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No.

207M

Analytical Methods for Oxygen Bombs

Combustion with oxygen in a sealed Parr bomb has with a fluted watch glass and keep just below boiling
been accepted for many years as a standard on a steam bath or hot plate until the volume is
procedure for converting solid and liquid combustible reduced to 75 ml, then allow the precipitate to settle
samples into soluble forms ready for chemical for another hour while cooling. Filter through an
analysis. It is a reliable whose effectiveness stems ashless filter paper and wash with warm water until
from its ability to treat samples quickly and free from chlorides.
conveniently within a closed system, thus ensuring
complete retention and potential recovery of all Transfer the paper and precipitate to a weighed
combustion products. The bomb combustion method crucible, dry at low heat, char the paper without
is an essential step is standard ANSI/ASTM methods flaming, then raise the temperature to a good red
for determining sulfur and chlorine in coal, and it has heat (approximately 925 °C) and heat to a constant
been applied successfully to the determination of weight. If the crucible is placed in a cold electric
arsenic, phosphorus and other elements as well. muffle furnace and the current turned on, drying,
charring and ignition will usually occur at the desired
The methods given here for sulfur and chlorine rate. After ignition is complete, allow the crucible to
correspond to the basic ASTM reference methods for cool to room temperature and weigh. Determine the
these elements, each of which calls for a gravimetric exact weight of the barium sulfate precipitate and
finish. Although these are reliable procedures, other calculate the percentage of sulfur in the sample as
less time consuming volumetric, nephelometric or ion follows:
chromatographic methods can be used for estimating
these elements after recovering the bomb washings. Sulfur, % = Wt. BaSO4 X 13.734
Such alternatives are suggested in the references Wt. Sample
which follow.
Sulfur in Combustible Liquids. For oils or other
Sulfur in Combustible Solids. Burn a 1.0 gram liquids containing 5% sulfur or less, use a sample
sample and collect the washings as described in the weighing from 0.6 to 0.8 gram. If the sample
basic procedure for using the 1108 oxygen bomb. contains over 5% sulfur, use a sample weighing from
Let the bomb stand for at least 5 minutes after firing; 0.3 to 0.4 gram and add an equal amount of sulfur-
then remove it from the water and release the free U.S.P. white oil. If the sample is not readily
residual gases slowly and at an even rate so that the miscible with white oil, some other low sulfur
pressure is reduced to atmospheric in not less than combustible diluent may be used. However, the
one minute. Open the bomb and wash all parts of its combined weight of sample and white oil or other
interior, including the combustion capsule, valve combustion aid must not exceed 1.0 gram. If the
passages and electrodes, with a fine jet of distilled sample is volatile it must be weighed in a sealed
water containing 1 ml of a saturated solution of holder.
methyl orange indicator per liter. Wash until no acid
reaction is observed, collecting the washings in a The procedure for filling the bomb, firing, recovering
beaker. If necessary, use a rubber policeman to the washings and determining sulfates is the same
transfer any precipitate from the bomb or capsule to for liquid samples as described in the preceding
the beaker. method for solids.

After neutralizing the solution, add 1 ml of ammonium Other less time consuming procedures have been
hydroxide, heat the solution to boiling, and filter suggested as an alternative to the gravimetric
through a rapid qualitative paper. Wash the residue methods described here for estimating sulfur in the
and filter paper with hot distilled water and add bomb washings. Among the titrimetric methods:
sufficient water to bring the total volume of solution to Hicks21, et al titrates with lead perchlorate and
approximately 250 ml. Neutralize with concentrated determines the equivalence point using a lead ion
hydrochloric acid and add 2 ml in excess. Add 10 ml specific electrode. Callan11 suggests converting to
of saturated bromine water and evaporate to benzadine sulfate and titrating with standard
approximately 200 ml on a hot plate or other source hydroxide solution. Siegfriedt41 titrates with barium
of heat. Adjust to a slow boil and stir constantly while chloride solution using tetra-hydroxyquinone as an
adding 10 ml of a 10% barium chloride solution from indicator. Randall37 adds barium chloride in excess
a pipette. Continue stirring for two minutes, cover and back titrates with disodium hydrogen phosphate
with the addition of alcohol. Herrig20 back titrates 600 ml beaker. Scrub the interior of the cylinder and
with Tritiplex III using phthalein purple as an the underside of the head with a rubber policeman.
indicator. A conductometric method has been Continue washing until no acid reaction is observed
suggested by Barthel6. Nephelometric methods for on any bomb parts or passages, which will normally
trace amounts of sulfate have been suggested by require at least 300 ml of wash water.
Toennies43 and Bailey5.
Acidify the solution by adding 1:1 nitric acid dropwise
Chlorine in Combustible Solids and Liquids. until the methyl red endpoint is observed; then add 2
Platinum combustion capsules and platinum ignition ml excess acid. Filter through a qualitative paper and
wire are recommended for these tests because of the collect the filtrate in a 600 ml beaker. Heat to about
extremely corrosive nature of chlorine and its 60 °C; protect from strong light and slowly add 5 ml of
compounds. After repeated use with such samples, silver nitrate solution (50 g per liter) while stirring.
the inner surfaces of the bomb will become etched to Heat almost to boiling and hold at this temperature
the point where appreciable amounts of metal salts until the supernatant liquid becomes clear. Add a few
will be introduced during each combustion. The drop of silver nitrate solution to test for complete
ability of the bomb to withstand such corrosion can precipitation. If cloudiness appears, repeat the above
be improved by keeping the inner surfaces highly operation.
polished. Any bomb which is being used for chlorine
determinations should be repolished at regular Allow the beaker to stand in a dark place for at least
intervals to prevent the development of deep pits. one hour. Filter the precipitate by suction onto a
The alternative to this procedure is to use an 1108CL weighed fritted glass filter. Wash with distilled water
bomb which offers much better resistance to chlorine containing 2 ml of 1:1 nitric acid per liter. Dry the
than the standard 1108 bomb. Or for ultimate precipitate and crucible at 110 °C for one hour. Cool
protection, use an 1105C or 1106C bomb with a in a desiccator and weigh.
platinum liner.
Make a blank determination with 0.7 to 0.8 gram of
Samples containing more than 2% chlorine by weight white oil, omitting the sample; then calculate the
should be diluted with U.S.P. white oil or some other chlorine content of the sample by substituting in the
non-volatile, chlorine-free diluent. The suggested following equation:
amounts of sample and diluent are shown in the
following table, but the user is cautioned that the Chlorine, % by wt. = (P-B) 24.74
combined weight of the charge must not exceed 1.0 m
gram. where,
P = grams AgCl obtained from sample
% Chlorine Grams of Grams of B = grams AgCl obtained from blank
in Sample Sample White Oil m = mass of sample in grams
Below 2 0.8 0.0
2 to 5 0.4 0.4 ASTM Methods for Sulfur and Chlorine. Oxygen
5 to 10 0.2 0.6 bomb procedures for determining sulfur and chlorine
10 to 20 0.1 0.7 in a broad range of combustible materials are given
20 to 50 0.05 0.7 in the following standard methods published by the
American Society for Testing and Materials, copies
Place about 5 ml of a 5% sodium carbonate solution can be obtained from ASTM at 1916 Race Street,
(135g Na2CO310H2O per liter) in the bomb, assemble Philadelphia, PA. 19103.
and fill with oxygen to a pressure of 35 atmospheres.
Immerse the bomb in a bath through which cold ASTM Method D129-91, “Standard Test Method for
water is circulating. Attach the ignition wire to the Sulfur in Petroleum Products (General Bomb
bomb terminal, then stand at least six feet from the Method)”.
bath when firing the charge. Keep the bomb in the
bath at least five minutes before removal. Release ASTM Method D3177-89, “Standard Test Method for
the residual gas slowly and at an even rate so that Total Sulfur in the Analysis Sample of Coal and
the pressure is reduced to atmospheric in not less Coke”.
than one minute. Open the bomb and examine for
traces of unburned sample or sooty deposits. If ASTM Method D2361-91, “Standard Test Method for
found, discard the determination and clean the bomb Chlorine in Coal”.
thoroughly before using it again.
ASTM Method D1619-88, “Standard Test Method for
If the combustion was satisfactory, wash the sample Sulfur in Carbon Black”.
cup and all interior surfaces of the bomb with a fine
stream of distilled water, collecting the washings in a
2
ASTM Method D808-91, “Standard Test Method for oxygen bomb replaces the acid digestion generally
Chlorine in New and Used Petroleum Products used in the standard methods for arsenic.
(Bomb Method)”.
Mercury Determinations. Borchardt7 used an
ASTM Method D1847-87, “Standard Test Method for oxygen bomb to determine mercury in paper. Fujita17
Total Chlorine Content of Epoxy Resins”. determined mercury in rice, rice hulls and hair, while
Ukita44 used the bomb method for mercury
ASTM Method D3684-78, (1988) “Standard Test determinations using atomic absorption spectrometry
Method for Total Mercury in Coal by the Oxygen for the final measurement.
Bomb Combustion/Atomic Absorption Method”.
Phosphorus Determinations. Oxygen bomb
ASTM Method D3761-91, “Standard Test Method for methods for determining phosphorus have been
Total Fluorine in Coal by the Oxygen Combustion/Ion given by Piercy35, Conrad13, Wreath47, and Buss10.
Selective Electrode Method”. One problem associated with this determination is the
formation of a phosphoric acid mist in the bomb
ASTM Method D4208-88, “Standard Test Method for which does not settle out after combustion. To
Total Chlorine in Coal by the Oxygen Combustion/Ion dissipate the mist, apply 20 v.d.c. to the electrodes.
Selective Electrode Method”. To minimize the formation of phosphoric acid mist,
add one gram of sodium carbonate to the sample,
ASTM Method E144-64, (1992), “Standard mix some sodium naphthenate or zinc oxide with the
Recommended Practice for Safe Use of Oxygen sample.
Combustion Bombs”.
Boron Determinations. An oxygen bomb technique
ASTM Method E775-87, “Standard Test Methods for suggested by Hill22 has been found excellent for the
Total Sulfur in the Analysis Sample of Refuse- destruction of animal and vegetable tissue
Derived Fuel”. preparatory to chemical analysis. A similar technique
for the analysis of blood samples has also been
ASTM Method E776-87, “Standard Test Method for recommended23. This procedure has been used
forms of Chlorine in Refuse-Derived Fuel”. successfully for determining small amounts of boron
in animal and vegetable matter, and it seems
ASTM Method E926-88, “Standard Test Method of reasonable to assume that it would work equally well
Preparing Refuse-Derived Fuel (RDF) Samples for for determining other elements. Burke9, Conrad13,14
Analysis of Metals”. and Kuck27 also describe methods for determining
boron after combustion in an oxygen bomb.
Halogen Determinations. Other halogens in
addition to chlorine can be determined by the oxygen Other Elements. Selenium, Zinc, Lead, Titanium,
bomb method. Agruss3 used the oxygen bomb to Iron, Sodium, Potassium, Calcium, Magnesium,
determine chlorine, bromine and iodine mineral oils. Copper, Carbon, Hydrogen, Oxygen, Tritium,
Longo30 applied this method to many different organic Beryllium, Chromium, Manganese, Nickel, Vanadium
compounds, with particular emphasis on the and Carbon-14, all can be determined by oxygen
determination of iodine. Intonti25 used an oxygen bomb methods.
bomb for analyzing insecticides and
antifermentatives. Bradford8 describes a bomb Selenium has been determined in solid wastes by
method for determining fluorine in coal. Bailey5 and Johnson26 and in plant and animal tissue by Dye15.
Selig38,39 describe the use of platinum lined bomb for
determining fluorine. The Monsanto Co. 32 uses the Zinc in rubber and copper in mushrooms has been
oxygen bomb combustion method for determining reported by Przybylski36. Edwards16 has sodium,
small amounts of pentachlorophenol and similar potassium, calcium and magnesium in fuels.
chlorophenols in wall board, wood, paperboard, fish Fujiwara18 describes methods for determining iron,
net, rubber etc. Recently, Nadkarni34 has used aluminum and titanium in polyethylene, and Anduze4
halogen selective electrodes to determine fluorine, on titanium in polyethylene. Lead in piston deposits
chlorine, bromine and iodine in coal samples and has been determined by Conrad13. Lead in coal has
polymers after combustion in an oxygen bomb. been determined by Lindahl29.

Arsenic Determinations. It has been shown by Carbon determinations by the oxygen bomb method
Carey12 that combustion in an oxygen bomb is a have been reported by Adam1,2, Lambris28,
reliable way of preparing samples for the Thomas42, Mehta31 and Nishioka33. Hydrogen has
determination of arsenic by the Gutzeit method, or by been determined by Mehta31 and Nishioka33 and
the Marsh-Berzelius method. In this application the Zhokovskay48. The use of two bombs for determining
oxygen is described by Witaker46.
3
Nadkarni34 has determined nitrogen in coal samples Lindahl29 describes a particularly useful method for
using a chemiluminescent method following the determination of beryllium, chromium,
combustion in an oxygen bomb. This method is manganese, nickel, vanadium, copper, lead and zinc
much faster than the traditional Kjeldahl method, in coal.
requiring only a minute to determine nitrogen
concentration. A procedures manual issued by the U.S.
Environmental Protection Agency recommends
A method for determining H3 and C14 in biological combustion in a Parr Oxygen Bomb for preparing all
materials is described by Sheppard40. combustible materials for inorganic analysis. Specific
procedures are given for mercury, antimony and
Fujiwara19 gives an excellent review of methods for arsenic.
determining trace elements in organic compounds by
the oxygen bomb method.

PROCEDURES FOR DETERMINING TRACE LINDAHL PROCEDURES FOR TRACE


ELEMENTS USING A QUARTZ LINER IN ELEMENTS IN COAL
THE 1108 OXYGEN BOMB
Extensive studies by Peter C. Lindahl29 of the Exxon
Trace amounts of heavy metals in coal and other Production Research Company have shown that a
combustible samples can be determined by the bomb quartz-lined Parr 1108 oxygen bomb provides a rapid
method but usually these procedures have required and accurate method for treating coal samples to
the use of an expensive platinum liner in the bomb to determine trace amounts of Be, Cd, Cr, Cu, Pb, Mn,
avoid problems introduced by the leaching of trace Ni, V and Zn by atomic absorption spectrometry. The
amounts of heavy metals from the bomb walls and basic Lindahl combustion is described below.
electrodes during combustion. This problem has now Further details covering final assays for each element
been resolved with the introduction of a cup and are provided in the complete Lindahl Paper, a reprint
cover which can be used in any 1108 Parr oxygen of which can be obtained from Parr Instrument
bomb to hold the combustion products. Although a Company on request.
quartz liner does not offer the complete protection
obtainable with a platinum liner, it is nevertheless an Weigh a pelletized coal sample (1.0-1.2g) in a silica
effective means for preventing heavy metal capsule. Transfer 10 ml of 1:10 HNO3 to either the
contamination in certain combustion procedures. combustion bomb or to the quartz liner. Assemble
the bomb and charge it with oxygen to 15 atm. Place
THE 513A QUARTZ LINER the bomb in a cooling water bath and ignite the
sample. Allow the bomb to remain in the bath for 5
The quartz liner now offered for use in the 1108 minutes, then remove the bomb and release the
oxygen bomb consists of a quartz cup, 61 mm dia. x pressure slowly. Open the bomb carefully and rinse
86 mm deep, with a flat quartz cover which rests on all parts thoroughly into a Teflon beaker; then
top of the cup. Holes are provided in the cover for evaporate the washings to dryness on a hot plate or
inserting platinum electrodes which extend into the in a microwave oven.
cup to support a short length of platinum fuse wire
and a fused silica sample holder. All of the parts Treat the residue in the Teflon beaker with 5 ml of
needed to add this liner to an 1108 oxygen bomb are aqua regia and 5 ml of HF and heat to dryness.
provided in the 1912 Conversion Set listed below. Treat the residue with the appropriate volume of
HNO3 along with water to make the final solution 1%
KRAFT (TRW) PROCEDURES in HNO3 after dilution to volume. For ash contents up
to 5%, dilute to 25 ml. For ash up to 10% dilute to
Some of the earlier combustion procedures using a 100 ml.
quartz-lined oxygen bomb were developed by M.L.
Kraft of TRW, Inc., Defense and Space Systems In Lindahl’s work, final assays were performed by
Group, who used this method to prepare spark atomic absorption spectrophotometric methods.
source mass spectrometry samples of coal, oil and Flame absorption analyses were run on a Perkin-
other organic matter. In the Kraft methods the Elmer Model 5000 AA Spectrophotometer.
sample is burned in a fused silica capsule using 10 Flameless analyses were performed using a Perkin-
ml of 1:1 nitric acid in the bottom of the quartz liner to Elmer Model 703 AA Spectrophotometer equipped
absorb the combustion products. Kraft found that with a Model 400 HGA. Hollow cathode lamps were
background quantities of Cr, Fe, Ni and Mn were used in all analyses except for cadmium and lead
completely eliminated by this arrangement. analysis in which electrodeless discharge lamps were
used.
4
the wire into a running loop around the periphery
of the capsule. This will allow the capsule to be
inserted and removed without disturbing the fuse.
It will also keep the wire out of the direct flame
and reduce the possibility of a melt. Always add
an auxiliary fuse to the heavy 26 ga. wire, using
either cotton or nylon thread or a thin strip of filter
513A paper for this purpose.
Quartz Liner 5. When firing the 26 ga. fuse do not hold the firing
with 514A button down more than one or two seconds. A
Cover for longer ignition period will melt the wire. If the
1108 Oxygen wire melts, use the 7 cm terminals on the ignition
Bomb unit to obtain a lower firing voltage; or add a
heavy, one-ohm resistor to the 10-cm firing circuit
to lower the voltage.
6. To assemble the bomb, slide the quartz cup into
QUARTZ LINER CONVERSION SET the cylinder and lower the head and quartz cover
into the bomb gently so as not to break the cover.
All of the parts needed to install a quartz liner in an 7. For zinc and cadmium determinations, the 230A
1108 oxygen bomb are provided in a conversion set synthetic rubber sealing ring on the bomb head
(No. 1912) obtainable from Parr. The set consists of: should be replaced with a similar ring made of
1 513A Quartz liner Viton, Part No. 230AJV.
1 4AFB Platinum electrode, straight 8. Handle the quartz cup and cover carefully as
1 5AFB Platinum electrode, loop these parts are easily broken. And, although
2 68AC Lock nuts, T303SS quartz is noted for its good resistance to thermal
1 45C3 Platinum fuse wire, 300 cm shock, these parts can be broken by a non-
4 43A3 Combustion capsules, fused silica uniform burn or other unusual conditions in the
Any of the above items can also be purchased bomb. Breakage can be minimized by always
separately. leaving as much moisture in the sample as
possible (up to 40% in some cases) to avoid the
PROCEDURE FOR INSTALLING THE LINER sometimes explosive reaction which may result
from burning a bone dry sample.
1. Unscrew the two alloy electrodes from the bomb
head. Insert 4AFB platinum electrode through
the hole nearest the center of the quartz cover;
attach a 68AC lock nut to the straight electrode
and screw the electrode into the insulated
terminal in the bomb head.
2. Insert the 5AFB loop electrode into the opening
nearest the edge of the quartz cover; attach a
68AC lock nut to the electrode and screw it into
the bomb head.
3. Position the straight electrode with the hook 1108
pointed outward and tighten the lock nut gently; Oxygen
then turn the loop electrode to its center position Bomb with
and tighten the lock nut. Bring the loop electrode 513A
to its final position by gentle pressure in the loop Quartz
itself, but remember that platinum is soft and the Liner
threads on the electrodes can be damaged by
tightening lock nuts more than necessary. Also,
it may be necessary to bend the loop electrode
slightly to allow the cover to slide freely on the
electrodes and still remain concentric with the
bomb cylinder.
4. Use either fused silica or platinum combustion
capsules with this assembly, and always use
platinum fuse wire, either 36 ga. or 26 ga. wire in
the same manner as the regular 45C10 alloy
wire. If the heavier 26 ga. wire is used, wrap two
or three turns around each electrode and shape
5
SELECTED BIBLIOGRAPHY OF OXYGEN BOMB METHODS
16. Edwards, A.H. and Pearce, A.O., “Determination of
1. Adam. J., J. Chem. Met. Mining Soc. S. Africa, 39, 1
Sodium and Potassium in fuels”, Nature 154, 463
(1938).
(1944).
2. Adam, J., “The Use of the Calorimetric Bomb for the
17. Fujita, M., Terao, M., Takeda, Y., Hoshino, O. and
Determination of Carbon in Coal”, J. Chem. Met. th
Ukita, C., Abstract Papers at the 24 Annual Meeting
Mining Soc. S. Africa 39, 69-70 (1938).
of the Pharmaceutical Society of Japan, p. 552 (1967).
3. Agruss, M.S., Ayers, Jr., G.W. and Schindler, H.,
18. Fujiwara, S. and Narasaki, H., Bunseki Kagaku 10,
“Organic Halogen Compounds in Mineral Oils,
1268 (1961).
Detection, Determination & Identification”, Ind. Eng.
Chem., Anal. Ed. 13, 69-70 (1941).
19. Fujiwara, S. and Narasaki, “Determination of Trace
Elements in Organic Material by the Oxygen Bomb
4. Anduze. T. A., “Calorimetric Determination of Titanium
Method”, Anal. Chem. 40, 2031-3 (1968).
in Polyethylene”, Anal. Chem. 29, 90 (1957).
20. Herrig, H.J., Brennstoff-Chem. 42, 355 (1961).
5. Bailey, J.J. and Gehring, D.G., “Determination of
Traces of S, F and B in Organic Materials by Oxygen
21. Hicks, J.F., Fleenor, J. F. and Smith H., Anal. Chim.
Bomb Combustion”, Anal. Chem. 33, 1760 (1961).
Acta. 68, 480-3 (1974).
6. Barthel, J., Herglotz, H. and Lissner, A., “Rapid Method
22. Hill, W. H., Seals, J. and Montiegel, Ethel, “Destruction
for the Determination of Total Sulfur in Solid Fuels”,
of Animal and Vegetable Tissue by Combustion in a
Chem. Tech. (Ger.) 2, 179-81 (1950).
Parr Oxygen Bomb”, Am. Ind. Hyg. Assoc. J. 19, 378-
81 (1958).
7. Borchardt, L.G. and Browning, B.L., “An Oxygen Bomb
Method for Determining Mercury in Paper”, Tappi 41,
23. Hill, W.H. and Smith, R.C., “Analysis of Blood for
669 (1958).
Boron”, Am. Ind. Hyg. Assoc. J. 20, 131-3 (1959).
8. Bradford, H. R., “Fluorine in Western Coals”, Mining
24. Huggler, N., “Sohio Modification of ASTM D-129,
Eng. 9, 78-9 (1957).
Sulfur in Petroleum Products and Lubricants by the
Bomb Method”. Standard Oil Co. (Ohio), March, 1956.
9. Burke, W.M., “Boron Determination in Volatile Organic
Compounds Using the Parr Oxygen Bomb”, Ind. Eng.
25. Intoni, R. and Gargiulo, M., “Determination of
Chem., Anal. Ed. 13, 50-1 (1941).
Halogens in Organic Substances by Means of the
Bomb Calorimeter”, Rend. Ist. Super. Sanita (Rome)
10. Buss, H., Kohlschutter, H.W. and Preiss, M.,
11, 731-42 (1948).
“Determination of Phosphorus in Organic Materials
After Decomposition with Sodium Peroxide or
26. Johnson, H., “Determination of Selenium in Solid
Compressed Oxygen”, Z. Anal. Chem. 214 (2), 106-9
Waste”, Environmental Science & Technology 4, 850-2
(1965).
(1970).
11. Callan, T.P. and Toennies, G., “Determination of Sulfur
27. Kuck, J.A. and Grim, E.C., Microchem, J. 3, 35 (1959).
in Organic Compounds”, Ind. Eng. Chem., Anal. Ed.
13, 450-5 (1941).
28. Lambris, G. and Boll, H., “A New Method for the Rapid
and Exact Determination of Carbon Content of Solid
12. Carey, F.P., Blodgett, G. and Satterlee, H.S.,
and Liquid Fuels”, Brennstoff-Chem. 18, 61-6 (1937).
“Preparation of Samples for Determination of Arsenic –
Oxygen Bomb Combustion Method”, Ind. Eng. Chem.,
29. Lindahl, Peter C., “An Oxygen Bomb
Anal. Ed. 6, 327-30 (1934).
Combustion/Atomic Absorption Spectrophotometric
Method for the Determination of Trace Elements in
13. Conrad, Anne L., “Modification of the Parr Bomb
Coal”, Exxon Production Research Company,
Method for the Combustion of Petroleum Products”,
Houston, Tx 77001. Reprints available from Parr
Mikrochemie ver. Mikrochim. Acta. 38, 514-20 (1951).
Instrument Company, Moline, IL 61265
14. Conrad, Anne L. and Vigler, M.S., “Determination of
30. Longo, B., “Determination of Halogens, Especially
Boron in Borine Compounds”, Anal. Chem. 21, 585
Iodine, in Organic Compounds Using the Calorimetric
(1949).
Bomb”, Atti. X° congr. Intern. Chim. 3, 427-8 (1939).
15. Dye, W.B., Bretthauer, E., Seim, H.J. and Blincoe, C.,
31. Mehta, R.K.S., “Determination of Carbon and
“Fluorometric Determination of Selenium in Plants and
Hydrogen by Calorimeter Bomb”, J. Sci. Ind. Research
Animals with 3,3’-Diamino-benzadine”, Anal. Chem.
(India) 13B, 195-203 (1954).
35, 1687 (1963).

6
32. Monsanto Co., Organic Chemicals Div., St. Louis, Mo., 41. Siegfriedt, R.K., Wiberley, J.S. and Moore, R.W.,
“Determination of Chlorphenols and Their Salts in “Determination of Sulfur after Combustion in a Small
Impregnated Materials”, Technical Bulletin 0-24 (March Oxygen Bomb”, Anal. Chem. 23, 1008-11 (1951).
15, 1945).
42. Thomas, M., “Rapid Method for Determination of
33. Nishioka, S. and Miwa, M., “Determination of Carbon Carbon in Explosive Materials”, Mem. poudres 34,
and Hydrogen with a Bomb Calorimeter”, J. Chem. 402-11 (1952).
Soc. Japan, Ind. Chem. Sect. 55, 377-9 (1952).
43. Toennies, G. and Bakay, B., “ Photonephelometric
34. Nadkarni, R.A., “Determination of Volatile Elements in Microdetermination of Sulfate in Organic Compounds”,
Coal and other Organic Materials”, Am. Lab., August, Anal. Chem. 25, 160-5 (1953).
1981.
44. Ukita, T., Osawa, T., Imura, N., Tonomura, M., Sayato,
35. Piercy, G.T., Plant, E.K. and Rogers, M.C., “Rapid Y., Nakamuro, K., Kanno, S., Fukui, S., Kaneko, K.,
Determination of Phosphorus in Linseed Oil by Oxygen Ishikura, S., Yonaha, M., and Nakamura, T., “A Novel
Bomb”, Ind. Eng. Chem., Anal. Ed. 12, 165 (1940). Quick Determination of Mercury”, The Jour. Of
Hygienic Chem. 16, 258-66 (1970).
36. Przybylski, E., “A New Application of the Calorimetric
Bomb for Quantitative Analysis”, Roczniki 45. U.S. Environmental Protection Agency, “IERL-RTP
Pantswowego Zakladu Hig. 5, 170 (1954). Procedures Manual: Level 1, 2nd Ed., Interagency
Energy/Environment R&D Program Report”, EPA-
37. Randall, M. and Stevenson, H.O., “Rapid Volumetric 600/7-78-201, Industrial Environmental Research
Method for the Determination of Sulfate Ion”, Ind. Eng. Laboratory, Research Triangle Park, NC 27711.
Chem., Anal. Ed. 14, 620-1 (1942).
46. Whitaker, J.W., Chakravorty, R.N. and Ghosh, A.K.,
38. Selig, W., “Fluorine Analysis of Viton and Viton “Oxygen Determination by combustion in a Bomb”, J.
Containing Explosives”, Univ. Calif. Radia. Lab. Bul. Sci. Ind. Research (India) 15B, 72-7 (1956).
14875 (1966).
47. Wreath, A.R., J. Assoc. Official Agr. Chemists, 31, 800
39. Selig, W., “Fluorine Analysis of Plastic-Bonded (1948).
Explosives and Plastics”, Univ. Calif. Radia. Lab. Bul.
70156 (1966). 48. Zhokovskaya, M.D., “A New Method for the
Determination of Hydrogen in Solid Fuel by
40. Sheppard, H. and Rodegker, W., “Determination of H3 Combustion in a Bomb Calorimeter”, Chem. Zentr. II.
and C14 in Biological Materials Using Oxygen Bomb 952-3 (1947).
Combustion”, Anal. Biochemistry 4, 246-51 (1962).

7
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Phone 800 872 7720 Fax 309 762 9453
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Rev. 07/04

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