Chemical Industry & Chemical Engineering Quarterly

Available on line at Association of the Chemical Engineers of Serbia AChE www.ache.org.rs/CICEQ

Chem. Ind. Chem. Eng. Q. 26 (2) 183−190 (2020) CI&CEQ

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HICHAM KEMMOUKHE1

SLAVICA TERZIĆ2 MIRJANA DIMIĆ2

DANICA SIMIĆ2 ZIJAH BURZIĆ2

LJILJANA JELISAVAC2 1Military Academy, University of

Defence, Serbia 2Military Technical Institute,

Belgrade, Serbia

SCIENTIFIC PAPER

UDC 662.238.1:662.215-027.3

INFLUENCE OF THE OCTOGEN QUALITY AND PRODUCTION SCALE ON CHARACTERISTICS OF GRANULATED PLASTIC BONDED EXPLOSIVE

Article Highlights • Granulated PBX based on HMX and Estane prepared on a laboratory and industrial

scale was analyzed • Recycled and pure explosives were used for samples preparation • The observed properties of this military explosive qualified it for use in cumulative

warheads Abstract

The compositions of granulated plastic bonded explosive (PBX), based on octogen (HMX) and Estane polymer were prepared by aqueous/solvent slurry coating tehnique, on a laboratory and industrial scale. Scale-up was done in an environmentally friendly and cost-effective way: with provided recyclage and reuse of the used organic solvent. The quality of the obtained granulated PBX samples was observed trough the following analyses: the quality of poly-mer coating layer on HMX crystals was examined by microscopic analysis; the phlegmatizer content in PBX samples was determined; granulometric analysis and the tests of sensitivity to friction and impact were carried out. Compres-sibility of granulated PBX was determined by pressing. Measured detonation velocities of pressed PBX charges were compared. The obtained properties of the examined pressed PBX indicated that it may find application as a promis-ing main explosive charge in cumulative warheads.

Keywords: high explosives, granulated PBX processing, microscopic analysis, compressibility, detonation velocity.

Plastic bonded explosives (PBXs) are mixtures of explosive materials and polymer binders (phlegma-tizers). These explosive compositions are known to have high performance and low sensitivity to friction and impact. PBXs have been commonly used in both military and industry because of their improved safety, enhanced mechanical properties, and reduced vulner-ability during storage and transportation [1-4]. There are different types of PBXs and different technologies for their production: granulated PBX produced by water-slurry method and further processed by pres-

Correspondence: Z. Burzić, Military Technical Institute, Ratka Resanovića 1, 11000 Belgrade, Serbia. E-mail: zijah.burzic@vti.vs.rs Paper received: 21 September, 2018 Paper revised: 24 October, 2019 Paper accepted: 24 October, 2019

https://doi.org/10.2298/CICEQ180921035K

sing; cast-cured PBX; plastic-moldable PBX; extruded PBX, etc.

Granulated PBXs are crystalline high explosives coated by thermoplastic phlegmatizers (polymer bin-ders). Pressed PBXs are used as boosters and main charges in most modern warheads [5].

The laboratory production technology (product-ion batch mass from 50 g to 1 kg) of granulated PBX, labeled as FOP-5E (similar to LX-14) has been def-ined at the Military Technical Institute, Belgrade.The processing and compacting of PBX, as well as the characterisation of granulated PBX samples and pressed PBX charges were defined [6-10]. PBX com-positions obtained by this technology meet the quality requirements of the military standard [11]. Afterwards, the transfer of granulated PBX production technology to the industrial scale has been carried out - the ind-ustrial processing of PBX was implemented on the

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adapted technological line for the production of phleg-matized explosives [12].

This paper gives a brief overview of laboratory examinations and the process of defining the techno-logical parameters of industrial production of granul-ated PBX, and compares the characteristics of PBX samples produced on laboratory and industrial levels for granulated PBX, FOP-5E (95% HMX and 5% Est-ane). The aim of the presented examinations is the estimation of applicability of pressed FOP-5E as the main explosive charge in cumulative warheads.

EXPERIMENTAL

Laboratory production of granulated PBX

Production technology of granulated PBX is based on the precipitation of polymer phlegmatizer from a solution in organic solvent, and formation of a coating layer on the particle surface of the explosive. All the techniques for the production of granulated PBXs [13] are performed in the liquid phase (aqueous slurry of the cristalline explosive and solution of phlegmatizer in organic solvent) and for this reason named aqueous-slurry (or water-slurry) methods.

In this research, on a laboratory scale, PBX compositions were prepared by water-slurry phleg-matization technique, using the following raw mat-erials:

– The crystalline octogen (1,3,5,7-tetranitro- -1,3,5,7-tetrazocane), HMX (produced by Dyno Nobel Norway, type DYNO A/C), was used as the explosive component. Bulk density of used HMX was 1.003 g/cm3. The size range of 80% HMX crystals was 140– –560 μm.

– Estane (BF Goodrich Co.) was used as phleg-matizer. This thermoplastic polyuretane, i.e., poly-(ester-uretane)-copolymer, was chosen for the coat-ing process due to its excellent physical, chemical and mechanical characteristics, as well as excellent compatibility with explosives [14,15].

The defining of the explosive's coating tech-nique was started by the production of a laboratory batch, mass 50 g, in a glass reactor with a hot bath and a mechanical stirrer. The first step was the select-ion of the most suitable solvent for the polymer phleg-matizer. For Estane, the solvent of choice was methylethyl ketone, since the selected organic solvent must satisfy specific requirements, in order to be used in the coating process of the explosive [8]. Thus, Est-ane was dissolved in methylethyl ketone, and this solution was added to the aqueous slurry of the crys-talline octogen in a glass vessel reactor (volume 1 dm3). The suspension was heated in a water bath and

mixed with a propeller stirrer. The temperature of the suspension was maintained at constant value until evaporation of the complete content of the organic solvent, while forming a coating layer on the surface of the octogen particles.

The characterization results (given below in Results and discussion) for this small batch, denoted as Lot 50 g, showed that this granulated PBX compo-sition, based on octogen and polymer Estane, com-pletely meets quality requirements [11], so it was pro-ceeded with further work within this research.

PBX quality has been confirmed in larger labor-atory batches (mass up to 1 kg), denoted as Lot 1 kg. Laboratory equipment for processing larger PBX batches consisted of a double-jacket reactor (volume up to 10 dm3), propeller stirrer, ventilation system and filtering system.

Further on, this research was focused on inc-reasing the production batch of granulated PBX on an industrial level.

Industrial production of granulated PBX

The small capacity and lack of technical con-ditions for the recyclage of solvents after removal (evaporation) from the reactor (i.e., the impossibility of its reflux) were the most important disadvantages of the used laboratory equipment. This reflects both the economic and the environmental aspects of the prac-tical application of PBX processing technology. The solvent reflux has been introduced during the transfer of technology to industrial scale. At this level, PBX processing was carried out on an adapted industrial technological line, in a closed system with provided solvent reflux, so the production costs were reduced (recycled solvent can be used in the next PBX batch) [12]. Loss of the solvent was approximately 10%, but this amount is offset by the addition of fresh solvent in the next batch of PBX.

The following materials were used: – Recycled HMX (Prva Iskra Namenska - Barič,

Serbia), for Lot I. The size range of 90% HMX crystals was 75–500 μm.

– HMX, type DYNO class A/C, for Lot II (same as for laboratory PBX batches).

– Polyurethane elastomer Estane (same as for laboratory PBX batches).

Phlegmatizer solution was prepared in a double- -jacket reactor and after that was transfered to a dos-age reactor by a vacuum pump and pipe system. Fur-ther, 250-300 L of water and 50 kg of crystalline octo-gen were added, and the obtained aqueous suspen-sion of the crystalline octogen was continuously heated by technical steam through the jacket wall and

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mixed by a propeller stirrer. The phlegmatizer solution was dosed in a slow stream into the heated aqueous suspension of octogen. The adding started at a tem-perature of 50 °C and the total volume of phlegmat-izer solution was dosed over a period of 20 min. During this period the temperature was increased up to 70 °C. The solvent evaporating was carried out until the temperature of the suspension reached 100 °C. At the end of the coating process, the suspension was cooled to the temperature of 50-55 °C and trans-ferred to a filtering system where PBX granules were washed and decanted.

Methods of PBX characterization

The characterization of the components and PBX included the following tests:

– Analysis of the chemical composition accord-ing to [11]: the contents of polymer binder and HMX in PBX samples were determined.

- Analysis of the granulometric size on selected sieves (425, 600, 850, 1190 and 1600 μm), according to [16].

– Determination of bulk density, according to [16]. – Microscopic analysis of explosives samples

(used octogen crystals and obtained granulated PBXs) by Leica Stereo Microscope with digital cam-era Canon Power Shot S40.

– Analysis of thermal characteristics of compo-nents and granulated PBX samples, using a DSC Q20 differential scanning calorimeter, at a tempera-ture range from 20 °C to a maximum of 450 °C, with a 10 °C/min heating speed.

– Determination of the explosive’s sensitivity to friction and impact, on a Julius–Peters apparatus, according to [17,18]. The sensitivity of an explosive to impact and friction are among the most important characteristics regarding the safety in handling, trans-portation or processing. For both friction and impact sensitivity, the following principle applies: when the sensitivity of an explosive to impact stimuli is high, the impact energy needed for its activation is low, and when the sensitivity is lower, the explosive is resistant to higher values of impact energy. The sensitivity to impact stimuli is tested by a falling drop weight, and in this research, it was done using a weight of 2 kg falling from the height of 30 cm.

– Analysis of compressibility (change of explo-sive density as a function of the specific pressure). Pellets of PBX were pressed, for compressibility examination, in a cylindrical pressing tool (diameter 20 mm), at room temperature, without vacuum. The compressibility of explosives was examined by pres-sing the explosive samples (at constant mass) by

successive increases of specific pressure, from 960 to 4160 bar/cm2.

– Determination of detonation velocity and cal-culation of detonation pressures of pressed PBX. Detonation velocity (D) was measured in the zone of stable detonation of experimental models made of PBX pellets (Figure 1) pressed in a cylindrical pres-sing tool (diameter 20 mm) using optical probes with a photo-detector to register the arrival of the deton-ation wave front to two positions in the sample, at a defined distance. Data were acquired using the elec-tronic counter Pendulum CNT-91.

Figure 1. Experimental model for detonation velocity

measurement and pressed PBX pellets.

Detonation pressures of pressed PBXs are cal-culated by the equations based on the experimental values of detonation velocity and explosive density, according to known methodology [9].

RESULTS AND DISCUSSIONS

Characteristics of PBX granules

The values of bulk density, chemical compo-sition and sensitivity to friction and impact of different production batches (Lots) of explosive FOP-5E are presented in Table 1.

The content of Estane in FOP-5E Lot II 50 kg was slightly higher (5.6%) than the designed value (5.0±0.5%), but the result for FOP-5E Lot I 50 kg was regular (Table 1).The values of bulk density of both industrial batches are in accordance with the standard values for the similar phlegmatized explosive compo-sitions (≥1.70 g/cm3) and suitable for pressing.

Results of the tests of sensitivity to friction and impact are given in Table 1 and compared to sensi-tivity of neat HMX crystals. In our tests, the obtained sensitivity of octogen crystals to friction was 128 N, and sensitivity to impact was 2 J. According to some literature sources, the results may vary. For example, it has been reported that impact sensitivity for HMX is about 6.37 J [19], but the results from different testing

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procedures vary a lot because of different testing methods or used equipment. However, in our com-parison, the results were obtained using the same testing procedure and applying the same loads on all the observed samples. The registered higher values of friction and impact energy needed to activate the phlegmatized explosive confirm that it is less sensitive than pure HMX, for which lower energies were regis-tered to initiate activation.

The presence of Estane in FOP-5E samples caused the reduction of their sensitivity to friction and impact compared to the sensitivity of the neat octogen with exposed crystal edges. The sensitivity to friction and impact of industrially obtained FOP-5E granules were at approximately the same level of sensitivity as those of laboratory-obtained FOP-5E samples (Lot 50 g and Lot 1 kg).

Microscopic analysis of explosives

Microscopic analysis was used to estimate the quality of the granulated PBX samples (coating effect-iveness). Microscopic photographs are presented in Figures 2 and 3 (octogen crystals and PBX granules).

Optical microscopy of industrially obtained FOP- -5E granules (Figure 3c and d) has shown that octo-gen crystals were uniformly coated with polymer mat-erial, same as in the case of the samples obtained in the laboratory (Figure 3a and b). The results of par-ticle size distribution (proportion of explosives that remains on the selected sieves) of the laboratory and industrial FOP-5E batches are presented in Table 2.

Figure 3. Samples: a) FOP-5E Lot 50 g; b) FOP-5E Lot 1 kg; c)

FOP-5E Lot I 50 kg; d) FOP-5E Lot II 50 kg.

The largest mass content of the granules of FOP-5E in case of the laboratory-obtained Lot 50 g and Lot 1 kg was observed for sieve fraction of 420 μm - 800 μm, while granules of industrially manufac-tured Lot I 50 kg and Lot II 50 kg are quite smaller (the largest fraction of 315–600 μm). This may be a consequence of the mixing regime, the different cons-truction of the propeller, as well as the total amount of the suspension.

Thermal analysis of explosives

Diagrams displayed in Figure 4 show the DSC curves of two used specimens of crystalline octogen.

Table 1. Characteristics of laboratory and industrial batches (Lots) of FOP-5E compared to HMX

Characteristic Lot 50 g Lot 1 kg Lot I 50 kg Lot II 50 kg HMX

Content of octogen (wt.%) 94.92 94.65 95.25 94.40 100

Content of Estane (wt.%) 5.08 5.35 4.75 5.60 -

Bulk density (g/cm3) 0.803 0.767 0.930 0.813 1.003

Sensitiveness to friction (N) 216 240 - 216 128

Sensitiveness to impact (J) 5 6.5 - 6 2

Microscopic analysis, Figure 3a 3b 3c 3d 2

Figure 2. a) Crystals of HMX DINO A/C; b) crystals of recycled HMX, PIN.

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The results of thermal analysis of FOP-5E Lot 1 kg, FOP-5E Lot I 50 kg and FOP-5E Lot II 50 kg are presented in Figure 5.

According to thermo-chemical analysis results, two specimens of crystalline octogen have very similar characteristics of DSC peaks, as well as two lots of FOP-5E. The presence of the polymeric phlegmatizer,

Estane, reduces the degradation temperature of the FOP-5E samples relative to the crystalline octogen by 4-6 °C. It can also be concluded that there are no major differences in the values of the characteristic temperatures of the laboratory-made FOP-5E batch Lot 1 kg and industrially produced FOP-5E batches, Lot I 50 kg and Lot II 50 kg (Figure 5). It is interesting

Table 2. Particle size distribution of the examined batches of FOP-5E

Sieve size/Particle size, μm Remaining explosive granules on the sieve, mass%

Lot 50 g Lot 1 kg Lot I 50 kg Lot II 50 kg

1600 0 0 0 0.15

1190 0.04 0.2 0.3 0.3

800 3.6 6.3 4.1 19.1

600 55.36 74.15 6.7 31

420 37.1 18.25 63.84 44.6

315 6.9 1.2 21.1 3.64

0 1 0 1 0

Figure 4. DSC curve of: a)HMX DINO A/C; b)recycled HMX, PIN.

Figure 5. DSC curves of FOP-5E: Lot 1 kg, Lot I 50 kg and Lot II 50 kg.

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to observe that the obtained DSC results are match-ing for the different batches although the size of the granules was not the same, neither was the content of the phlegmatizer identical. Decomposition tempera-tures of industrial and laboratory-produced PBXs based on HMX DINO A/C (278.65 °C for FOP-5E, Lot II 50 kg and 279.04 °C for FOP-5E, Lot 1 kg) differ only by 0.4 °C. This means that regardless of these differences, the thermal stability of HMX in all the batches was successfully enhanced by the phlegmat-ization with Estane.

Compressibility

Compressibility of PBXs was tested by pressing on vertical hydraulic presses. Values of specific pressure were increased successively until a „plateau“ effect of the compressibility curve was achieved. Compressibility curves for FOP-5E are pre-sented in Figure 6.

Figure 6. Compressibility of FOP-5E.

All lots of FOP-5E showed good compressibility characteristics and pressed explosive pellets were easily taken out from the pressing tool. They were well-pressed at low specific pressures and the „plateau“ effect was achieved with very low specific pressures. On the graphic display of the results we

can see how achieved PBX densities („plateau“ of compressibility curves) are „far“ from their theoretical maximal densities (TMD).

Detonation velocity and pressure of detonation

The values of experimentally determined deton-ation velocities and calculated values of detonation pressure (Pd) as functions of explosive charge density (ρ) are given in Table 3.

Analysis of the results shows that laboratory and industrial lots of FOP-5E pressed to the similar den-sity have very similar values of detonation velocity. This means that the scale-up was performed suc-cessfuly, and that the obtained explosive from all the batches has good detonation properties. By com-paring the results of the examined explosive with the known results for explosive composition HMX/Estane 95/5, it was concluded that the values of the para-meters of detonation of tested explosives are in accordance with the literature data (for 1.86 g/cm3 density of this explosive D = 8600 m/s) [20,21].

CONCLUSIONS

The parameters of octogen phlegmatization with 5% Estane by water-slurry process were defined. The industrial processing equipment was adapted and the PBX production technology was transferred to the industrial scale. The solvent used, methylethyl ket-one, was recycled during industrial production. This reduced PBX production cost, maintaining production safety and environmental protection.

Microscopic analysis showed that industrially produced PBX batches were well phlegmatized. The increased mass of production batch did not affect the quality of PBX. The results of comparative character-ization of laboratory- and industrially produced PBX (bulk density, chemical composition, sensitivity to fric-tion and impact, compressibility, DSC thermograms, and detonation velocity) showed that the quality of

Table 3. Detonation parameters of laboratory and industrial batches (Lots) of FOP-5E

FOP-5E Nominal charge density

ρ / g cm–3 Practical value of TMD

% Detonation velocity

D / m s–1 Detonation pressure

Pd / kbar

Lot 1 kg 1.72 93.07 8373.5 301.5

1.76 95.45 8508.3 318.5

1.79 97.54 8600.3 329.1

Lot I 50 kg 1.72 93.57 8382.7 302.8

1.76 95.90 8539.2 322.1

1.79 97.67 8652.7 336.9

Lot II 50 kg 1.72 93.48 8328.4 298.8

1.76 95.69 8489.9 317.7

1.79 97.09 8579.5 329.4

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industrially obtained PBX samples were similar to laboratory batches. Thermal properties of the tested explosive encourage further examinations in different testing regimes in order to be sure that FOP-5E will have good stability in aging during enough time so this explosive could be considered for cumulative warheads for military purposes. The values of the parameters of detonation of tested FOP-5E were in accordance with the literature data for similar explo-sive compositions.

Based on these results it can be concluded that the quality of industrially produced lots are on the same quality and performance levels as laboratory lots. Also, recycled HMX was shown to have good qualities in comparison to HMX DINO A/C.

Good properties of industrially produced FOP-5E qualified this explosive for use in military pur-poses, as a shaped charge in cumulative warheads.

REFERENCES

[1] A.S. Cumming, Propellants Explos. Pyrotech. 24 (1999) 46-49

[2] J. Mathieu, H. Stucki, Chimia 58 (2004) 383-389

[3] A. Cumming, J. Aerosp. Technol. Manage. 1 (2009) 161- –165

[4] J.P. Agrawal, Propellants Explos. Pyrotech. 30 (2005) 316-328

[5] J. Corleone, Tactical Missile Warheads, Aeroyet General Corporation, California, 1993, pp. 81–156

[6] S. Terzić, M. Šestović, Flegmatizacija oktogena sa termo-plastičnim polimerom, in Proceedings of OTEH 2005, Belgrade, Serbia, 2005, рp. IV-22-IV-27 (in Serbian)

[7] S. Terzić, Z. Borković, Izrada i karakterizacija granuli-sanog PBX na bazi oktogena i termoplastičnog flegma-tizatora, in Proceedings of OTEH 2007, Belgrade, Serbia, 2007, рp. III-9-III-13 (in Serbian)

[8] S. Terzić, Sci. Techn. Rev. 62 (2007) 34-38

[9] S. Terzić, V. Džingalašević, Z. Borković, Eksplozivne karakteristike presovanog PBX na bazi oktogena i termo-plastičnog flegmatizatora, in Proceedings of OTEH 2009, Belgrade, Serbia, 2009, pp. 341-346 (in Serbian)

[10] S. Terzić, V. Džingalašević, Z. Borković, Plastic Bonded Explosives based on Octogen and Estane, in Pro-ceedings of OTEH 2011, Belgrade, Serbia, 2011, pp. 319-323

[11] MIL-H-48358(AR) Military specification HMX/resin explo-sive composition LX-14-0, 1980

[12] S. Terzić, S. Biočanin, A. Đorđević, Ž. Krstić, B. Kostadi-nović, Z. Borković, Transfer of granulated PBX production to thе industrial scale, in Proceedings of OTEH 2016, Belgrade, Serbia, 2016, pp. 297-303

[13] U. Teipel, Energetic Materials: Particle processing and characterization, WILEY-VCH, Weinheim, 2005, pp. 188- –208

[14] X. Shi, J. Wang, X. Li, C. An, Cent. Eur. J. Energy Mater. 11 (2014) 433-442

[15] T. Hongxiang, Appl. Sci. 2 (2012) 496-512

[16] SORS8457/97, Metode kontrolisanja brizantnih eksplo-ziva, 1997, Serbian Military Standard (in Serbian)

[17] EN 13631-4, Explosives for civil uses – High explosives - Part 4: Determination of sensitiveness to impact of explosives, 2002

[18] EN 13631-3, Explosives for civil uses – High explosives - Part 3: Determination of sensitiveness to friction of explosives, 2002

[19] C.B. Storm, J.R. Stine, J.F. Kramer, Sensitivity Relation-ships in Energetic Materials, in Chemistry and Physics of Energetic Materials, S.N. Bulusu (Ed.), Kluwer Acad. Pub., Dordrecht, 1990, p. 605

[20] R. Meyer, J Kohler, A. Homburg, Explosives, Wiley-VCH, Weinheim, 2007, p. 224

[21] Ј.P. Agrawal, High Energy Materials: Propellents, Explo-sives and Pyrotehnics, WILEY-VCH, Weinheim, 2010, p. 175.

HICHAM KEMMOUKHE1 UTICAJ KVALITETA OKTOGENA I NIVOA

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SLAVICA TERZIĆ2 MIRJANA DIMIĆ2

DANICA SIMIĆ2 ZIJAH BURZIĆ2

LJILJANA JELISAVAC2 1Vojna akademija, Univerzitet odbrane,

Pavla Jurišića Šturma 1, 11000 Beograd, Srbija

2Vojnotehnički institut, Ratka Resanovića 1, 11000 Beograd, Srbija

NAUČNI RAD

PROIZVODNJE NA KARAKTERISTIKE GRANULISANOG PBX EKSPLOZIVA

Sastavi granulisanog PBX (Plastic Bonded eXplosive), na bazi oktogena (HMX) i poli-mera Estana, pripremlјeni su tehnikom prevlačenja u smeši vode i rastvarača na labora-torijskom i industrijskom nivou. Podizanje na industrijski nivo je izvršeno na ekološki pri-hvatlјiv i ekonomičan način: uz obezbeđenu reciklažu i ponovnu upotrebu korišćenog organskog rastvarača. Kvalitet dobijenih granulisanih uzoraka PBX praćen je sledećim analizama: kvalitet sloja prevlake polimera na kristalima HMX je ispitan mikroskopskom analizom; utvrđen je sadržaj flegmatizatora u uzorcima PBX; izvršena je granulomet-rijska analiza i testovi osetlјivosti na trenje i udar. Kompresibilnost granulisanog PBX je određena presovanjem. Upoređene su izmerene brzine detonacije presovanih PBX pu-njenja. Dobijena svojstva ispitanih presovanih PBX ukazuju na to da on može naći pri-menu kao obećavajuće glavno eksplozivno punjenje u kumulativnim bojevim glavama.

Ključne reči: brizantni eksploziv, prerada granulisanog PBX, mikroskopska analiza, kompresibilnost, brzina detonacije.