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Foodstuffs and cellulosic materials, Coarse samples, Corrosive samples – Parr Instrument 1108 User Manual

Page 9: Liquid samples, Gelatin capsules, 1108 oxygen combustion vessel

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1108 Oxygen Combustion Vessel

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9

way to destroy any trace of carbon or combustible

matter which might remain in the capsule from a

previous test. After heating, place the capsules in a

clean container and handle them only with forceps

when they are removed to be weighed on an ana-

lytical balance.

Capsules should be monitored for wear. Do not use

the capsule if the wall or base thickness is less than

0.025”.

Foodstuffs and Cellulosic Materials

Fibrous and fluffy materials such as vegetable fibers

may have to be packed into the combustion capsule

and moistened to slow the burning rate, but food-

stuffs and cellulosic samples generally burn with

little difficulty. Partial drying may be necessary if the

moisture content is too high to obtain ignition. But

if the sample is heat sensitive and cannot be dried,

a water soluble combustion aid such as ethylene

glycol can be added to promote ignition.

Coarse Samples

In most cases it may be necessary to burn coarse

samples without size reduction since grinding or

drying may introduce unwanted changes. There is

no objection to this if the coarse sample will ig-

nite and burn completely. Whole wheat grains and

coarse charcoal chunks are typical of materials

which will burn satisfactorily without grinding and

with no additives or special procedure.

Corrosive Samples

Although the Parr Oxygen Combustion Vessel is

made of corrosion resistant alloys, repeated use

with high sulfur samples or with samples contain-

ing over 20 mg of chlorine may corrode the metal

surfaces and produce a dull film on the inner walls

of the bomb. Materials containing appreciable

amounts of caustic; such as dried black liquor from

a pulp mill, may also damage the bomb, with the

caustic attacking the alloy capsule and causing the

metal capsule and the bomb electrodes to ignite and

burn. These corrosive attacks on the bomb can be

reduced by using smaller samples and by increas-

ing the amount of liquid placed in the bottom of

the bomb. If a corrosive film develops on the bomb

surfaces it should be removed by proper polishing

before it grows to a point where deep pitting occurs.

Liquid Samples

Non-volatile samples are treated in the same man-

ner as solid materials. Oils and other liquids which

are not volatile at room temperature can be weighed

directly into open combustion capsules. The loop of

the fuse should be positioned just slightly above the

surface of the sample. Some operators place one

end of a short piece of fine cotton thread over the

fuse loop, with the other end touching the liquid. In

any case, the wire itself should not be submerged in

the liquid.

Gelatin Capsules

Volatile liquid samples to be burned in an oxygen

bomb can be handled conveniently in Parr 3601

Gelatin Capsules. These 0.9 mL capsules consist of

two cups which telescope together with a friction fit

adequate to retain most liquids. Corrections must

be made for the heat of combustion of gelatin (ap-

proximately 4600 cal/g) if the capsules are used for

43A6 Combustion Capsule with

Adhesive Tape Seal

3601 Gelatin Capsules

43AS Combustion Capsules