DISCLAIMER. -21CmRaCTERISTICS OF H.E. & H.E.

Transcription

1 21CmRaCTERSTCS OF HE & HE SYSTEMS This p r o j e c t c o n s i s t s of t h e e s t a b l i s h m e n t of methods t o c h a r a c t e r i z e h i g h e x p l o s i v e s w i t h p a r t i c u l a r emphasis d i r e c t e d toward p r e d i c t i n g t h e q u a l i t y and performance of t h e raw powder and t h e r e s p o n s e of HE l o t s t o v a r i o u s c o n d i t i o n s of p r e s s u r e, t e m p e r a t u r e, f a b r i c a t i o n t e c h n i q u e s, e t c XE p a r t i c l e p a r a m e t e r s ( s i z e, shape and a r e a ) a r e c u r r e n t l y of major i n t e r e s t DSCLAMER This report was prepared as an account of work sponsored by an agency of the United States Government Neither the United States Government nor any agency thereof, nor any of their employees, makes any warranty, express or implied, or assumes any legal liability or responsibility for the accuracy, completeness, or usefulness of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights Reference herein to any specific commercial product, process, or service by trade name, trademark, manufacturer, or otherwise does not necessarily constitute or imply its endorsement, recommendation, or favoring by the United States Government or any agency thereof The Views and opinions of authors expressed herein do not necessarily state or reflect those of the United States Government or any agency thereof H B C a r r o l l, J r Q u a r t e r l y Report f o r O c t o b e r, November, December, 1964 E n g i n e e r i n g Order No _

2 DECLAMER

3 22 ABSTRACT S e v e r a l samples of HNX t o be used i n LX041 were p a r t i c l e s i z e d and r e p o r t e d i n t h i s report Most of t h e l o t s s i z e d were v e r y s i m i l a r, w i t h t h e major d i f f e r e n c e s i n t h e l o t s b e i n g a t 2p S e v e r a l c o u n t s i n "Rainbow" Lot 26B of LX041, made t o o b t a i n a c o l o r and weight d i s t r i b u t i o n i n s e v e r a l samples, and a l s o a c o l o r count made i n each s i e v e on a g r a n u l a t i o n a n a l y s i s, show e a c h c o l o r t o b e e q u a l l y d i s t r i b u t e d ; i e, m n e t h i r d of e a c h c o l o r, g r e e n, yellaw and w h i t e LX041 g r a n u l e s, was p r e s e n t i n t h e sample Photographs and p a r t i c l e s i z e c u r v e s of r e c r y s t a l l i z e d PETN used i n LX021 a r e presented These d a t a were o b t a i n e d by examining t h e o r i g i n a ' l PETN used i n a l o t of LX021, t h e n performing s e v e r a l m i l l h g o p e r a t i o n s and r e c o v e r i n g :he PET3 from t h e 3 F n d e r f c r a n o t h e r exs5nation i n e z z j c r L t y of t h e PZTX z a p e a r s : c m be crushed o r broken i n t h e f i r s t s i x p a s s e s o n t h e t h r e e r o l l m i l l with s r c a l l e r changes taking place i n the tworoll n i l l concentrated i9 the 4 t o 8p r e g i o n The f i n a l li shows most of t h e PETN t o be Photographs of two p r o d u c t i o n l o t s of LY021 subjected t o a milling operation a r e a l s o included A d e s c r i p t i o n of t h e procedure used t o r e c o v e r t h e PETN from t h e LX021 b i n d e r is included are listed S e v e r a l s o l v e n t s f o r t h e LX021 b i n d e r and f o r d i f f e r e n t HE's These were examined i n a n e f f o r t t o f i n d a new e l u t a n t t o use w i t h LX041 The e f f e c t s of d i f f e r e n t m i l l i n g t i m e s on t h e b i n d e r have been examined by checking t h e s o l u b i l i t i e s i n s e v e r a l of t h e s o l v e n t s r

4 23 n i t i a l s t u d i e s on t h e i n f r a r e d s p e c t r a of HE's i n t h e wave length r e g i o n show p r o m i s e f o r d e t e r m i n a t i o n of,pdx c o n t e n t i n HEX, and f o r d e t e r m i n a t i o n of t h e polymorphs of W S p e c t r a a r e i n c l u d e d i n t h i s r e p o r t on t h e v a r i o u s polymorphs of HXX a l o n g w i t h s p e c t r a o f PETN and RDX PREVOUS APPLCABLE WORK The wide p a r t i c l e s i z e r a n g e of p a r t i c u l a t e e x p l o s i v e material made i t n e c e s s a r y t o d e v e l o p a t e c h n i q u e t o d e t e r m i n e t h e s i z e of t h i s m a t e r i a l from 350 t o 111 The t e c h n i q u e developed u s e d s t a n d a r d wirewoven sieves (350 Xears e l e c t r o f o r m e d sieves (40 lp), 44p) and Buckbee and i s d e s c r i b e d f u l l y i n p r e v i o u s r e p o r t s ' Coxparison w i t h p h o t o s e d i m e n t a t i o n showed t h e method t o b e a d e q u a t e, and r e p r o d u c i b i l i t y was a l s o v e r y good Lottolot v a r i a t i o n s i n the T of the r e c o v e r e d from PBX 9401; and LX041 have been measured u s i n g t h e a f o r e n e c c i o n e d s i e v i n g t e c h n i q u e These v a r i a t i o n s i n LY021 have b e e n c o r r e l a t e d t o d e n s i t y i n a p r e v i o u s r e p o r t 2 tl"x's p r e p a r e d by o t h e r methods s u c h a s B r i d g w a t e r, H o l s t o n, and H o l s t o n s i m u l a t e d B r i d g w a t e r p r o c e s s have been s i e v e d '2nd & 3 r d Q u a r t e r l y P r o g r e s s R e p o r t s f o r r d Q u a r t e r l y P r o g r e s s Repprt f o r

5 , 24The predominant f e a t u r e of t h e Bridgwatertype HXX was i t s v e r y l a r g e s i z e ; most M was above 109;~ of t h e ' B n y l o t s o f HXf used i n LX041 and s e v e r a l l o t s of FETN may b e found i n p r e v i o u s r e p o r t s The PerkinElmer s o r p t o m e t e r s u r f a c e a r e a measurements appeared t o be i n e r r o r due to e x t r a n e o u s peaks a p p e a r i n g b e f o r e d e s o r p t i o n peaks 3 These e x t r a n e o u s * peaks were removed by i n s e r t i n g a c o i l e d 3fOOt l e n g t h of 1/16inch copper t u b i n g between t h e sample a n d t h e d e t e c t o r, n e r t samples o f p a r t i c u l a t e m a t e r i a l were o b t a i n e d from Numeco C o r p o r a t i o n t o u s e a s " s t a n d a r d samples" f o r t h e P e r k i n Elmer sorptometer The s u r f a c e a r e a of t h e s e samples had been determined by t h e c o n v e n t i o n a l pressurevolume BET t e c h n i q u e A d d i t i o n a l work on t h e e f f e c t s of u l t r a s o n i c v i b r a t i o n on HXX h a s been r e p o r t e d E s s e n t i a l l y, t h i s s t u d y i n d i c a t e d a t i m e of t h r e e t o f i v e mtnutes was a d e q u a t e t o d i s p e r s e t h e a g g i o n e r a t e s, depending u?cn t h e d e g r e e o f a g g l o m e r a t i o n i n t h e i o i DSCUSSCN c S e v e r a l n ' s of XMX u s e d i n LX041 have been o b t a i n e d by c o n t i n u e d m o n i t o r i n g of all l o t s of e x p l o s i v e s r e c e i v e d a t Pantex The n ' s on t h e s e m a t e r i a l s a r e shown i n t h l s r e p o r t p l o t t e d two ways; a Line graph on semilog paper (graph A) and by h t s t o g r a m on a r i t h m e t i c p a p e r ( g r a p h B), was u s e d w i t h e a c h l o t The s t a n d a r d procedure f o r s i e v i n g HXX A l l l o t s a r e now done by t h e Chemical Laboratory a s a r e g u l a r p r o c e d u r e, a n d w i l l n o t h e r e a f t e r b e r e p o r t e d h e r e i n except a s t h e y may b e of s p e c i a l i n t e r e s t A book of t h e 's h a s been s t a r t e d, t o c o n t a i n a l l t h e f u t u r e n's 1st Q u a r t e r l y P r o g r e s s Report f o r 1964

6 ,,l *, ' F i g u r e s 1A t h r o u g h 3A r e p r e s e n t t h e of L o t s 26A, 27A, and 28A f r o m t h e i n p u t Em P r e s s i n g, d e n s i t y, and s t r e n g t h d a t a a r e i n T a b l e simila r l y The l o t s p r e s s e d The J ' s shown i n F i g u r e s 4 A through 8A were obcained f r o n WX i n p u t samples t o Lots 37A64, 38A64, 39A64, 40A64, and 41A64, These HMX l o t s, i n g e n e r a l, were v e r y s i m i l a r and somewhat c o a r s e r ( l e s s t o t a l m a t e r i a l 2 6, 2 7, and 28 <lop, on'the a v e r a g e ) than T h e ' l o t s p r e s s e d s i m i l a r l y, e x c e p t f o r 39, A s may be s e e n i n Table, and a l l had good d e n s i t y P a r t i c l e s i z e d i s t r i b u t i o n s w e r e r u n on s e v e r a l samples of HMX from Lot t h a t had been m i l l e d f o r d i f f e r e n r : t i m e s The 2 ' s on t h i s m a t e r i a l showed t h e T k s e d a r a s a y be s z z n in t h e F o r x i l a t i o n S e c t i o n of t h i s r e p o r t n v e s r i g a r i o n s on t h e "Bainbow" Lot 2613, a s f a r a s g r a n u l a t i o n s and c o l o r d i s t r i b u t i o n s a r e concerned, have been completed Three 100gram samples w e r e chosen a t d i f f e r e n t p o s i t i o n s and d e p t h s from e a c h of t h e t h r e e boxes of powder t o g e t g r a n u l a t i o n and c o l o r d i s t r i b u t i o n d a t a Each 100gram samples was s p l i t i n t o a 10gram and two 25gram samples, a n d a c o l o r count was made on e a c h The number of d i f f e r e n t c o l o r e d g r a n u l e s, i n a d d i t i o n t o t h e w e i g h t of e a c h f r a F t i o n, was t a k e n and used t o c a l c u l a t e t h e weight and c o l o r d i s t r i b u t i o n shown i n Table 11 The weight and c o l o r d i s t r i b u t i o n shown i n Table 1 i n d i c a t e t h e g r e e n, yellow, and w h i t e f r a c t i o n s t o be a p p r o x i m a t e l y e q u a l l y d i s t r i b u t e d, t h a t i s, t h e sample c o n t a i n e d a b o u t o n e t h i r d of each f r a c t i o n

7 , 1' 1 J L ; 1 j!

8 27 0 io ' 'A)

9 J Weight X n 1n:erv O S i e v e S i z e (p)l ti0 1

10 1 ;, 29 4 ;$eight % i n nterval _ E

11 WeLght Z n nter _*_ +* $! *! _ L SO +>0 j /U 80 OC Sieve Size ( p ) l LO !;0 35

12 31

13 * t LOO Sieve Size (p) d l L j C 9 >

14

15 Table Weight & Color Distribution on Lot 26B Sample No Weight Tota 1 Green Yellow wh Distribution% Distribution% DisG Number Weight Number Weight Number :e jution% Weight ~

16 ? 37The samples were t h e n recombined i n t o e a c h o r i g i n a l 100gram sample f o r g r a n u l a t i o n The g r a n u l a t i o n a n a l y s i s was performed i n t h e s t a n d a r d way, p l a c i n g t h e analysis s i e v e s t a c k c m t a i n i n g t h e sample i n t h e RoTap s h a k e r f o r f i v e minutes and weighing t h e m a t e r i a l r e c e i v e d i n each s i e v e s i e v e s w e r e made i n two ways: Color c o u n t s on t h e m a t e r i a l c o n t a i n e d i n t h e (1) a l l p a r t i c l e s w e r e counted i n s i e v e s c o n t a i n i n g o n l y a s m a l l number of p a r t i c l e s, and ( 2 ) s i e v e s c o n t a i n i n g l a r g e number of p a r t i c l e s w e r e a g i t a t e d t o smooth t h e m a t e r i a l o u t, t h e n F+: o n e f o u r t h of t h e m a t e r i a l was counted The g r a n u l a t i o n a n a l y s i s shows t h e samples t o be c o n c e n t r a t e d i n t h e number 6, 8, 1 2, 1 6 and 20 s i e v e s 7 The c o u n t s t a b u l a t e d i n T a b l e 111 i n d i c a t e t h e same a s b e f o r e ; t h e m a t e r i a l i s approximately e q u a l l y d i s t r i b u t e d (% o n e t h i r d of each color) P a r t i c l e s i z e a n a l y s i s from t h r e e of t h e samples a r e shown i n F i g u r e 9, PETN from Lot was used t o make a s m a l l l o t of LX021 The of t h e PETN a f t e r r e c r y s t a l l i z a t i o n and b e f o r e i n c o r p o r a t i o n i n t o LX021 i s shown i n F i g u r e 10, Most o f t h e m a t e r i a l a p p e a r s i n t h e 10 t o 40p r e g i o n w i t h a small peak a t 6 ~ 1,and photographs of t h i s m a t e r i a l shown i n F i g u r e s 11 and 1 2 i n d i c a t e a prominent " s n o w f l a k e l i k e " c r y s t a l h a b i t with a v a r i e t y of o t h e r s h a p e s, Number d i s t r i b u t i o n s on t h e "snowflake" and o t h e r c r y s t a l h a b i t s a r e l i s t e d i n the 3 r d Q u a r t e r l y Report f o r 1964 The p r e p a r a t i o n and t r e a t m e n t of t h e LX021 (Lot No ) made from t h i s m a t e r i a l a r e d e s c r i b e d f u l l y i n t h e F o r m u l a t i o n Report B r i e f l y, t h e t r e a t m e n t was t o d i v i d e t h e m a t e r i a l i n t o t h r e e samples,

17 39The f o l l o w i n g p r o c e d u r e was used t o remove t h e b i n d e r from t h e LX021; then t h e s t a n d a r d s i e v i n g t e c h n i q u e was used f o r s i e v i n g A 10gram sample of LX021 was p l a c e d i n a 250 m l f l a s k w i t h a p p r o x i m a t e l y 150 ml of carbon t e t r a c h l o r i d e 18 h o u r s ( o v e r n i g h t ) G e n t l e The m i x t u r e was allowed t o s o a k f o r s h a k i n g on t h e w r i s t a c t i o n s h a k e r was a p p l i e d f o r w 10 minutes a t the start (3) Most of t h e carbon t e t r a c h l o r i d e and d i s s o l v e d b i n d e r was drawn o f f with a pipette (4) The m a t e r i a l was washed w i t h x 100 m l of carbon t e t r a c h l o r i d e and poured i n t o t h e s i e v e s The i n i t i a l m a t e r i a l and e l u t a n t p a s s i n g t h e l a s t sieve c a u g h t and t h e <lop PETN c e n t r i f u g e d o u t (lop) was The s i e v e s were washed w i t h Freon TF s a t u r a t e d w i t h PETN and t h e s t a n d a r d s i e v i n g t e c h n i q u e c a r r i e d o u t from t h a t p o i n t Photographs o f t h e PETN e x t r a c t e d from t h e A, B, and C LX021 samples a r e shown i n F i g u r e s 13 t h r o u g h 18 The p a r t i c l e s a p p e a r i n t h e photographs a s i r r e g u l a r f r a g m e n t s and t h e "snowflakelike" p a r t i c l e s a r e not present F i g u r e s 23 t h r o u g h 3 4 show PETN r e c o v e r e d from two l o t s of LX021 used by p r o d u c t i o n This c r y s t a l l i n e m a t e r i a l a p p e a r s, i n g e n e r a l, t o be more r e g u l a r throughout t h e m i l l i n g o p e r a t i o n t h a n t h e r e c r y s t a l l i z e d PETN

18 PETN Recovered From L o t x OL PETN,ot 43C, vyr) Six P a s s e s i n T h r e e R o l l M i l l ; TwoRoll Mill [ S i x P a s s e s i n T h r e e R o l l Mill: TwoRoll M i l l With 10 Y i l l Gap F o r T h r e e Ylinutes r'igure?etn From L o t Soaked i n PETN PETN From Lot Soak S a t u r a t e d F r e o n TF F o r 60 Hours 20 x C V L L V L A e Soaked i n PETN Freon MF F o r 20 Hours 20 x OE' 1

19 R e c ry s t a 11 i zed P ETN Lot T T s ~ r l in T n t h? of LX X OBJ p [Recrystallized PETN Lot $3 Used i n Lot of LX x ORT$

20

21 1 PETN From TX021, L o t A335, > O XO B J M i l l e d 3 M i n, Gap, R o l l S p e e d 1 5 / 2 0 PETN From Lx021, Lot A335, 2 0 x OB3 '1 PETN From LS021, Lot A335, 40 x O B J M i l l e d 5 $ f i n, G a p, R o l l S p e e d 15/20 1

22 1B LC W t % Color wt % C o l o r Ret D i s t Ret D i s t Sieve No 4 G 5 Y W 6~ 8~ G W G W G Y W G Y W G Y W G 25 Y i<40 ^ W G Y W G Y W 2c 3A Color W t % Color W t % Color Dist R e t, Dist Ret Dist i 351 i , , t ~ t 4 26 t _ t 208 t ~ 20 t 224 t F97!126i 3ti9 LleL, 3L l i7 3;' 1 3' L _yl_ L _ ; 8 3:' 1 J 3! b ,3 ;;q 135:5, L_ \04?;:: ) , , ' ) ,5 506 " 'L ~ 3L ' " 7, " L7 305 Color Dist _ 1' ! ! ! ,2 33,l d 7 3 ~ _ G = G r e e n, Y = Yellow, W = W h i t e (Each percent:a):,(' i:; i 1/11 i v c to the number of p a r t i c l e s count:c$d ill Lhat s i e v e,?too sma1l a number sample f o r a v a l i d number c i i ~ s lib(t! t O!+ $ P a r t i c l e s s o s m a l l a n d dust:lilte, a count w a s n o c a i i,,:r~;)~~>d6 4L c

23 45 Table V S o l u b i l i t y Data S o l v e n t s Amb ien t Temp e r a t u re L 0 L i g r o i n e Octant MChloroPChlorobenzobenzoBenz ododecanc t r i f l u o r i d e t r i f l u o r i d e t r i f l u o r i d e , B u t y l Rubber Citroflex A :s 3,957 3,913 1, ,192 4, , B u t y l Rubber Citroflex A, 6 p a s s e s, no 90" turns B u t y l Rubber + C i t r o f l e x A, 25 p a s s e s, no 90" turns Viton ~ ~~~ Citroflex A, rolled 25 p a s s e s on 3roil m i i i, 90" t u r n s a t t emp t e d Butyl Rubber Citroflex A, 6 p a s s e s on 3roll mill, 90" t u r n s attempted Butyl Rubber t , 'L 3, e e e 005 i ~ * 993 3, e 040, , 028 0, ,731 e 024

24 46nfrared Studies H B C a r r o l l, J r & W T Q u i n l i n n i t i a l i n v e s t i g a t i o n have been made of t h e i n f r a r e d s p e c t r a of s e v e r a l e x p l o s i v e s i n t h e 15 40p wave l e n g t h r e g i o n A PerkinElmer Model 2 1 s p e c t r o p h o t o m e t e r w i t h a C s B r p r i s m was u s e d t o o b t a i n t h e s p e c t r a shown i n F i g u r e s 3 5 t h r o u g h 39 The s p e c t r a of t h e s e e x p l o s i v e s show s e v e r a l s t r o n g a b s o r p t i o n bands p r e s e n t i n t h i s r e g i o n which may b e u s e f u l f o r a n a l y s i s of RDX i n HMX o r v i c e v e r s a The r e g i o n from 30p t o t h e l i m i t of t h e p r i s m (Z 4 0 ~ )i s n o t a s w e l l d e f i n e d i n t h e f i g u r e s shown a s t h e y c a n b e, The r e a s o n was K p e l l e t s were u s e d a s a sample medium and t h e s p e c t r o p h o t o m e t e r was n o t n i t r o g e n purged F i g u r e s 38 and 39 a r e i n i t i a l s p e c t r a of polymorphs of HNX show marked changes i n t k e a b s o r p t i o r, p e a k s, t h e s p e c t r a o f t h e These s p e c t r a 9 p ~ l y x o r p 5h a s n o t

25 T p +, % i 1 j j i C c T U n

26 0 N 17 i i j

27 L ' _ } ~

28

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30 52FUTURE WORK; COMMENTS; CONCLUSONS Montoring t h e of a l l l o t s of e x p l o s i v e s r e c e i v e d a t P a n t e x w i l l be c o n t i n u e d, a l o n g w i t h r e l a t i o n s h i p s t o d e n s i t y and s t r e n g t h s The HMX l's, now measured by t h e Chemical L a b o r a t o r y r e g u l a r l y, w i l l no l o n g e r be r e p o r t e d h e r e u n l e s s t h e y a r e of s p e c i a l interest A book of t h e 's i s a v a i l a b l e i n t h i s report The ll, d e n s i t y, and p r e s s i n g d a t a c o n t a i n e d, coupled w i t h t h e s t a t i s t i c a l a n a l y s i s 4 r e p o r t e d p r e v i o u s l y have indicated t h a t deviations i n the l f o r LX041 may make a s i g n i f i c a n t change i n t h e p r e s s i n g d e n s i t y f o r t h e m a t e r i a l, and perhaps i n t h e s t r e n g t h The c o l o r d i s t r i b u t i o n s, by weight and number, have i n d i c a t e d t h e "Rainbow" Lot 26B t o have equal p o r t i o n s of t h e c o l o r s p r e s e n t, G r a n u l a t i o n and p a r t i c l e s i z e a n a l y s i s also show t h e m a t e r i a l t o be uniform w i t h r e s p e c t t o t h e s e v a r i a b l e s? S t u d i e s w L l l b e c o n t i n u e d on t h e LX021 m t e r i a l S;r e x a a i z a t i s n o r c n e r e c r y s t a l l i z e d PETN, m i l l i n g t r e a t m e n t and b i n d e r t?e One i n t e r e s t i n g p o i n c a r i s e s w i t h r e s p e c t t o t h e subsequent m i l l i n g t r e a t m e n t a f t e r t h e t h r e e r o l l m i l l, and t h a t i s, w h e t h e r o r n o t t h a t t r e a t m e n t changes t h e b i n d e r, because t h e seems t o be moderate and i n what one f e e l s i s t h e wrong d i r e c t i o n f o r t h e observed improvement i n e x t r u d a b i l i t y The s o l u b i l i t i e s of t h e b i n d e r w i t h d i f f e r e n t m i l l i n g t r e a t ments change somewhat, a l t h o u g h t h i s may n o t be s u f f i c i e n t e v i d e n c e of a l a r g e change i n t h e binder The i n i t i a l i n f r a r e d a n a l y s i s i n t h e p r e g i o n h a s i n d i c a t e d seemingly u s e f u l a b s o r p t i o n peaks on which q u a n i t a t i v e a n a l y s i s work might be b a s e d 3 r d Q u a r t e r l y Report f o r 1964, CsBr pellets

31 53 and a nitrogen purge systemwill be used during this next quarter to obtain better spectra tion band Also, work will begin upon assignment of bond vibrations to each absorp A meand forquantitative analysis of impurity contents i n different explosives will also be examined