ttchnkaluwarv technical 5 0712 01016679 0 l library» - … · explosion temperature tnt petn 20....

A&-A loft 15"*

TECHNICAL L LIBRARY»

TtCHNKALUWARV

5 0712 01016679 0

AD-E4O0 628

TECHNICAL REPORT ARLCD-TR-81010

U.S. (ARRADCOM) TEST RESULTS

FOR

NATO ROUND-ROBIN TEST ON HIGH EXPLOSIVES

L. AVRAMI M. S. KIRSHENBAUM

MAY 1981

US ARMY ARMAMENT RESEARCH AND DEVELOPMENT COMMAND LARGE CALIBER

WEAPON SYSTEMS LABORATORY DOVER. NEW JERSEY

APPROVED FOR PUBLIC RELEASE: DISTRIBUTION UNLIMITED.

The views, opinions, and/or findings con- tained in this report are those of the au- thors) and should not be construed as an official Department of the Army position, policy or decision, unless so designated by other documentation.

Destroy this report when no longer needed. Do not return it to the origin- ator.

UNCLASSIFIED SECURITY CLASSIFICATION OF THIS PAGE (When Data Entered)

REPORT DOCUMENTATION PAGE READ INSTRUCTIONS BEFORE COMPLETING FORM

1. REPORT NUMBER

Technical Report ARLCD-TR-81Q1Q

2. GOVT ACCESSION NO 3. RECIPIENT'S CATALOG NUMBER

4. TITLE (and Subtitle)

U.S. (ARRADCOM) TEST RESULTS FOR NATO ROUND-ROBIN TEST ON HIGH EXPLOSIVES

5. TYPE OF REPORT & PERIOD COVEREO

6. PERFORMING ORG. REPORT NUMBER

7. AUTHORC«;

L. Avrami M.S. Kirshenbaum

8. CONTRACT OR GRANT NUMBERfsj

9. PERFORMING ORGANIZATION NAME AND ADDRESS

ARRADCOM, LCWSL Energetic Materials Div (DRDAR-LCE-D) Dover, NJ 07801

10. PROGRAM ELEMENT, PROJECT, TASK AREA ft WORK UNIT NUMBERS

It. CONTROLLING OFFICE NAME AND ADDRESS

ARRADCOM, TSD STINFO Div (DRDAR-TSS) Dover, NJ 07801

12. REPORT DATE

May 1981 13. NUMBER OF PAGES

5J_ 14. MONITORING AGENCY NAME a ADDRESSfff dltletent from Controlling Otltce) IS. SECURITY CLASS, (of thla report)

Unclassified

IS«. DECLASSIFI CATION/DOWN GRADING SCHEDULE

16. DISTRIBUTION STATEMENT (of thla Report)

Approved for public release; distribution unlimited.

17. DISTRIBUTION STATEMENT (ol the abstract entered In Block 20, It dltlerent from Report)

18. SUPPLEMENTARY NOTES

19. KEY WORDS (Continue on reverae aide It neceeaary and Identity by block number)

Explosives Impact sensitivity Picatinny Arsenal impact tester ERL (NOL) impact tester

% Bruceton test

Picatinny Arsenal 10% point Tetryl Run-down test RDX Thermal sensitivity HMX Explosion temperature TNT PETN

20. ABSTRACT (Continue en reversm attta ft nexreaaary aid Identify by block number)

As part of the NATO Round-Robin Test program using explosives from one source, the US (ARRADCOM) performed a series of tests on five BICT-furnished explosives. The explosives tested were PETN, RDX, HMX, tetryl and TNT. A series of impact tests were conducted utilizing the 50% Bruceton, the Picatinny Arsenal 10% point and the full run-down test methods. Additional tests, including melting point, chemical analysis, vacuum stability test, explosion temperature, DTA/TGA, DSC, IR, NMR and particle size distribution,

DO i JSJJ'W M73 EDtTIOM OF » MOV 65 IS OBSOLETE UNCLASSIFIED SECURITY CLASSIFICATION OF THIS PAGE (When Data Entered)

UNCLASSIFIED SECURITY CLASSIFICATION OF THIS PAGEfWhan Data Entered)

20. ABSTRACT (cont)

were conducted. For impact sensitivity and thermal sensitivity, relative rankings for the explosives were determined.

UNCLASSIFIED SECURITY CLASSIFICATION OF THIS PAGEfWTien Data Entered)

CONTENTS

Introduction

Test Program

Results

Impact Sensitivity Thermal Sensitivity and Chemical Analysis Electrostatic Sensitivity Infrared Spectroscopy Nuclear Magnetic Resonance Particle Size Distribution

Conclusions

References

Appendix

Distribution List

Page

1

1

2

2 3 3 4 4 4

4

6

39

51

TABLES

Page

1 Run-down test results of NATO round-robin explosives obtained with PA impact tester 7

2 Run-down test results of NATO round robin explosives obtained with ERL (NOL) impact tester 8

3 Comparison of Bruceton 50% up-and-down and ARRADCOM 10% points with run-down test 9

4 Relative ranking of NATO round-robin explosives according to impact sensitivity tests 10

5 Characteristics of NATO high explosives 11

6 Time to explosion temperatures of NATO round-robin explosives 12

7 Thermoanalytical characterization of NATO round-robin explosives 13

8 DSC results of NATO round-robin explosives 14

9 Particle size distribution (sieve method) 14

FIGURES

Page

1 Explosion temperature curves for NATO round-robin explosives 15

2 DTA/TGA thertnogram of TNT (in air) 16

3 DTA/TGA therraogram of TNT (in nitrogen) 17

4 DTA/TGA thermogram of PETN (in air) 18

5 DTA/TGA thermogram of PETN (in nitrogen) 19

6 DTA/TGA thermogram of tetryl (in air) 20

7 DTA/TGA thermogram of tetryl (in air) (2nd run) 21

8 DTA/TGA thermogram of tetryl (in nitrogen) 22

9 DTA/TGA thermogram of HMX (in air) 23

10 DTA/TGA thermogram of HMX (in nitrogen) 24

11 DTA/TGA thermogram of RDX (in air) 25

12 DTA/TGA thermogram of RDX (in nitrogen) 26

13 IR spectra of PETN 27

14 IR spectra of HMX 28

15 IR spectra of tetryl 29

16 IR spectra of RDX 30

17 IR spectra of TNT 31

18 NMR spectra of PETN 32

19 NMR spectra of HMX 33

20 NMR spectra of RDX 34

21 NMR spectra of tetryl 35

22 NMR spectra of TNT 36

23 Integral of NMR spectra of tetryl 37

24 Integral of NMR spectra of TNT 38

INTRODUCTION

In compliance with a request of NATO AC 225, Panel IV, Subpanel 2 during its November 1976 meeting, the United States participated in a Round-Robin test program with explosives coming from the same source. The purpose of the program was to develop and standardize methods for characterizing the sensitivity of explosives for main and booster explosives. Each participating country was to test the identical explosives with its own procedures and equipment so that the sensitivity data developed would give Information on sensitivity levels leading to relative rankings for acceptance criteria.

The NATO nations who participated In the Round-Robin test program were Belgium, Federal Republic of Germany, France, Italy, The Netherlands, United Kingdom, and the United States. For the United States the tests were performed by the Energetic Materials Division, Large Caliber Weapon Systems Laboratory, U«S. Army Research and Development Command, (ARRADCOM), Dover, NJ 07801.

The five candidate explosives selected for the program were PETN, HMX, RDX, TNT, and tetryl. These materials were obtained and distributed by Bundesinstitut fur chemisch-technische Untersuchungen (BICT), Federal Republic of Germany. The analytical data on these materials are listed in a BICT document dated 7 April 1978, which is included in the appendix.

TEST PROGRAM

For the United States the following sensitivity and characterization tests were conducted on the five BICT-furnished explosives:

Impact Sensitivity Tests

Picatinny Arsenal Impact Tester

Full curve - 20 samples per point 50% Point (Bruceton method) 10% Point (Picatinny Arsenal method)

ERL (N0L) - Type 12 Impact Tester

Full curve -20 samples per point 50% Point (Bruceton method) 10% Point (Picatinny Arsenal method)

Thermal Sensitivity

Melting point 373 K (100°C) vacuum stability test Explosion temperature test Differential thermal analysis/thermogravimetric analysis

(DTA/TGA) Differential scanning calorimetry (DSC)

Electrostatic sensitivity test Infrared spectroscopy (IR) Nuclear magnetic resonance (NMR) Chemical analyses Particle size distribution

RESULTS

The test program began with a drying period. Each of the explosives were placed in a vacuum oven at 333 K (60°C) over a weekend and then sieved through a 1mm mesh coarse screen.

Impact Sensitivity

The impact sensitivity tests were performed on the Picatinny Arsenal (PA) (now ARRADCOM) impact apparatus and the ERL (NOL) Type 12 Tool impact tester. The PA impact tester utilizes a 2-kg dropweight (refs 1,2) with the sample in a confined environment. The ERL impact apparatus uses a 2.5-kg dropweight with the sample resting on sandpaper between two anvils (refs 1,2).

The impact sensitivity tests were conducted in a controlled environment - 55% relative humidity at 293 K (20°C) (68°F).

Three test methods were conducted: the full run-down firing curve, (also known as the up-and-down or staircase method), the 50% Bruceton method, and the 10% Picatinny Arsenal point. The run-down and Bruceton methods are well known. The 10% PA point is the minimum height at which at least one of ten trials result in a reaction.

In all the impact tests performed any reaction, i.e. smell, burn, snap, noise, etc. is considered a "fire" or "go".

The results of the run-down tests on the Picatinny Arsenal impact apparatus are listed In table 1. For the same type of tests conducted on the ERL (NOL) Type 12 apparatus the results are listed in table 2.

Table 3 lists the 50% points obtained by the Bruceton up-down method for the NATO explosives as determined with the Picatinny Arsenal and the ERL apparatus. Included are the 10% firing points obtained with the two impact testers. As a comparison, the 50% and 10% points obtained from the full run-down curves of both testers are listed.

Thermal Sensitivity and Chemical Analysis

The following characteristics were determined for the five BICT- supplied NATO explosives: melting point (setting point), acidity (as sulfuric acid), purity, sodium content, insoluble matter, acetone insolubles, inorganic insolubles, nitrogen, and 373 K (100°C) vacuum stability test. The results are listed in table 5. Comparisons are made with the results listed in the appendix.

The confined explosion temperature test (ref 3) was conducted on the five explosives. The results are plotted in figure 1 and the time-to-explosion temperatures for 1-sec and 5-sec are listed in table 6. The results are compared with those of similar United States made explosives (ref 4).

The DTA/TGA thermograms were obtained simultaneously with the Mettler apparatus at a heating rate of 10 K per min. The DTA/TGA thermograms were run in air and nitrogen atmospheres. These are shown in figures 2 through 12. Table 7 lists the endotherms and exotherms, the start of decomposition, and the 10% weight loss temperature for each of the materials.

The DSC runs were obtained with a Perkin-Elmer apparatus, model DSC-1 at a heating rate of 10 K per min. The melting points and the rapid decomposition points (peak) for each of the explosives are listed in table 8.

Electrostatic Sensitivity

Each of the five explosives were subjected to the electrostatic sensitivity test (ref 1). The test was conducted at a voltage of 5000 VDC and a capacitance of 0.02 microfarad at ambient temperature - 293 K (20°C) - and a relative humidity of 55%. For all of the explosives no fires occurred in 20 consecutive tests for each explosive at the 0.25 joule level. This is the acceptance level for the interim qualification of explosives for military use.

Infrared Spectroscopy

The infrared spectra of the five NATO explosives were obtained and are shown in figures 13 through 17. Comparisons were made with IR spectra of United States made explosives (ref 5). The spectra were in close agreement with the referenced materials.

Nuclear Magnetic Resonance

Nuclear magnetic resonance spectra were obtained for a 10% solution of:

PETN in deuteroacetone, (fig. 18) HMX in deuterodimethylsulfoxide, (fig. 19) RDX in deuterodimethylsulfoxide (fig. 20) Tetryl in deuteroacetone (fig. 21) TNT in deuteroacetone (fig. 22)

These NMR spectra (figs. 18 through 22) were compared to those published in reference 6 and they were found to be the same within experimental error. Integrals of the spectra for tetryl and TNT (figs. 23,24) show the expected peak area ratios (within experimental error) for the three methyl and two ring protons found in these compounds.

The procedures for obtaining the NMR spectra also are described in reference 6.

Particle Size Distribution

The particle size distribution for each of the NATO Round-Robin explosives was obtained by the sieve method. The percent retained on each sieve Is noted in table 9.

CONCLUSIONS

For the NATO Round-Robin test program both the Picatinny Arsenal impact and the ERL (NOL) Type 12 Tool tests indicated that PETN was the most sensitive, and TNT the least sensitive explosive. However, HMX, tetryl, and RDX interchanged positions in the relative sensitivity ranking obtained for one impact tester when compared to the other.

A comparison was made not only between the test apparatus but also with the methods used. The Bruceton 50% point and the Picatinny Arsenal 10% point were compared to the same values obtained from the full run-down test data.

Black particles were seen in the solution but not in the powder.

The following points are observed with reference to the relative rankings:

1. The PA impact test produced the same relative sensitivity ranking based on the Bruceton 50% and PA 10% points:

PETN > HMX > tetryl > RDX > TNT

(In this connotation the term > means "more sensitive than")

Using the 50% and 10% points from the run-down tests to obtain relative rankings, the results were the same as above except that tetryl and RDX switched places (although HMX and RDX had almost the same value in the 10% point).

2. The ERL test produced the following relative ranking based on the 50% Bruceton point: PETN > tetryl > HMX > RDX > TNT. For the rankings obtained with the PA 10% point and the run-down 10% point, HMX and tetryl reversed positions. The run-down 50% point produced a ranking of PETN > HMX > RDX > tetryl > TNT.

3. The 50% Bruceton and PA 10% point on the Picatinny tester had produced the same rankings as that obtained with the PA 10% point with the ERL tester, namely PETN > HMX > tetryl > RDX > TNT. However, in the ranking obtained with the 50% Bruceton using the ERL tester, HMX and tetryl reversed positions.

4. In the run-down tests the 50% point on the Picatinny and ERL testers produced the same rankings, namely, PETN > HMX > RDX > tetryl > TNT. With the 10% point, RDX and tetryl reversed positions.

The ranking of the explosives in accordance with the explosion temperature test was as follows: PETN > tetryl > RDX > HMX > TNT.

Within experimental error the chemical analysis agrees with the data furnished in the appendix.

The explosion temperature data show some slight differences when comparing similar data obtained with similar United States made explosives. The DTA/TGA thermograms confirm the DSC data. In terms of thermal sensitivity the explosion temperature data agrees with the DTA/TGA and DSC data.

The IR and NMR spectra of each explosive were compared to referenced spectra and the traces are in agreement.

In the electrostatic sensitivity test no fires occurred for each explosive at the 0.25 joule level.

The data in this report is to be forwarded to BICT for analysis with the data generated by the other NATO participants.

REFERENCES

1. Joint Service Evaluation Plan for Preferred and Alternate Explosive Fills for Principal Munitions, Volume IV, Joint Service Safety and Performance Manual for Qualification of Explosives for Military Use, prepared by Joint Technical Coordinating Group for Air-Launched Non Nuclear Ordnance, 12 May 1972 (based on NAVORD Report OD-44811), (AD-A-086259).

2. G.R. Walker (Ed.), "Manual of Sensitiveness Tests," TTCP Panel 0- 2 (Explosives). Canadian Armament Research and Development Establishment, Valcartier, Quebec, Canada, February 1966.

3. H. Henkln, R. McGill, Ind Eng Chem., 44, 1952, p 1391.

4. L. Avrami, H.J. Jackson, M.S. Kirshenbaum, "Radiation-Induced Changes in Explosive Materials," Technical Report PATR 4602, Picatinny Arsenal, Dover, NJ, December 1973.

5. F. Pristera, W.E. Fredericks, "Compilation of Infrared Spectra of Ingredients of Propellants and Explosives," Technical Memorandum PATM 1887, Picatinny Arsenal, Dover, NJ, September 1969.

6. V.D. Hogan, T.A.E. Richter, "A New Convenient Tool for Identifying Composite Explosives: Proton Magnetic Resonance Fingerprinting," Technical Report PATR 4790, Picatinny Arsenal, Dover, NJ, June 1975.

Table 1. Run-down test results of NATO round-robin explosives obtained with PA impact tester

cm Height

in. PETN

12.7 5 0

15.2 6 20

17.8 7 15

20.3 8 45

22.9 9 50

25.4 10 55

27.9 11 55

30.5 12 70

33.0 13 80

35.6 14 85

38.1 15 100

40.6 16

43.2 17

45.7 18

48.3 19

50.8 20

53.3 21

55.9 22

58.4 23

63.5 25

68.6 27

71.1 28

Explosives - percent fired HMX RDX Tetryl TNT

0

10

10

15

25

50

65

70

90

100

0

25

30

35

50

65

85

80

95

100

0

10

25

30

40

55

70

80

90

100

0

10

15

30

35

45

60

70

75

75

85

100

Conditions: (1) 2.5-kg dropweight

(2) 20 samples per height

Table 2. Run-down test results of NATO round-robin explosives obtained with ERL (NOL) impact tester

Height cm in.

25.4 10

33.0 13

40.6 16

50.8 20

55.9 22

63.5 25

71.1 28

76.2 30

88.9 35

101.6 40

106.7 42

127.0 50

132.1 52

152.4 60

157.5 62

177.8 70

182.9 72

203.2 80

228.6 90

279.4 110

Conditions:

PETN

0

25

55

70

100

Explosives - percent fired HMX RDX Tetryl TNT

10

30

65

65

90

100

15

10

50

70

90

100

10

55

65

80

100

0

10

20

40

70

80

50

75

95

(1) 2.5-kg dropweight

(2) 20 samples per height

4-J

03 »H >H

OJ a» CU 4J 4->

CO

4-1

CO

e CU O O O CO o CU 4-1 • • • • ■ 4-1 B

o TJ 0l m ON co \o i-i T3 CJ

1 o

rJ o <n<r Hio O

c 4-1 o 4-1 o

e 01 6

z g z

4J g ä s ä

iH o W o W ^ TJ O st 00 CO CO *o

1 CM V40 i-l i-H CM I CO d n 6 d M 4-1 3 cu o St O CO >tf 00 3 CU B d PÜ 4-1 st -tf st CM <t Pi 4-1 0

•H 10 CO

o cu CU o. 4J

st O O m o 4-1

^s s • • • ■ • ■ X d o o c N vO N O^ O o •H I-l CJ •H i-l t-l f-l i-l CJ

X 9 <5 o pc OH CJ p 53 3 3 4-1 4-1

3 c d •H

O ON O 00 CM 00 O |H •a Pk rJ vo oo r^ CM oo PH CU c 1) 4-1

« c

4-* CO

CO i-l CO ,CM CM 00 d

CO

CU

g iH cu +1 +1 +1 +1 +1 iH 4-1 B r4 4J 0 u 0

o •H CJ in o co m o •H <~\ •a Pn ON O CO o o • • • • •

Pn rJ O

•a S^ o i-i to in i^ st 6*5 Z c o z co co «a- i-i st O s-x

« in Nw* i-l

I •a ä ä

s o •o w j= w o

&^ 4J CO S * 1^ VO JC o 01 i-H CO CM st \C 4J u-i B • • • • • S d o

G o

CO •"-! CM St 00 e n +1 +1 +1 +1 +1 s U B

4-1 4J cu e o cu 0 cu 0) 4J CJ oo oo CM r^ vo CJ 4-1

u CJ CO i-H <t 00 CO st Q CO 3 3 cu • • • • • <c cu U l>4 4-1 CO i-l CO 00 CO p£ 4J

pa pa <t St St CM St pq

<*H s ^ s o cj VO St ON VC I-l

CM m oo r» st CJ

e 3 • • • • • <c o PS i-l O O i-t CO pj CO

•H CO <c • +1 +1 +1 +1 +1 <c d H 4-1 3 •H «) iH •H o co m r» oo a s O CO CM i-l o S co • • • • ■ o cu NvCNi-ld

CJ VJ i-l i—l i-l i-l i-l

• CO

rH ai >N

■H U Z 4J P< X H H

H 53 2 PH H H

00000 m 00 00 C co CM rH CM l-H CO

vo 10 m CM i-i

NO C O "1 ON CO CO CO i-H CO

St CM CM NO

ON i-H i-H O ITl CM CM CO i-H CO

NO St l-H CM VO

m in 00 u-\ o CO CM CO rH St

st o m ,_ vo i-H i-H i-H ^ rH

u 0) EH !

Z X H

Pi

Table 4. Relative ranking of NATO round-robin explosives according to impact sensitivity tests

a. ARRADCOM impact test

Bruceton ARRADCOM Full run-down curve 50 % pt 10% pt 50% pt 10% pt

PETN PETN PETN PETN HMX HMX HMX HMX Tetryl Tetryl RDX RDX RDX RDX Tetryl Tetryl TNT TNT TNT TNT

. b. ERL (NOL) impact test

PETN PETN PETN PETN Tetryl HMX HMX HMX HMX Tetryl RDX Tetryl RDX RDX Tetryl RDX TNT TNT TNT TNT

NOTE: The rankings are listed as the most to the least sensitive explosive.

10

oo oo

CM O m I-. CO

O o • • .-i 00 in r~- CO

o> I o .-I

O

o

«3- O

CO CD > CO o

rH a x 

o o

CO o

m CM

o

1 CO CJ

•H 4J CO

•H tJ 0) 4J O CO u CO

CM C> rH O CM S* <* rH U 4J 1 1 CU H oo oo • •

rH 00 O CM «tf rH

o o O r- m CM

CM

o vO CO

«0 oo

vO o o o o CM

X> CO H

oo oo CO o rH «tf

Ss -d- t-i H W 1 1 cm

VO vO ■ •

CM O^ i-H CO «* rH

CO o

o> r-.

CO CM

■ä 4J 00 M m

ft« tu-^ 4J x: X M

CJ s^

u s^o S SÜ ^ o

4J ■u 4-> -<r

»-S B~S •M •> C 4-J ^? s-s I-H »"s CM CN 3^ o CD CO M U • •

•H 4-1 •rH 4J B ft M S-« ■O 0 CM O o a M e CO CO * o a 3 o M-H fr^ 4= QJ X C XI 4-1 4J 4J T3 T3 ■H •H o 4-1 O M o IJ 3 3 3 i-l CO CO X

11

Table 6. Time to explosion temperatures of NATO round-robin explosives

PETN HMX Tetryl RDX TNT

1 sec 562 K 614 K 564 K

289°C 341°C 291°C

5 sec 496 K 560 K 507 K

223°C 287°C 234°C

5 sec (ref 4) 501 K 573 K 516 K

228°C 300°C 243°C

Explosion temperature ranking

PETN Tetryl RDX HMX TNT

577 K 776 K

304°C 503 °C

521 K 473 K

248°C 400°C

534 K 669 K

261°C 396°C

12

W tu >

•H CO o a tu

c ■H XI O l-i I

c 3 O u o H

O

c o

•H 4-1

<fl N

■H IJ. CD 4J U cd M cd

O

Ü •H 4-1

cd Ö cd O

CD

H

cu

XI cd H

^ S /-^ •"■* 0 W u 0 O M 3 o r^ 00

r*. cn o • co - 1 B fc^ 0 1 C m

0 f^ o o 01 •H 0> •H r4 £ äO^ Ö0 v^ 4J

0) 04 IJ co i* CO K

0) -* ■a —' o ^^ CD co a> o

o in •C MD -Q MD

m oo o m CM co

o co r^ MD CM co

O co

00

CM

co w r-* co *tf MD

O MD co cn

co u-i m

m m

o o 0 0 o CM 0 0 0 0 0

00 O O CM r-. cn o o o in CM CM CN in \D MO r^ cn 00 -tf r^ MD o O CM CM l-i <—1 i-i w .-i cn CM CN CM CM

o m m o

rn cn in f-t «a- MO

co co <r cn m in S

B B 1

^ cn

-» -3-

O 00 so in

< EH a

0 0 0 0 D 0 0 o o at*: O r- m in m m r- cn m co p r-* r* r-* r» O-N a« r^ r* f-t l-t tu « i~* >-* " i-H i-< .—i .—1 CN CM CM CM CO 03

-X < oo Ü T4

P.CJ B o o ^ o , o a •o

CM * 0 B

o

< rH U o H >

o -o SD SO

U •H

CJ J3 -H ai a t-) (o tQ 40 O iH

0 o 3 B 4) CM co 03 4J .B MD MD « »H •—1 B CJ

sed o

re of

/min

sampl

m MD n a w co CO •O co O " <LT <t

proximate,

level pres

ting rate 1

or to trial

H ft. CS CO *H ■H CM ca at ai u < SS

Values are

e: 1.

S 2.

H 3.

P

X X 44

ä ä 0 * 1Z

13

Table 8. DSC results of NATO round-robin explosives

Perkin-Elmer DSC-1, 10°C/min (lid crimped on sample)

Explosive M.P. Rapid decomposition (peak) K UC K UC

PETN 414 141 475 202

Tetryl 403 130 479 206 (detonated)

RDX 483 210 500 227 (detonated)

HMX - 551 278 (detonated)

TNT 346 73 606 333

Table 9. Particle si ze distribution ( sieve metho« a)

(mm size) Percent retained

Sieve PETN HMX Tetryl RDX TNT

# 30 (0.59) 0.9 21.9 90.3 0.4 61.0 # 80 (0.177) 98.0 77.0 9.7 94.1 29.8 #100 (0.149) 0.7 0.8 3.9 3.9 #140 (0.105) 0.3 0.2 1.1 4.8 //200 (0.074 0.1 0.1 0.5 0.5

14

CO 0) >

■rl

CO

O rH O, X CU

£> O U I

■a c 3 O

o H < S3

M O

> 3 O

CD

4-1

« a> a e 01

e o

•H a? o

.-H a w

0)

15

30 40

,o ei-

.-* I .no ,/ ' ^ r~, .*

°C. ;:

(

\

50

\

60V

I CO efltn

»

80 I

\ \

X

100

00

G) u S CD

■H CO

C

H

o

e ca u

o

0>

< Ü H

< H a

0)

bO

* I. 20

< !L5

t Q

so

I 90 100

Q.

E

16

i\

/

U 30 40 SO 60 7ol go loo:

o

> ^ J*

to 50

<

a

a; uo o

00 4J

\ f\ •H c

0) c u •H

(D Q H

2 ^r H

"~ o

^ \ 0 & *> CO •$& :.

bO O

90 \ioo

i

u

30 40 SO 60 BO 90

Q. E

,(L)'

100

m m

bO

17

10

io

/ ( I i I

io 30 40 SO «O 7©

— oo

80

ioo > -»•■

90 1O0

\

fh vZ S r g-

-V,

!•■ <■•§ < Jfc p O) (0 h ^E «< <^y *— Q f „^ TlC . .

20

00

0 u

CM

so 60-

Q

80 90 100

->

Q8§

SO 40 SO 60 80 90

Q.

100

ed

c

H w

14-1

o

g u o

0)

H

a)

c5

1-8

i 30 40 100

<

I-

5 m —

'25 .OF

20

<

30 40 50

— X

4-

^

03 r\ Q u CD Q 00

too

c OJ uo o JJ t-i c c

•H

z H W Pu

H-l o

u bO O B M 0)

o H

tu 1-1

bO

19

20 40 SO

3

V.

tf

vs

f 30 40 50

■a/

i*> 30 40

lOO

/*P 'mo <->,> x>£j/

oo (\ 0) /—s

u •H

<U O •H

ro w

*"" r-J

lOO 4-1 01

4-1

<4-<

o

l-l ■ bO

o

E a; ^ 4-1

: < ' o ( H

< 1 H

C

50

dl t-i 3 bo

100 I

* 1 C

■'., J <ni

1- m 4- • i^

5.

5 HJ.fi

T

^

$*-

£E NS4_

< ■4 Q. E

2D

20 30 40 SO 60 70 80 90 100

(ft J .

'i.

<? o

V o (S

3 O f£ V <a 00

...v* r "

v? £ !

ao >'

> C* .'■• ■;

fo

•3

g CD01

^E

,-5 ^.j CJ

ctf

i

2d-

• - 0 -

d o ^*

1 w ■ S v fc'--.

«5- a/

.4c.°

2

30 40 SO 60- 70 60 99 100

\ C s h

T3 C

00 CM

l\ •~\

CD u , re u CD c Q •H

r— ^~ iH

rt

■*-

30 40 SO J 80 90

^ Q P

< eft f2 E

1ÖO'

E ,0)

> O) < 3C

S2. -—>~ 7

Uj

a re M

o e 01

J3

0)

21

40 SO 60 too

) I

•NO KV

8 i 3 \ i \

■^

*$

> > ? )

o 1 E ^*- -'

'i «S '. ,/ 1 < J

( \ >

I ": i

I! OP a-i •— c

V = 4 i- <r —c£ •/ <t 3o 4 ä J.4. j-

'-—i~ii ^& n, .r. —■

5 l T

>^J

4o

00

u (ü Q ro

1(10

Q.

^

c a; bo O U

u

o

B to M be O e a)

3 < H

oo

•H

40 SO 60 SO JOO

22

so

Z* to '

.>-

40 SO 60 ! | 70

"h 1—i

5S

80 90 i »bo

■r) CO

c •H

2"*

i

40 SO

! 6oi 70

00 r\ CD u

&

80 90 too

B CO IJ bo o e u 0)

< o H

H Q

0)

3 ■H I*

< < 0

b O

Q. E

20 SO 40 SO 60 70 80 90 100

23

Q uj

s •a

o

'S"

10

g s:

Si 5 4»

1! '3

.1.0

30 40 50 70 80 90 IOO.

V

gf J

,♦4 *■ x 5- s

52:

**> v0o

f j' J20 f

0

-?**-

O) < ZI en Q_ E ,0

c oj W O M

4-1 o

O

OJ

3

H n

0)

3

20 30 40 SO eo 70 80 90 100

24

i 5

* Vu

20 V <

30

2>

40 SO

/

/. S «

\

60 100

\

r- 0

\ \ .1 i V w J ft. i 1 I

w i 5 ti !

i i

J i 1 t

\S i

l-l •H ed

(3

i f

}

!

J

1^ f o 19-' *.

GA

g/

in

<

15 -i -£ Q

I <t -^ O i l~~ <*< «7 -J * «* - Ü .1 £ ■4.* '1 1 5~ ir .0 1"

<i_> i>S :■» f» 5^

X *a £* -*o --I ex =w <d

30

\ 40 V 50

*.u

■\

\

30 40 50.

eo!

5

60

CDF

25

70

70 BO 90 KO

Ü.

|2

e (0 1-1 W) O

<U

ü H

H O

u 3 be

« ^1 .

10 20 30 40 SO 60

la 3 la

t ?.

*3 o

/

M 70 _ V,

o *

.\

as

20 30 40 SO

80 SO IOO

30 40 qo

00

u

Q

90 100

90

CL

,<D

100

c

o

c •H

X Q

M-i O

bO O

0)

3 H

H C

CN

0) l-l

•H

26

> w u PM

■*-—» IM

>- o u M

z 4-1 l_L) O

ID 0)

O CO

C£ pfi

CU

3

% 3DNVlilWSNVäl

27

o m u 4-1 o <u p. tfl

a; u bO

% 3DNVillWSNVäl

28

oo o CM

o o

o o oo

o o r~— 1 rH 1

t-l

> 4->

U 4-1 ^~—~ o U-i r-> >- o "<* u 1 z U

LU 4-1

Z) a 09

o o

LU

u_ H

■

i—i

(l)

o 3 bO

o CM

% 3DNVlilWSNV^l

29

2 X

>- u U-t z O

LU R) ID M

U LU Qi 03

BÜ

sO

3 bO

•H

% 3DNVLLIWSNVäl

30

2 u >- u z UJ => O UJ

u 4-1

O 0) & to

pi

3 i-l

% 3DNVlllWSNVai

31

I —o

X w t*^ z h

"S

i .

o — o ■

.

o — o

<

o — o CO

z

CM

■^

■

<

'

> o

(-9 ■

■

"

■

■

o —o in

'

1

53 H W a.

w w Ä p iu ui u i s s 5 u. 0) in u. I

Al Q U i;

— = D £ W H => £ i -. i- E

CO is u_ _ < U. 2 _i OJ< Q. E K

3 o. t co co £

Wf

00 I—I

<D M a to

32

■ £ 1 —o

■

<A

- ■

- ■

- ■

- - • - ■

- o — o

.

- O

o in r ■

- o

1—o —= • - *? ■

- "

- ■

- ■

- - ■

- -8

< ■

■

- ro

■

■—-^

_ • - . o —o , .

< - ■

- • - 1

- '

- -8 —

■

m CO

s Si. * «^ 8 « r r* T * V «o i] s Z. « ^

« _^ o 's (M j LLI I -UJ co

X s

CT>

u s

LU 2 9 a. i i s UJ UJ £ p

s s 5 u. co co u. tz

Ml ■ . n UJ ^ -§ Q cp 15 K = fc x ti •- E

o

UJ

3 3 °- w- < 1 5

i<£ a: tr - r. o z z

5 £ CO CO

O _

o 5

33

O CM

0) v> u =r- 3 V* bo

34

-8

£

£*•>■ N U

o £ ^ P3 UJ 5 \D o 3

■ o CO

D 3 <

1

O

UJ

UJ £

2x"H

7^

CM

0) M 3 bO

a. o. i * UJ UJ m p UJ UJ £ fi S ä 5 u. co co u. cr

< a

rf» l 111 ■ '

3gsg UJ CO < I- HI

55 u-2« O 3 < o. E cr UJ cj « UJ a 5 a- z ._ — ^

x C5 z z z

- ^ z it CO CO S CO

> a.

< 5 * -o

<> ii o „

o 2 ?5

35

1 -8

t\ \n > •< v;

u

to

ii

o >

\n •^ sa

■>

-§

U

V-

3.

UJ ij

£^p □ m H£

I_ Q- ^J LLI w s I fe li_ < DC U- S _l [r, ° 2 < Z Q. £ oc 5

£ iLl ff 2 3 o. t a. CO CO £ CO

m CM

0) M 3 DO

> a.

37

x 1

•

■^

-8 >

■

-8 CM

>> ■

it

■

O O

CO

to ^

V»

- ■

■ • ■ -

■

- . ■

-

o —o -<* O

>•

1: . . ■

■

'

-8 — ■

o HI CO

w t 2 9 P 5 0. CL UJ 111 UJ UJ

s s co v>

@ 8 rl «* 8 ~ X > f 8 " r S - e

(** « 1 N X - _i ™"

I K ii

^ NA

eg

OJ M 3 bO

tu

l\ d u. u. IT

3

*! ni IS

Ö P Q <0

*5 •- £ UJ 2 </) < It a ° 5

5 o. co co

fc = UJ 0.

? '< < a.

n - o z

£ co

> Q.

< 5

o Ä CO Q

si o s

38

APPENDIX

SAMPLES OF HIGH EXPLOSIVES SELECTED FOR A NATO ROUND-ROBIN TEST

39

Bundesinstitut für chemisch-technische Untersuchungen CBICT)

5357 SwiSttal, 7.^.1976 Hoimerzho'm

Fornaorochor: (0222S) «061 Fernscnroiüer: 8600310 cli a PoBionocnrifti Poatfacn ' 7 02 00 0300 Bonn 1

Samples of High-Explosives

selected for a NATO-Round-Robin Test

The for the NATO, for explosives competent gremium, AC/225,

subpanel IV 2, was asked by the Air Armaments Working Party

(AAV/P) to develop and standarize methods for characterizing

the sensitiveness of explosives for lead- and booster charges,

and to define the sensitiveness limits of STANAG 3525 (see

also AC/225, panel IV, D/77).

To accomplish this task, the subpanel IV 2 arranged a Round- Robin Test, where the participating nations were to ascertain,

with their usual test equipment and methods, the sensitiveness of identical high explosives. <

As typical explosives TNT, HMX, RDX, Tetryl and PETN were selected for these investigations.

The BICT supplied countries, willing to participate on the Round-Robin Test, with 1* kg each of above mentioned explosives and provided following places with samples:

BELGIUM

FRANCE

NETHERLANDS

UNITED KINGDOM

260 Cie Mun.; Camp Reine Astrid

518 Probsteierwald über Eschweiler, RFA

Etablissement technique de Bourges -

Division de Contröle Pyrotechnique - 18015 Bourges

Technologisch Laboratorium TNO

Prins Maurits Laboratoria

Rijswijk (Z.H.) -2100, Lange Kleiweg 137

Procurement Executive

Ministery of Defence, PERME

Waltham Abbey, Essex EN 9 1BP, Powdermill Lane

41

- .2 -

UNITED STATES ARRADCOM - DRDAR

Large Caliber Weapon Systems Laboratory

Energetic Materials Division (-LCE)

Dover, N.J. 07 801

ITALY MARIPERMAN, La Spezia

Italy on its own accord received a Tetryl-sample only.

The shipping of TNT and Tetryl took place in the state as

received from the manufacturer, HMX, RDX and PETN were shipped

moistened with 30 % water to comply with shipping regulations.

Prior to the tests the moist samples were dried at 50°C under

vacuum until a constant weight was reached. Then the dried

samples were screened through a coarse sieve (1 mm mesh) to rid

them of lumps. Thus a uniform, free flowing product was obtained.

All samples should be tested without additives or further break-

down of particles.

The explosives were purchased by us since we ourselves are not

in a position to produce lots of this size. Later difficulties arose, since the supplier were not able or willing to furnish

the manufacturing history of the various explosives.

In the enclosures 1 to 5 you will find further details on said explosives. Moreover it will remain our endeavour to obtain

details on manufacturing procedures which will be forwarded to the involved nations.

Dr. Bartels

42

Anlage 1

zu 3.4-9/4510/78

TNT-Probe für Round-Robin Test

Hersteller:

(Manufacturer)

Probenbezeichnung:

(sample symbol)

Fa. Dynamit Nobel AG (W-Germany)

Werk Leverkusen-Schlebusch

S - 1 - 32, Charge 7 vom 14.12.1972

Herstellungsverfahren:

(manufacturing-process)

Aussehen: (appearance)

Erstarrungspunkt:

(Solidification point)

Schmelze:

(melting).

flüchtige Bestandteile;

(volatile material)

Acidität:

(acidity)

Alkalität:

(alkalinity)

Benzolunlösliches: (insoluble in Benzene)

Glührückstand: (ash)

Natrium:

(sodium)

Chargenverfahren, Nitrierung in 3 Stufen und anschließende Reinigung des Roh-TNT durch Natriumsulfit-Wäsche

(Batch-process, three-stage nitration and purification with Sodiumsulfite)

hellgelbe Schuppen, ca. 0,54 mm dick

(light-yellow flakes, ca. 0,54 mm thick)

80,77°C

klar, ohne Bodensatz

(clear, without insoluble material)

<0,01 %

<0,001 %

keine

(none)

< 0,001 %

- 2

43

- 2 -

Anlage 1 zu 3.4-9/4510/78

Oxidierbare Bestandteile:

(oxydable components)

Ausseigerung':

(exudation)

Fleck-Probe:

(spot-test)

Vakuumstabilität:

(Vacuum stability)

Verpuffungspunkt:

(deflagration-point)

2,6 - DNT

2.4 - DNT

3.5 - DNT

r - TNT ß - TNT

0,002 %

0,020 %

0,030 %

0,050 %

0,004 %

Beim Zufügen von 0,002 n KMnO,-Lösung zu einem durch Kochen mit Wasser er-. haltenem Auszug keine Entfärbung in 1 h

(no decoloring of a KMnO^-solution 0,002 n for 1 h after adding an extract from TNT obtained by boiling with water)

0,08 %

23 mm 0

0,02 ml (2,5 g/l00°C)

297°C (0,5 g; 20°C/min)

(Die Daten sind dem Prüfbericht 2.1-2/3724/75 entnommen)

44

Anla/re 2 zu 3.4-9/4510/78

HMX-Probe für Round-Robin Test

Hersteller:

(manufacturer) Fa. Soc. Nationale des Poudres et

Explosifs (SNPE) Poudrerie de Sorgues, Frankreich

Probenbezeichnung: (sample symbol)

Herstellungsverfahren:

(manufacturing process)

grade I classe I Nr. 122 60844

Lieferung vom 21.8.1973 (receiving date: 21 of August 1973)

keine Angaben, konnte auch anläßlich eines Besuches bei der Herstellerfirma nicht in Erfahrung gebracht werden. (not yet available)

Aussehen:

(appearance) farblose Kristalle (colourless crystals)

Schmelzpunkt: (melting point)

271,8°C

Acetonunlösliches: (insoluble in acetone)

Glührückstand: (ash)

Unlösliches auf US-Sieb 60:

(insoluble particles)

Acidität: (acidity)

0,01 %

0,01 %

0,002 % (als CH,C00H)

KornVerteilung:

(particle distribution)

Hexogengehalt: (RDX-content)

> 0,5 mm 31,22 % > 0,3 mm 44, oo % > 0,15 mm 20,8o % > 0,125 mm 1,56 % > 0,075 mm 1,52 % < 0,075 mm 0,9o %

2,2 %

- 2 -

45

Anlage 2 zu 3.4-9/4510/78

- 2 -

Vakuumstabilität: 0,13ml' (2,5 g/l00°C)

(Vacuum stability)

Verpuffungspunkt: 274°C (0,5 g; 20°C/min)

(deflagration point)

(Die Daten wurden aus dem Prüfbericht 2.1-2/3711/75 entnommen)

46

Anlage 5 zu 3.4-9/4510/78

RDX-Probe für Round-Robin Test

Lieferant: (supplier)

Probenbezeichnung': (sample symbol)

Hersteller: (manufacturer)

Herstellungsverfahren: (manufacturing process)




Alkalität: (alkalinity)

Acetonunlösliches: (insoluble in acetone)

Fa. Dynamit Nobel AG, Troisdorf

Lieferung vom 22.4.1974 (receiving date)

Fa. Soc. Nationale des Poudres et Explosifs (SNPE) Frankreich

keine Angaben Die Lieferfirma wurde gebeten, sich mit dem Hersteller in Verbindung zu setzen. (not yet available)

weiße Kristalle (white crystals)

204,6°C

0,003 % (als CHjCOOH)

keine (no)

0,01 %

sandige Bestandteile: (sandy materials)

Aschegehalt: (ash)

keine (no)

./.

Kornverteilung: (particle distribution)

Rieselfähigkeit.; (purling)

>0,5 , mm 1 ,oo % > 0,4 mm 1,58 % > 0,315 mm 21, o4 % > 0,2 mm 56,49 % > 0,1 mm 18,89 % > 0,05 mm 0,92 % <0,05 mm 0,08 %

Trei fließend,'ohne Klumpen (free flowing, without lumps)

- 2 -

47

Anla/re 3 zu 3.4-9/4510/78

- 2 -

Vakuumstabilität 0,26 ml (2,5 g/l00°C) (vacuum stability)

Verpuffungspunkt: 238°C (0,5 g; 20°C/min) (deflagration point)

NH^+, Cl~, SO^, NO," nicht nachweisbar (not detectable)

(Die Daten stammen aus dem Prüfbericht 2.1-2/3729/75)

48

An 1,",,"■>; 'i

zu ~j. 4-9/4510/78

Tetryl für Round-Robin Test



Fa. Dynamit Nobel AG (W-Germany) Züfa, Troisdorf

Charge 43, Lieferung vom 2.4.1976 (receiving date)




flüchtige Bestandteile: (volatile material)

Benzolunlösliches: (insoluble in benzene)

Aschegehalt: (ash)

mechanische Verunreinigungen; (impurities)



Kornverteilung: (particle distribution)

Stufenweise Nitrierung von Dinitro- methylanilin, Stabilisierung, an- schließend Umkristallisation aus Aceton und Granulierung (stepwise nitration of DNMA, stabilization, recrystaliisation from acetone followed by granulation)

hellgelbes, feinkörniges Granulat (light-yellow, fine granules)

129,2°C

< 0,01 %

0,02 %

./.

keine (no)

0,003 % (als HNO»)

keine (no)

> 1,0 mm 14,2 % > 0,5 mm 85,8 % < 0,5 mm

Rieselfähigkeit: (purling)

Schüttdichte: (bulk density) Vakuumstabilität: (vacuum stability)

Verpuffungspunkt: (deflagration point)

fließt ohne Stocken durch einen Trichter mit einer Öffnung von 6 mm 0 (free flowing through a funnel with 6 mm 0 stem opening)

0,94 g/ml

0,15 ml (2,5 g; 100°C)

200°C (0,5 g; 20°C/min)

49

.AnIngo 5

zu .5.4-9/4510/78

PETN-Probe für Round-Robin Test


Fa. Dynamit Nobel AG (W-Germany) Züfa Troisdorf





Stickstoffgehalt: (nitrogen content)



Acetonunloslich.es: (insoluble in acetone)

sandige Bestandteile: (sandy materials)

Bergmann-Jung-Test:

Abel Test bei 80°C:

Korngröße: (grain size)

Rieselfähigkeit: (purling)

Vakuumstabilität: (vacuum stability)

Verpi:f fungspunkt: (deflagration point)

Lieferung vom 30.5.1974 (receiving date)

kontinuierliche Nitrierung von Pentaerythrit und Umkristallisieren aus Aceton (continuous nitration of pentaerythritol and recrystallisation from acetone)

weiße Kristalle (white crystals)

141,4°C

17,7 °/o

< 0,001 % (als HNO,)

keine (no)

< 0,01 %

keine (no)

0,3 ml/g

keine Färbung innerhalb 60 min (no color in 60 min)

sehr fein, wegen elektrostatischer Aufladung nicht bestimmbar (very fine, because of electrostatic phenomena not determined) rieselt ohne zu stauben, keine Klumpen (free flowing without dust, no lumps)

0,64 ml (2,5 g; 100°C)

(0,5 g; 20°C/min) 203°C

(Die Daten stammen aus dem Prüfbericht 2.1-2/3732/75)

50

DISTRIBUTION LIST

Commander U.S. Army Armament Research and

Development Command ATTN: DRDAR-GCL

DRDAR-LCA, Dr. H.D. Fair DRDAR-LCE, Dr. Walker (3)

Mr. L. Avrami (15) Mr. M.S. Kirshenbaum (5)

DRDAR-SFS, Mr. E. Demberg DRDAR-TSS (5)

Dover, NJ 07801

Administrator Defense Technical Information Center ATTN: Accessions Division (12) Cameron Station Alexandria, VA 22314

Director U.S. Army Materiel Systems Analysis Activity ATTN: DRXSY-MP Aberdeen Proving Ground, MD 21005

Commander/Director Chemical Systems Laboratory U.S. Army Armament Research and

Development Command ATTN: DRDAR-CLB-PA

DRDAR-CLJ-L APG, Edgewood Area, MD 21010

Director Ballistics Research Laboratory U.S. Army Armament Research and

Development Command ATTN: DRDAR-TSB-S Aberdeen Proving Ground, MD 21005

Chief Benet Weapons Laboratory, LCWSL U.S. Army Armament Research and

Development Command ATTN: DRDAR-LCB-TL Watervliet, NY 12189

51

Commander U.S. Army Armament Materiel

Readiness Command ÄTTN: DRSAR-LEP-L

Scientific and Technical Info Div Safety Office

Rock Island, IL 61299

Commander U.S. Army Materiel Development and

Readiness Command ATTN: Scientific and Technical Info Div

Research Development & Engineering Dir Research Division Engineering Division Safety Office

5001 Eisenhower Avenue Alexandria, VA 22333

Department of Defense Explosives Safety Board ATTN: Mr. R. Sawyer Washington, DC 20314

U.S. Army Foreign Science and Technology Center

ATTN: Code DRXST-CSI, Mr. J. Jacoby Charlottesville, VA 22910

Commander U.S. Naval Sea Systems Command ATTN: SEA-04H13, Mr. E.A. Daugherty

SEA-064E, Mr. R.L. Beauregard Washington, DC 20362

Commander U.S. Naval Weapons Center ATTN: Code 3262, Mr. J.C. Whitson

Technical Library China Lake, CA 93555

Commander Naval Weapons Station ATTN: Mr. W. McBride

Dr. L.R. Rothstein Yorktown, VA 23491

52

Commander Naval Surface Weapons Center ATTN: Code R, Research and Tech Dept.

Code X-21, Mr. F. Menz, Tech Lib White Oak Laboratory Silver Spring, MD 20910

Director U.S. Army TRADOC Systems

Analysis Activity ATTN: ATAA-SL White Sands Missile Range, NM 88002

CDR N. Clausen (15) Material Management Systems Section Defense Support Division NATO Headquarters 1110 Brussels, Belgium

British Embassy ATTN: Dr. G. Hooper 3100 Massachusetts Ave., N.W. Washington, DC 20008

Dr. R. Derr OUSDRDR&E The Pentagon 3D1089 Washington, DC 20301

Commander DARCOM ATTN: DRCIRD-I, R. Schlegel Alexandria, VA 22333

53

ttchnkaluwarv technical 5 0712 01016679 0 l library» - … · explosion temperature tnt petn 20....

Documents