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BaCrO 4

90

560 (29.5 ml per

oxidizers. The low temperatures shown for potassium chlorate B

10

gram of evolved

and potassium nitrate may well account for the large number of Vinyl alcohol/

1 (additional %)

gas)

mysterious, accidental ignitions that have occurred with compo-acetate resin

sitions containing these materials.

Ease of initiation also depends upon the particle size and sur-IIIA. NaNO 3

50

772b (50 mg sam-

face area of the ingredients. This factor is especially important Ti

50

ple, heated at

for the metallic fuels with melting point higher than or comparable 50°C/min.)

to that of the oxidizer. Some metals - including aluminum, magnesium, titanium, and zirconium - can be quite hazardous when IIIB. NaNO 3

50

357

present in fine particle size (in the 1-5 micrometer range). ParTi

50

ticles this fine may spontaneously ignite in air, and are quite Boiled linseed

6 (additional %)

sensitive to static discharge [4]. For safety reasons, reactiv-oil

ity is sacrificed to some extent when metal powders are part of a mixture, and larger particle sizes are used to minimize accidental ignition.

aReference 10.

Several examples will be given to illustrate these principles.

bReference 2.

In the potassium nitrate/sulfur system, the liquid state initially appears during heating with the melting of sulfur at 119°C. Sulfur occurs in nature as an 8-member ring - the S a molecule. This ring begins to fragment into species such as S 3 at temperatures above 140°C. However, even with these fragments present, re-Once sufficient heat is generated to begin decomposing the ox-action between sulfur and the solid KNO

idizer, the higher-temperature combustion reaction begins, in-3 does not occur at a

volving free oxygen gas and very rapid rates. We are concerned rate sufficient to produce ignition until the KNO 3 melts at 334°C.

Intimate mixing can occur when both species are in the liquid here with the processes that initiate the ignition process.

Professor G. Tammann, one of the pioneers of solid-state chem-state, and ignition is observed just above the KNO 3 melting point.

istry, considered the importance of lattice motion to reactivity, Although some reaction presumably occurs between sulfur and

102

Chemistry of Pyrotechnics

Ignition and Propagation

103

TABLE 5.2 Tammann Temperatures of the Common Oxidizers Melting

Melting

Tammann

point,

point,

temperature,

Oxidizer

Formula

°C

°K

°C

Sodium nitrate

NaN0 3

307

580

17

Potassium nitrate

KNO 3

334

607

31

Potassium chlorate

KC1O 3

356

629

42

Strontium nitrate

Sr(NO 3) 2

570

843

149

Barium nitrate

Ba(N0 3 ) 2

592

865

160

Potassium perchlorate

KC10 4

610

883

168

Lead chromate

PbCr0 4

844

1117

286

Iron oxide

Fe 2 0 3

1565

1838

646

FIG. 5.2 Thermogram of pure potassium nitrate. Endotherms are observed near 130° and 334°C. These peaks correspond to a solid KNO 3 below the melting point, the low heat output obtained rhombic-to-trigonal crystalline phase transition and melting. Note from the oxidation of sulfur combined with the endothermic de-the sharpness of the melting point endotherm near 334°C. Pure composition of KNO B prevent ignition from taking place until the compounds will normally melt over a very narrow range. Impure entire system is liquid.

Only then is the reaction rate great

compounds will have a broad melting point endotherm.

enough to produce a self-propagating reaction. Figures 5.2-5.4

show the thermograms of the components and the mixture. Note the strong exotherm corresponding to ignition for the KNO 3 /S

mixture.

In the potassium chlorate /sulfur system, a different result is generating oxygen to react with additional sulfur.

More heat is

observed. Sulfur again melts at 119°C and begins to fragment generated and an Arrhenius-type rate acceleration occurs, lead-above 140°C, but a strong exotherm corresponding to ignition of ing to ignition well below the melting point of the oxidizer. This the composition is found well below 200°C! Potassium chlorate combination of low Tammann temperature and exothermic decomposition helps account for the dangerous and unpredictable na-has a melting point of 356 11 C, so ignition is taking place well below the melting point of the oxidizer. We recall, though, that ture of potassium chlorate. Figures 5.5-5.6 show the thermal KC1O

behavior of the KC1O 3 /S system.

3 has a Tammann temperature of 42 1 C.

A mobile species --

such as liquid, fragmented sulfur - can penetrate the lattice As we proceed to higher-melting fuels and oxidizers, we see well below the melting point and be in position to react. We also a corresponding increase in the ignition temperatures of two-component mixtures containing these materials. The lowest ig-recall that the thermal decomposition of KC1O 3 is exothermic (10.6

nition temperatures are associated with combinations of low-melt-kcal of heat is evolved per mole of oxidizer that decomposes). A compounding of heat evolution is obtained -- heat is released by ing fuels and low-melting oxidizers, while high-melting combinations generally display higher ignition points. Table 5.3 gives the KC1O 3 /S reaction and by the decomposition of additional KC1O 3

some examples of this principle.

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Chemistry

Ignition

of Pyrotechnics

and Propagation

105

100

200

300

400

500

REFERENCE TEMPERATURE, "C

FIG. 5.4 The potassium nitrate /sulfur /aluminum system. Endo-FIG. 5.3 A sulfur thermogram. Endotherms for a rhombic-to-therms for sulfur can be seen near 105° and 119 1C, followed by monoclinic crystalline phase transition and melting are seen at the potassium nitrate phase transition near 130 1C. As the melt-105° and 119°C, respectively. An additional endotherm is ob-ing point of potassium nitrate is approached (334 1 C), an exo-served near 180°. This peak corresponds to the fragmentation therm is observed. A reaction has occurred between the oxidizer of liquid S

and fuel, and ignition of the mixture evolves a substantial amount 8 molecules into smaller units. Finally, vaporization is observed near 450°C.

of heat.

of components, degree of mixing, loading pressure (if any), heat -

ingrate, and quantity of sample can all influence the observed Table 5. 3 shows that several potassium nitrate mixtures with ignition temperature.

low-melting fuels have ignition temperatures near the 334°C melt-The traditional method for measuring ignition temperatures, ing point of the oxidizer. Mixtures of KNO 3 with higher-melting used extensively by Henkin and McGill in their classic studies metal fuels show substantially higher ignition temperatures.

of the ignition of explosives [6] , consists of placing small quan-Table 5. 4 shows that a variety of magnesium-containing compo-tities (3 or 25 milligrams, depending on whether the material sitions have ignition temperatures close to the 649°C melting detonates or deflagrates) of composition in a constant-tempera-point of the metal.

ture bath and measuring the time required for ignition to occur.

A problem with trying to develop logical theory using litera-Ignition temperature is defined, using this technique, as the ture values of ignition temperatures is the substantial variation temperature at which ignition will occur within five seconds.