L a b o r a t o r y W a s h - P r i n e d S u r f ace P h o s p h a t f z e d I T m b e r Panel, S u r f a c e 0 ° C -15°C - 2 S 0 C

oOc

- 1 5 ° C - 2 5 ° C C . R . C a R a

N o

C . N , C . No C 0 N , C o N e C o N o C o C o R o C . R , C e R o C e R o C a R e C , R , C U R o C e R o C . R , C o R e C ,

R.

C.R. N , C , N o C o C o R ,

C,K.

COR. C o R e C m R o C.H, C o R o C.R. C , R , C.R. C . H , cefi.

No

C C , I3 0 C * I j a C e R o C o R e C.H, L Z G E J D : C , R e

-

C r a c k e d ; N , C o = . NG C h a n g e -

-

C O i i 8 9 5 1 0 3 T R E S I S T A N C E OF C O A T I N G S ON WASH-PRIMED S T E L L L a b o r a t o r y D a y s N u m b e r P a n e l Exposed C o n d i t i o n S i x

#8

b l i s t e r s s c a t t e r e d o v e r p a n e l

-

t h e y a r e r u s t i n g and s t r e a k i n g

-

F A I L E D N o change N o change

No

chs*lge A b o u t 500 s m a l l r u s t s p o t s ( 1 / 1 6 " d i a m , :

-

20% a r e s t r e a k i n g

-

F A I L E D N o change N o change N o change S e v e r a l w h i t e s p o t s b e n e a t h s u r f a c e ( 3 / 1 6 I t d i a m , ) 40% a r e s t a r t i n g t o r u s t

(20)

TABLE V I c o n t i n u e d Lalr,oratory Days l\T urib e r P a n e l Lxpo s e d -- - -- 1 1 0 3 5 A 25 25;: o f p a n e l c o v e r e d i n ~ > ? n i t ~ : ~ p o t s (3/16" diarn, ) t h a t a r e r 1 i ~ s t i 1 z ; ;:?ld

blister in^

-

FAIL-l5D 2 No chnn:?;e

3

TJo change

1 1 No change

1 0 About 2 5 w h i t e s p o t s benca.tl:~ ::urTf'ace 2 5 ?;evere r u s t i n g ant? strc:zLl;i~p;

-

I,"ii2:Li:~I;

2 IJo c h . a n ~ e

3

?To cln ange 11 1b:edium d e n s e b l l . - t e r i n ? ; ~ar.:; L o s s of a d h e s i o n o v e r

1.p $

o f p a n e l

-

PI'LILY:,G

2

No ch.ange

3

No change 11 S e v e r e b l i s t e r i l l ; , r u s t i n g an:' s t r e a . 1 ~ - ills

-

FAILLE 2 N o change

3

No change

11 MeL'liuri cie:l:,c, 1, 0 b l i s t e r l ~ . i ; _ tij-iii loss of'

z~Cil:esi~n o v r b-0$ of n a n e l

-

FAILED

2

P*-tjout 1 2

$-'8

bl4 s t e r s which a r e r ~ s ~ s i n g

SO:.;'

a r e s t r e a k i n g

-

I;'I:ILZI; 2 Four r u s t l j l i s t e r s

( l / 4 "

d i m , ) two a r e s t r e a k i n g

-

FAILLL 2 I\'o ch.ange

3

No change 11 Two r u s t b l i s t e r s

( l / I . l l f

d i a n i , )

18

S e v e r e r u s t i n g and s t r e a k i n 2

-

5 3 I L i L ----

-

--- ----

-

.---.-. -,- TALLE 7 J j - I

---

CORR3SION H3F.;IETH7.'?CE 3F C O A T I I J G W T J PEi:CEPiT:7Y'IZ>i!j STTI;II%

-. --

-

.---.--- .-. - -.-.--.-, --"-

--

L a b o r a t org :lags 1Iu:cnb e r P a n e l Exuosed C o n d i t i o n No cilange

?TO

changc No change Wo change

Fetr

#3

b l i s t e r s which art r,s.';f I(- a

-

20$ a r e s t r e a k i n g

-

FAILS3 No change No chznge

NO

cl?ai?ge No c h a n ~ e lsledium

$3

b l i s t e r i n g b u t no rust y e t

-

FAILED

(21)

TA1,LE V I L c,on.t in u e d --.-- - L a b o r a t o r y 3ay s JTmb

er

P a n e l Exposed C o n d i t i ~ ~ l i :i\Jo change No change No change No change About

6

a r e a s

( 3 / 8 "

diam. o f r u . s t l . n g and s t r e a k z n g

-

FAILED No change IJo change No change No change About

6

a r e a s

(3,1'8"

d i a m , ) o f r u s t i r l g and s t r e a k i n g

-

FAILEG NG chznge No change

NG

changs About 1 0 a r e a s o f r u s t i 2 g

-

3

a r e s t r e a k i n g

-

FAILED No change No change No e h a q e No cl-lange S e v e r e r u s t i n g and s t r e a k i n g

-

FAILED No change No change No change About 50 w h i t e s p o t s (3/1bYt d i a m , ) b e n e a t h t h e s u r f a c e L o s s of a d h e s i o n o v e r 40$ of p a n e l

-

FAILED No change TJo change ITo charwe Few s m a 1 . l PUS^ s p o t s ( l / l h " d i m , ) S e v e r e r u s t i n g and s t r e a k i n g

-

FAIL5D About:

6

s m a l l r u s t s p o t s

i,1./0"

d i a r r . )

Nc

change One a r e a (20':; - . o f n a n e l j of s e v e r e r u s t i n g and s t r e a l r ~ & and a f ' e w srnall r u s t s s p o t s

-

FAILEC No change No change One a r e a (20$ o f p a n e l ) s e v e r e r u s t i n g and s t r e a k i n g

-

FAILED

9 ,

Summary o f R e s u l t s on P r e t r e a t e d S u r f a c e s

The u s e o f a wash-primed s t e e l surf'ace improved t h e a d h e s i o n and c o r r o s i o n - r e s i s t a n t p r o p e r t i e s of t h e system, S e v e r a l c o a t i n g s w i t h - s t o o d t h i s r e v e r s e i m p a c t t e s t a t

.

2 5 ' ~ when t h e s u r f a c e was wash-primed,

(22)

The use of the phosphatized surface did not improve the

results obtained i n the reverse impact test, however, this type of

surface pretreatment did inprove the corrosfon-resistant properties

of the system,

10, Summary

Thirty-three samples were tested in this section of the

project, Four of these were commercial thermo-setting epoxy

formulations of which the detailed

compositions

were not known.

The general non-volatile ,vehicle

combinations c,onsidered were:

catalytically cured epoxy

epoxy-phenolis

phencllie

phenolfa,-epoxy-.urea

formaldehyde

phe~olir-epoxy-polyviny1

butyrak

phenolic-polyvinyl butyral

phenolic-alkyd-polyvinyl formal

vinylidene chloride-acrylonitrile copolymer

modified vinyl chloride-vfnyl acetate copolymer

The properties of the formulations prepared i n these

laboratories varied markedly,

In

general, sample 11023, which is

vinylidene chloride-aerylonitrire formxiation, had the best all-

round properties, but is difficult to appiy by spraying, Coating

11032,

which is

a

phenolic-,vinyl formulation, showed excellent

resistance to corrosion by the method used, however, its resistance

to impact was not as g ~ o d

as many other materials.

Several samples showed better resistance to fracture by

impact at low temper3atures than the remainfng compositions, These

samples, 11031? l1040, and

11049

were of phenolic-,epoxy-vinyl.,

phenolic.-.v-f.nyl

and vinyl compc

sition.

All the samples tested showed excellent resistance to

gasoline, From the tests carried out on the ffrst series of

co:tfngs and from general information on the resin structures,

ft

may be assumed that any formulation containing appreciable a m o ~ m t s

of alkyd, polyvinyl butyral or polyvinyl formal resins will

b e

attacked by hot caustic

solutions,

On the basis of these tes-t

rbesult.s

the following coatings

are recommended for further

testing through field exposures:

1) llOl,rg

Phenolic-polyvinyl butyral coatfng

2 )

21022

Catalytf

eally cilred epoxy coating

3 )

11023

Vinylidene chloride-aerylonftrila copolymer

coating

(23)

P h e n o 1 . i ~ - e p o x y - p o l y v i n y l b u t g r a l c o a t i n g Phenoli c-polyvinyl b u t y ~ a l c o a t i n g

.

Vinyl c h l o r i d e - v i n y l a c e t a t e copolymer

c o a t i n g

8 )

10965 Commercial epoxy c o a t i n g

T e s t s were a l s o c a r r i e d out i n t h i s p r o j e c t with w a s h - ~ ~ i r n e d and phosphatfzed s t e e l a s s u b s t r a t e s f o r t h e s e c o a t i n g s , The t e s t s show t h a t t h e s e s u r f a c e p r e p a r a t i o n s w i l l improve t h e adhesion of t h e organic c o a t i n g s and t h e c o r r o s i o n r e s f s t a n c e of t h e system as well,

It

i s recommended t h a t drums with s u r f a c e p r e t r e a t m e n t be included i n t h e f i e l d t e s t s ,

(24)

APPENDIX

A

FORPIULATION OF THE COATINGS

A.

Composition of Interior Erum Coatings

Phenolic-Vinyl Coating

Laboratory number llOllC

N,R,P,

50

Parts by weight

-

Phenolic resin solution

:Resinox P-97

51.0

Polyvinyl butyral resfn

:Butvar B-76

13.5

Sol.vent

;Methyl isobutyl ketone

35.5

Baking schedule: 20 minutes at 350°F',

2.

Phenolic-Epoxy Coatfn~

Laboratory number 11015

N.R,P.

51

Parts by weiaht

Phenolic resin solution

:Resinox P-97

30.3

Epoxy resin

"rpon

1007

15.3

Solvent

:n-Butanol

13*2

:Xylene

13.2

:Methyl isobutyl ketone

27.6

Iron oxide pigment

~Mapico

420

1

.

0

Baking schedule: 30 minutes at

3 5 0 ~ ~ ~

Phenolic

---

Vfn;E:P -

Coating

-

Laboratory number 11016

N.R*Pa

52

-

Parts by weight

Phenolic resin solutfon

:Resinox P-97

Polyvinyl formal resin

a

Formvar F-770

Solvent

:

n-But

an01

:

Xylene

:Methyl isobutyl ketone

Baking schedule: 20 minutes at 3 5 0 ' ~ ~

(25)

Phenolfc-Vinyl Coatinq Laboratory number 1101.7 Ne30P,

53

-

P a r t s by weight P h e n o l i c r e s i n

:R-108

7

0

5

P o l y v i n y l b u t y r a l r e s i n s o l u t i o n

:lo$

s o l u t i o n of Butvar B-76 i n s e c - b u t a n o l 50.0 S o l v e n t : Sec-butanol 29

4

~ D i a c e t o n e a l c o h o l

13.1

C a t a l y s t :

857:

Phosphoric a c i d 0.13 Baking schedule: 40 m i n u t e s a t 330°F0 Phenolic-Alkyd C o a t i n 8 Laboratory number 11018 N"R.P,

54

P a r t s by weight P a r t A ~ l k y d r e s i n s o l u t i o n : Glypt a 1 2480 60,

0

I r o n o x i d e pigment ~ M a p i c o 420 1 0 6 S o l v e n t :n-Butanol 6,O o, Xylene 3 0 9 0 :Methyl e t h y l ketone

3

0 0 :Isophorone 3.0 P a r t B P h e n o l i c r e s i n S o l v e n t C a t a l y s t

:R-108

20

.

o

: E t h y l a c e t a t s 1 1 , O :

85%

Phosphoric a c i d

om5

I n s t r u c t f m f o r uses

One hundred grams of P a r t A were added w i t h s t i r r i n g t o s f x t y - t h r e e grams of P a r t B, The m i x t u r e was u s e d w i t h i n e i g h t h o w s ,

(26)

Laboratory number 11019

N o R o P e

55

Part.s by weight

Phenolic resin

:

K-108

22.3

Zpoxy resin solution

solution of Epon

1007 in a mixed

solvent of

66

parts

of toluene to 22

parts of methyl ethyl

ketone to

12

parts

'

of methyl isobutyl ketone

55.8

Solvent

~957;

Ethyl alcohol

10-6

:

Toluene

10.6

Catalyst

:

85%

Phosphoric acid

065

Baking schedule:

25

minutes at 400°F.

Phenolic-E~osrv-Melamine

Formaldehvde Coatina

Laboratory number

11020

N,E,P.

56

-

Parts by weight

-

Phenolic resin

:R-108

2000

Epoxy resin solution

:SO$

solution of Epon

1007 in a mixed

solvent of

50

parts

of diacetone alcohol

to

50

parts of xylene

32.0

Melamine-f

ormaidehyde re

sin

solution

~Resimene

875

8,o

Solvent

:Gfacetone alcohol

20.0

:

Xy-bene

16,0

Catalyst

:

85%

Phosphoric acid

002

Baking schedule:

26

minutes at

40o0F0

8,

----

Phenolic-Alkyd Coating

Laboratory number

11021

N , R , P .

57

Phenolic resin solution

:Re sinox P-97

Alkyd resin solution

:Rezyl

387-5

Solvent

:

n-But

an01

:

Xylene

Parts by weight

(27)

C o l d S e t t i n g E p o q C o a t i n g L a b o r a t o r y number 1 1 0 2 2

r

58

P a r t

A

Zpoxy r e s - i n : i p o n 1 0 0 1 U r e a - f o r l n a l d e h y d e r c s i . n s o l u t i o n : B e e t l e 216-8 S o l v e n t : M e t h y l i s o b u t y l k e t o n e : B u t y l c e l l o s o l v e : T o l u e n e P a r t

E

E t h y l e n e di.amine W a t e r I n s t r u c t i o n s f o r Use: I m e d i a t e l g p r 5 o r t o u s e , 1 3 0 g ; r z ; : s of Pa1.t L.

werl-;

7 , - t h o r o u g h l y m i x e d with 1 5 0 0 g r a m s o f P a r t A.. ; h i s i s a c a t a l y s e d a i r - d r y i n g f'ornnllati.on. V i n y l i d e n e C h l o r i d e

-

l i c r y l o n i t r i - l e Copolymer --- Coati:np; L a b o r a t o r y number 1 1 0 2 3 TJ,H,P, 59 P a r t s

1~-

rdei.;ht V i n y l i d e n e c h l o r i d e - ' a c r y l o n i t r i l e c o p o l y m e r : S a r a n F-120, 1 0 0 0 c p s 1 5 . 0 S o l v e n t : M e t h y l e t h y l k e t o n e

2,s

0 T h i s i s a n a i r - d r y i n g f o r m u l a t i o n , 11,

-

Phenolic-3i;poxy-Polyvinyl .--- B u t y r a l C o a t i n g L a b o r a t o r y number 1 1 0 2 4 N , R , P , 60 P h e n o l i c r e s i n

:R-108

20,O

Lpoxy r e s i n s o l u t i o n

:SO$

s o l u t i o n o f Epon 1 0 0 7 i n a m i x e d s o l v e n t o f 5 0 p a r t s o f x y l e n e t o 5 0 p a r t s o f d i a c e t o n e

(28)

11. ( c o i i t i n u e d ) P h e n o l i c - E p o x y - P o l y v i n y l B u t y r a l C o a t i n 8 L a b o r a t o r y number 1 1 0 2 4

man,?.

60 -- P a r t s ... .-

by

weic;ht P o l y v i n y l b u t y r a l r e s i n s o l u t i o n

:lo<$

s o l u t i o n o f B u t v a r S o l v e n t C a t a l y s t

B-76

i n

a mixed s o l v e n t o f 50 p a r t s o f x y l e n e t o 50 > a r t s o f d i a c e t o n e a l c o h o l 12,O : M a c e t o n e a l c o h o l 20,O : Xylene 20.0 :

85,,:

P h o s p h o r i c a c i d 0 , 2 Baking s c h e d u l e :

15

m i n u t e s a t ~ O O ~ F , 1 2 , P h e n o l i c - P o l y v i n y l B u t y r a l C o a t i n g L a b o r a t o r y number 11025 W.H.P. 6 4 P a r t s by w e i g h t P h e n o l i c r e s i n :H-108 P o l y v i n y l b u t y r a l r e s i n s o l u t i o n : 1 0

,;

s o l ~ l t l o n of B u t v a r

F-76

i n s e c - b u t a n o l S o l v e n t : s e c - S u t a n o l : L i a c e t o n e a l c o h o l C a t a l y s t :

35,;

P h o s p h o r i c a c i d Baking s c h e d u l e : 4.0 m i n u t e s a t

3 3 0 ~ ~ ~

Phenolic-Lpoxy-Polyvinyl

B u t y r a l C o a t i n q L a b o r a t o r y number 11026 N.H.P.

65

P h e n o l i c r e s i n :R-108 P a r t s by w e i g h t Epoxy r e s i n s o l u t i o n :50jl s o l u t i o n o f Epon 1007 i n a mixed s o l v e n t o f 50 p a p t s x y l e n e t o 5 0 p a r t s o f d i a c e t o n e a l c o h o l

31.3

P o l y v i n y l b u t y r a l r e s i n s o l u t i o n

:lo$

s o l u t i o n o f B u t v a r B-76 i n a mixed s o l v e n t o f 50 p a r t s o f x y l e n e

t o

50 p a r t s o f d i a c e t o n e a l c o h o l . 24,0

(29)

13

(continued) Phenolic--Epoxy-Polyvinyl

Butyral Coat

i n s

Solvent

Catalyst

:Liacetone alcohol

1 6 * ' j '

:Xylene

l b $ 7

:85;:

Phosphoric acid

0:

1.6

Baking schedule:

15

minutes at 400'~.

Phenolic-Alkyd Coating

Laboratory number 11027

N.R.P.

66

Phenolic resin solu-tion

:Re

sinox P-97

~llkyd

resin soliltion

:Rezyl

387-5

Solvent

:

n-But

ano

1

:

Xylene

Baking schedule:

30

minutes at

350'~.

Vinyl-Urea-Formaldehyde Coatinq

Laboratory n-~niber

11020

x , t i , p .

67

Parts

by

IAJ~~S-.~?~

Parts

hg

weight

Vinyl chloride-vinyl

acetate copclymer

:V.R.G.H.

Urea-formaldehyde resin

solution

:Uformite I"-240

Stabilizer

:

A-5

Solvent

:Methyl isobutyl ketone

Baking schedule:

20 minutes at 320°1?,

16,

Epoxy-Urea-Formaldehyde Coatinq

Laboratory number 11029

N.R.P,

69

Parts

by weight

Epoxy resin

:Epon 1007

21,O

Urea-formaldehyde resin

solution

:Beckamhe

P-138

9=0

Solvent

:Methyl isobutyl carbinol

17e5

:Methyl isobutyl ketone

17.5

:

Toluene

1Tj5

:Xylene

17.5

(30)

Phenolic-Epow-Vinyl C o a t i s

Laboratory number 11031

N,H,P,

76

- - . -

Parts

.)-\- -Lli---

ljsic;l~t

Phenolic resin solution

:Bakelite

10673

' '7

- < :-

:Epon 1004

Epoxy resin

./ n b

Polyvinyl butyral resin

:X.Y.H.L.

5

7

Chlorinated biphenyl

:

Aroclor

1254

Solvent

:Methyl isobutyl ketone

3 7 , 3

Baking schedule:

20

minutes at 325'F.

18,

Phenolic-Vinyl C o a t i q

Laboratory number 10032

N,R,P,

77

--

Parts

&

if:2i,;!it

Phenolic resin solution

:Bakelite

10673

Lk? a

3

Polyvinyl butyral resin

:

XeY*13*La

5+2

Solvent

:liethy1 ethyl ketone

l s J O

:n-Butanol

d ~ O , O

asking

schedule:

20

minutes at 325'F.

Vinylidene Chloride

-

Acrylonitrile Copolylner Coatin$

Laboratory number

11033

N.R.P.

89

Parts

by.

weight

Vinylidene chloride-

acrylcnitrile copolymer ;Saran F-120,200 cps

1 s O O

Solvent

:Methyl ethyl ketone

8 s O O

This is an air-drying formulation,

Phenolic

-Epoxy Coatinq

Laboratory number

11035

N.R.P,

132

--

Parts

by

weight

Phenolic resin solution

:Resinox P-97

12,O

Epoxy resin solution

:50$

solution of Lpon

1001

i n a mixed

Solvent

solvent of SO parts

of xylene to

50

parts

diacetone alcohol

ZR,O

:Methyl ethyl ketone

/ O J 2 L'

(31)

Laboratory number 11036

N.R.P.

133

Phenolic resin solution

: H e

sinox P-97

-

Epoxy resin solution

:SO):

solution of Epon

1001

in

a

mixed

solvent of

-50 pa-ts

of xylene to

50

parts

diacetone alcollol

Solvent

:Methyl ethyl ketone

Baking schedule:

30

minutes at

350°F.

Laboratory number

11037

N.H.P,

135

Parts by ;,reight

Phenoli? resin solution

:Resinox P-97

50,O

Epoxy resin aolution

~50;:

solution of Epon

1001 i n a mixed

solvent of 50 parts

of xylene to

50

parts

of diacetone zlcohol

50,O

Baking schedule:

30

minutes at

350'~.

Phenolic-Bpoxy Coatin8

Laboratory n'mber

11038

N.R.P.

136

Phenolic resin solution

:Resinox P-97

Epoxy resin solution

:50$ solution of

Epon

Parts

by

wei;;ht

1001 in

a mixed-

solvent of

50

>arts

of xglene to

50

parts

of diacetone alcohol

300.0

Baking schedule:

30

minutes at

350'~.

24-

Phenolic-Polyvinyl Butyral Coating

Laboratory number 11039

N.H.P.

137

Phenolic resin solution

:Resinox P-97

Parts

by

weight

21,o

(32)

24. ( c o n t i n u e d ) P h e n o l i c - P o l y v i n y l E u t y r a l

--

Coat* P o l y v i n y l b u t y r a l r e s i n s o i u t i o n

:lo;:

s o l u t i o n o f P a r t s

-

L y wc:l&l P. Butval*

L.-76

i n n - b u t a n 0 1 !j,Y4O P h e n o l i c - P o l y v i n y l G u t y r a l Coat* L a b o r a t o r y number 11040

iJ.Fi.P. 1 3 8

-..F

Pnr ?-.--A by/-

---

mi& P h e n o l i c r e s i n s o l u t i o n : R e s i n ~ ~

P-97

24 " 0 P o l y v i n y l b u t y r e l r e s f n s o l u t i o n :lo$ s o l u t i o n o f Gutvar

E-76

i n n-but a n 0 1

t10,

0 Baking s c h e d u l e : 20 m i n u t e s a t 3 5 0 ' ~ . 26, P h e n o i i c - P o l y v i n y l

-

B u t y r a l C o a t i n g L a b o r a t o r y number 1104.1 N.R.P.

139

P h e n o l i c r e s i n s o l ~ t i o n :Hesinox P--97 P o l y v i n y l b u t y r a l r e s i n s o l u t i o n

:lo:;

s o l u t i o n o f B u t v a r

B-76 in

n-But a n 0 1 Baking s c h e d u l e : 20 m i n u t e s a t 350°i?, V i r m y l c h l ~ r i d e - , V i n y l A c e t a t e Copolymer C o a t i s

---

L a b o r a t o r y number 11042 N.R.P.

141

---. P a r t s by weigh2 V i n y l c h l o r i d e - v i n y l a c e t a t e copolymer :V.A.G,H, 3 6 , O S o l v e n t :Methyl e t h y l k e t o n e 79,O T h i s i s a n a i r - d r y i n g f o r m u l a t i o n .

(33)

V i n y l C o a t i n g Lator.at o r g number

ll0!{4

T~'l.il.F. 1 L l

=,

Viny 1 . c h l o r i i i e - v i n y l a c e t a t e copolyrner :V.Y.E.F. Yodif i e d v i n y l c h l o r i d e - v i n y l a c e t a t e copolymer :V.M.C.H. S o l v e n t : I l e t h y l e t h y l &retone P a r t s .-. 'by --.--- il:ei&_t, T h i s i s an 2 i r - d r y i l l g formflulation.

29

V i n y l Chlor>ide-Vinyl .-- A c e t z t e Copoly-mer

-

-.-.

coati^^

P a r t s

-

by

---- wei& V i n j r l c h l o r i d e - v i n y l a c e t s t e copolymer

:V.A.G.H.

7 @ 0 P l a s t i c i z e r : F l e x 0 1

H-2H

S e O

S o l v e n t :Methyl e t l i y l k e t o n e 10,O T h i s i s a n a i r - d r y i n g f o r m u l a t i o n . V i n y l C h l o r i d e - V i n y l A c e t a t e Copolymer -C o a t i n 9 - a L a b o r a t o r y number

1101~6

N.R.P.

151

--

P a r t s by w e i g h t V i n y l c h l o r i d e - v i n y l a c e t a t e co3olymer :V.A.G.H.

2L,Q

P l a s t i c i z e r : B a k e r ? s

#16

P a l e Blown C a s t o r O i l g o G S o l v e n t :Methyl e t h y l k e t o n e 70.C

310

V i n y l C h l o r i d e - y i n y l A c e t a t e Copolymer .-. Coatti!il; L a b o r a t o r y numbcr 1104.7 1S.E.P. 1 5 6 V i n y l c h l o r i d e - v i n y l

a c e t a t e copolymer :V.A.

G.H.

2rjOC;

P l a s t i c i z e r :Baker 1 s 7716 P a l e Blown

C a s t o r O i l

36c

S o l v e n t :Methyl e t h y l k e t o n e 7 0 0 0 T h i s i s an a i r - d r y i n g f o r m u l a t i o n

(34)

P a r t s -.-..- V i n y l c h l o r i d c - v i n y l a c e t a t e c o p o l y m e r n l

..

:v.L'L.:3.?:. L L . ,"I P l a s t i c i z e r : L ~ , . k e r f s $16 P a l e B l o ~ r n , - C a s t o r , O i l t-J , 0 s o l v e n t ; M e t h y l e t h y l k e t o n e * 7 c e C T h i s i s a n a i r - d r a y i n g f o r m u l a t i o n , V i r ~ y l C h l o r > i d e - V i q l

--

A c e t a t e

-

Copolymer Contfrsg

--

-- L a b o r a t o r y number 1101.+9

?.r.n.?.

158

V i n y l c h l o r i d e - v i n y l a c e t a t e copolynlcr :V.A.G.II. 27 P l a z t i c i z e r : P a r a p l e x G-25

9 - 0

S o l v e n t :?'lethyl e t h y l l r c t c n e 7 O O O T h i s i s a n a i r - d r y i n g f o r m u l a . t i o n . C , C o m p o s i t i o n o f P r i m e r Wash P r i m e r L a b o r a t o r y n m b e r 1 1 1 3 0 la.x,F. 1 2 -- P a r t s by

~ s T q h t

-

P a r t A P o l y v i n y l b u t y r a l r e s i n :X.Y.H.L.

~ i ,

e Z i n c c h r o m a t e , b a s i c t y p e : I m p e r i a l X-2259

5b1

g

Magnesium S i l i c a t e :fishes-tine

3 X

S o l v e n t : n - B u t y l a l c o h o l 1 2 5 L1 : Z t h y l a l c o h o l ,

95';;

3 5 0 . ~

The a b o v e i n g r e d i e n t s w e r e d i s p e r s e d i n a p e b b l e m i l l . f o r a b a u t

48

h o u r s . The f i n e n e s s o f g r i n d was 6 u n i t s a s ,neasu- re^ oc t h e N o r t h S t a n d a r d Gauge, P a r t I3 P h o s p h o r i c a c i d ,

85%

wat eE E t h y l a l c o h o l , 9 9 ; B w i t h good s t i r r i n g f P a r t A was m i x e T h i s m i x t u r e was d w i t h o n e p a r t o f P a r t u s e d w i t h i n

8

h o u r s ,

Figure

TABLE  V I   c o n t i n u e d   Lalr,oratory  Days  l\T  urib  e  r  P a n e l   Lxpo  s e d   --  -  --  1 1 0 3 5   A  25  25;:  o f   p a n e l   c o v e r e d   i n   ~ &gt; ? n i t ~   : ~ p o t s   (3/16&#34;  diarn,  )  t h a t   a r e   r 1 i ~ s

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