No. 207M

Analytical Methods for Oxygen Bombs

Combustion with oxygen in a sealed Parr bomb has been accepted for many years as a standard procedure for converting solid and liquid combustible samples into soluble forms ready for chemical analysis. It is a reli-able whose effectiveness stems from its ability to treat samples quickly and conveniently within a closed sys-tem, thus ensuring complete retention and potential re-covery of all combustion products. The bomb combus-tion method is an essential step is standard ANSI/ASTM methods for determining sulfur and chlorine in coal, and it has been applied successfully to the determination of arsenic, phosphorus and other elements as well.

The methods given here for sulfur and chlorine corre-spond to the basic ASTM reference methods for these elements, each of which calls for a gravimetric fi nish. Although these are reliable procedures, other less time consuming volumetric, nephelometric or ion chromato-graphic methods can be used for estimating these ele-ments after recovering the bomb washings. Such alter-natives are suggested in the references which follow.

Sulfur in Combustible Solids. Burn a 1.0 gram sample and collect the washings as described in the basic pro-cedure for using the 1108 oxygen bomb. Let the bomb stand for at least 5 minutes after fi ring; then remove it from the water and release the residual gases slowly and at an even rate so that the pressure is reduced to at-mospheric in not less than one minute. Open the bomb and wash all parts of its interior, including the combus-tion capsule, valve passages and electrodes, with a fi ne jet of distilled water containing 1 ml of a saturated solu-tion of methyl orange indicator per liter. Wash until no acid reaction is observed, collecting the washings in a beaker. If necessary, use a rubber policeman to transfer any precipitate from the bomb or capsule to the beaker.

After neutralizing the solution, add 1 ml of ammonium hydroxide, heat the solution to boiling, and fi lter through a rapid qualitative paper. Wash the residue and fi lter pa-per with hot distilled water and add suffi cient water to bring the total volume of solution to approximately 250 ml. Neutralize with concentrated hydrochloric acid and add 2 ml in excess. Add 10 ml of saturated bromine wa-ter and evaporate to approximately 200 ml on a hot plate or other source of heat. Adjust to a slow boil and stir constantly while adding 10 ml of a 10% barium chloride solution from a pipette. Continue stirring for two min-utes, cover with a fl uted watch glass and keep just below boiling on a steam bath or hot plate until the volume is

reduced to 75 ml, then allow the precipitate to settle for another hour while cooling. Filter through an ashless fi lter paper and wash with warm water until free from chlorides.

Transfer the paper and precipitate to a weighed crucible, dry at low heat, char the paper without fl aming, then raise the temperature to a good red heat (approximately 925 ºC) and heat to a constant weight. If the crucible is placed in a cold electric muffl e furnace and the current turned on, drying, charring and ignition will usually oc-cur at the desired rate. After ignition is complete, allow the crucible to cool to room temperature and weigh. De-termine the exact weight of the barium sulfate precipi-tate and calculate the percentage of sulfur in the sample as follows:

Sulfur, % = Wt. BaSO4 X 13.734

Wt. Sample

Sulfur in Combustible Liquids. For oils or other liq-uids containing 5% sulfur or less, use a sample weighing from 0.6 to 0.8 gram. If the sample contains over 5% sulfur, use a sample weighing from 0.3 to 0.4 gram and add an equal amount of sulfur-free U.S.P. white oil. If the sample is not readily miscible with white oil, some other low sulfur combustible diluent may be used. How-ever, the combined weight of sample and white oil or other combustion aid must not exceed 1.0 gram. If the sample is volatile it must be weighed in a sealed holder.

The procedure for fi lling the bomb, fi ring, recovering the washings and determining sulfates is the same for liq-uid samples as described in the preceding method for solids.

Other less time consuming procedures have been sug-gested as an alternative to the gravimetric methods de-scribed here for estimating sulfur in the bomb washings. Among the titrimetric methods: Hicks21, et al titrates with lead perchlorate and determines the equivalence point using a lead ion specifi c electrode. Callan11 suggests converting to benzadine sulfate and titrating with stan-dard hydroxide solution. Siegfriedt41 titrates with bari-um chloride solution using tetra-hydroxyquinone as an indicator. Randall37 adds barium chloride in excess and back titrates with disodium hydrogen phosphate with the addition of alcohol. Herrig20 back titrates with Tritiplex III using phthalein purple as an indicator. A conductomet-ric method has been suggested by Barthel6. Nephelo-

Analytical Methods for Oxygen Bombs

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metric methods for trace amounts of sulfate have been suggested by Toennies43 and Bailey5.

Chlorine in Combustible Solids and Liquids. Platinum combustion capsules and platinum ignition wire are recommended for these tests because of the extremely corrosive nature of chlorine and its compounds. After repeated use with such samples, the inner surfaces of the bomb will become etched to the point where ap-preciable amounts of metal salts will be introduced during each combustion. The ability of the bomb to withstand such corrosion can be improved by keeping the inner surfaces highly polished. Any bomb which is being used for chlorine determinations should be repol-ished at regular intervals to prevent the development of deep pits. The alternative to this procedure is to use an 1108CL bomb which offers much better resistance to chlorine than the standard 1108 bomb. Or for ultimate protection, use an 1105C or 1106C bomb with a platinum liner.

Samples containing more than 2% chlorine by weight should be diluted with U.S.P. white oil or some other non-volatile, chlorine-free diluent. The suggested amounts of sample and diluent are shown in the follow-ing table, but the user is cautioned that the combined weight of the charge must not exceed 1.0 gram.

% of Chlorine in Sample

Grams of Sample

Grams Of White Oil

Below 2 0.8 0.0

2 to 5 0.4 0.4

5 to 10 0.2 0.6

10 to 20 0.1 0.7

20 to 50 0.05 0.7 Place about 5 ml of a 5% sodium carbonate solution (135g Na2CO310H2O per liter) in the bomb, assemble and fi ll with oxygen to a pressure of 35 atmospheres. Immerse the bomb in a bath through which cold water is circulating. Attach the ignition wire to the bomb ter-minal, then stand at least six feet from the bath when fi ring the charge. Keep the bomb in the bath at least fi ve minutes before removal. Release the residual gas slow-ly and at an even rate so that the pressure is reduced to atmospheric in not less than one minute. Open the bomb and examine for traces of unburned sample or sooty deposits. If found, discard the determination and clean the bomb thoroughly before using it again.

If the combustion was satisfactory, wash the sample cup and all interior surfaces of the bomb with a fi ne stream of distilled water, collecting the washings in a 600 ml beaker. Scrub the interior of the cylinder and the un-derside of the head with a rubber policeman. Continue washing until no acid reaction is observed on any bomb

parts or passages, which will normally require at least 300 ml of wash water.

Acidify the solution by adding 1:1 nitric acid dropwise until the methyl red endpoint is observed; then add 2 ml excess acid. Filter through a qualitative paper and collect the fi ltrate in a 600 ml beaker. Heat to about 60 ºC; protect from strong light and slowly add 5 ml of sil-ver nitrate solution (50 g per liter) while stirring. Heat almost to boiling and hold at this temperature until the supernatant liquid becomes clear. Add a few drop of silver nitrate solution to test for complete precipitation. If cloudiness appears, repeat the above operation.

Allow the beaker to stand in a dark place for at least one hour. Filter the precipitate by suction onto a weighed fritted glass fi lter. Wash with distilled water containing 2 ml of 1:1 nitric acid per liter. Dry the precipitate and crucible at 110 ºC for one hour. Cool in a desiccator and weigh.

Make a blank determination with 0.7 to 0.8 gram of white oil, omitting the sample; then calculate the chlo-rine content of the sample by substituting in the follow-ing equation:

Chlorine, % by wt. = (P-B) 24.74 mwhere, P = grams AgCl obtained from sample B = grams AgCl obtained from blank m = mass of sample in grams

ASTM Methods for Sulfur and Chlorine. Oxygen bomb procedures for determining sulfur and chlorine in a broad range of combustible materials are given in the following standard methods published by the Ameri-can Society for Testing and Materials, copies can be ob-tained from ASTM at www.astm.org.

ASTM Method D129, “Standard Test Method for Sulfur in Petroleum Products (General Bomb Method)”.

ASTM Method D3177, “Standard Test Method for Total Sulfur in the Analysis Sample of Coal and Coke”.

ASTM Method D2361, “Standard Test Method for Chlo-rine in Coal”.

ASTM Method D1619, “Standard Test Method for Sul-fur in Carbon Black”.

ASTM Method D808, “Standard Test Method for Chlo-rine in New and Used Petroleum Products (Bomb Meth-od)”.

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w w w . p a r r i n s t . c o m 3

ASTM Method D1847, “Standard Test Method for Total Chlorine Content of Epoxy Resins”.

ASTM Method D3684, “Standard Test Method for To-tal Mercury in Coal by the Oxygen Bomb Combustion/Atomic Absorption Method”.

ASTM Method D3761, “Standard Test Method for Total Fluorine in Coal by the Oxygen Combustion/Ion Selec-tive Electrode Method”.

ASTM Method D4208, “Standard Test Method for Total Chlorine in Coal by the Oxygen Combustion/Ion Selec-tive Electrode Method”.

ASTM Method E775, “Standard Test Methods for Total Sulfur in the Analysis Sample of Refuse-Derived Fuel”.

ASTM Method E776, “Standard Test Method for forms of Chlorine in Refuse-Derived Fuel”.

ASTM Method E926, “Standard Test Method of Prepar-ing Refuse-Derived Fuel (RDF) Samples for Analysis of Metals”.

Halogen Determinations. Other halogens in addition to chlorine can be determined by the oxygen bomb meth-od. Agruss3 used the oxygen bomb to determine chlo-rine, bromine and iodine mineral oils. Longo30 applied this method to many different organic compounds, with particular emphasis on the determination of iodine. In-tonti25 used an oxygen bomb for analyzing insecticides and antifermentatives. Bradford8 describes a bomb method for determining fl uorine in coal. Bailey5 and Selig38,39 describe the use of platinum lined bomb for determining fl uorine. The Monsanto Co.32 uses the oxy-gen bomb combustion method for determining small amounts of pentachlorophenol and similar chlorophe-nols in wall board, wood, paperboard, fi sh net, rubber etc. Recently, Nadkarni34 has used halogen selective electrodes to determine fl uorine, chlorine, bromine and iodine in coal samples and polymers after combustion in an oxygen bomb.

Arsenic Determinations. It has been shown by Carey12 that combustion in an oxygen bomb is a reliable way of preparing samples for the determination of arsenic by the Gutzeit method, or by the Marsh-Berzelius method. In this application the oxygen bomb replaces the acid digestion generally used in the standard methods for arsenic.

Mercury Determinations. Borchardt7 used an oxygen bomb to determine mercury in paper. Fujita17 deter-mined mercury in rice, rice hulls and hair, while Ukita44 used the bomb method for mercury determinations us-

ing atomic absorption spectrometry for the fi nal mea-surement.

Phosphorus Determinations. Oxygen bomb meth-ods for determining phosphorus have been given by Piercy35, Conrad13, Wreath47, and Buss10. One problem associated with this determination is the formation of a phosphoric acid mist in the bomb which does not settle out after combustion. To dissipate the mist, apply 20 v.d.c. to the electrodes. To minimize the formation of phosphoric acid mist, add one gram of sodium carbon-ate to the sample, mix some sodium naphthenate or zinc oxide with the sample.

Boron Determinations. An oxygen bomb technique suggested by Hill22 has been found excellent for the de-struction of animal and vegetable tissue preparatory to chemical analysis. A similar technique for the analysis of blood samples has also been recommended23. This procedure has been used successfully for determining small amounts of boron in animal and vegetable matter, and it seems reasonable to assume that it would work equally well for determining other elements. Burke9, Conrad13,14 and Kuck27 also describe methods for deter-mining boron after combustion in an oxygen bomb.

Other Elements. Selenium, Zinc, Lead, Titanium, Iron, Sodium, Potassium, Calcium, Magnesium, Copper, Car-bon, Hydrogen, Oxygen, Tritium, Beryllium, Chromium, Manganese, Nickel, Vanadium and Carbon-14, all can be determined by oxygen bomb methods.

Selenium has been determined in solid wastes by John-son26 and in plant and animal tissue by Dye15.

Zinc in rubber and copper in mushrooms has been re-ported by Przybylski36. Edwards16 has sodium, potas-sium, calcium and magnesium in fuels. Fujiwara18 de-scribes methods for determining iron, aluminum and titanium in polyethylene, and Anduze4 on titanium in polyethylene. Lead in piston deposits has been deter-mined by Conrad13. Lead in coal has been determined by Lindahl29.

Carbon determinations by the oxygen bomb method have been reported by Adam1,2, Lambris28, Thomas42, Mehta31 and Nishioka33. Hydrogen has been determined by Mehta31 and Nishioka33 and Zhokovskay48. The use of two bombs for determining oxygen is described by Witaker46.

Nadkarni34 has determined nitrogen in coal samples us-ing a chemiluminescent method following combustion in an oxygen bomb. This method is much faster than the traditional Kjeldahl method, requiring only a minute to determine nitrogen concentration.

Analytical Methods for Oxygen Bombs

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A method for determining H3 and C14 in biological mate-rials is described by Sheppard40.

Fujiwara19 gives an excellent review of methods for de-termining trace elements in organic compounds by the oxygen bomb method.

Lindahl29 describes a particularly useful method for the determination of beryllium, chromium, manganese, nickel, vanadium, copper, lead and zinc in coal.

A procedures manual issued by the U.S. Environmental Protection Agency recommends combustion in a Parr Oxygen Bomb for preparing all combustible materials for inorganic analysis. Specifi c procedures are given for mercury, antimony and arsenic. Procedures For Determining Trace Elements Using A Quartz Liner In the 1108 Oxygen Bomb

Trace amounts of heavy metals in coal and other com-bustible samples can be determined by the bomb meth-od but usually these procedures have required the use of an expensive platinum liner in the bomb to avoid problems introduced by the leaching of trace amounts of heavy metals from the bomb walls and electrodes dur-ing combustion. This problem has now been resolved with the introduction of a cup and cover which can be used in any 1108 Parr oxygen bomb to hold the combus-tion products. Although a quartz liner does not offer the complete protection obtainable with a platinum liner, it is nevertheless an effective means for preventing heavy metal contamination in certain combustion procedures.

The 513A Quartz Liner

The quartz liner now offered for use in the 1108 oxygen bomb consists of a quartz cup, 61 mm dia. x 86 mm deep, with a fl at quartz cover which rests on top of the cup. Holes are provided in the cover for inserting plati-num electrodes which extend into the cup to support a short length of platinum fuse wire and a fused silica sample holder. All of the parts needed to add this liner to an 1108 oxygen bomb are provided in the 1912 Con-version Set listed below.

Kraft (TRW) Procedures

Some of the earlier combustion procedures using a quartz-lined oxygen bomb were developed by M.L. Kraft of TRW, Inc., Defense and Space Systems Group, who used this method to prepare spark source mass spec-trometry samples of coal, oil and other organic matter. In the Kraft methods the sample is burned in a fused silica capsule using 10 ml of 1:1 nitric acid in the bottom of the quartz liner to absorb the combustion products.

Kraft found that background quantities of Cr, Fe, Ni and Mn were completely eliminated by this arrangement.

Lindahl Procedures For Trace Elements In Coal

Extensive studies by Peter C. Lindahl29 of the Exxon Pro-duction Research Company have shown that a quartz-lined Parr 1108 oxygen bomb provides a rapid and ac-curate method for treating coal samples to determine trace amounts of Be, Cd, Cr, Cu, Pb, Mn, Ni, V and Zn by atomic absorption spectrometry. The basic Lindahl combustion is described below. Further details cover-ing fi nal assays for each element are provided in the complete Lindahl Paper, a reprint of which can be ob-tained from Parr Instrument Company on request.

Weigh a pelletized coal sample (1.0-1.2g) in a silica cap-sule. Transfer 10 ml of 1:10 HNO3 to either the combus-tion bomb or to the quartz liner. Assemble the bomb and charge it with oxygen to 15 atm. Place the bomb in a cooling water bath and ignite the sample. Allow the bomb to remain in the bath for 5 minutes, then remove the bomb and release the pressure slowly. Open the bomb carefully and rinse all parts thoroughly into a Tef-lon beaker; then evaporate the washings to dryness on a hot plate or in a microwave oven.

Treat the residue in the Tefl on beaker with 5 ml of aqua regia and 5 ml of HF and heat to dryness. Treat the resi-due with the appropriate volume of HNO3 along with water to make the fi nal solution 1% in HNO3 after dilu-tion to volume. For ash contents up to 5%, dilute to 25 ml. For ash up to 10% dilute to 100 ml.

In Lindahl’s work, fi nal assays were performed by atom-ic absorption spectrophotometric methods. Flame ab-sorption analyses were run on a Perkin-Elmer Model 5000 AA Spectrophotometer. Flameless analyses were performed using a Perkin-Elmer Model 703 AA Spec-trophotometer equipped with a Model 400 HGA. Hol-low cathode lamps were used in all analyses except for cadmium and lead analysis in which electrodeless dis-charge lamps were used.

Quartz Liner Conversion Set

All of the parts needed to install a quartz liner in an 1108 oxygen bomb are provided in a conversion set (No. 1912) obtainable from Parr. The set consists of: 1 513A Quartz liner 1 4AFB Platinum electrode, straight 1 5AFB Platinum electrode, loop 2 68AC Lock nuts, T303SS 1 45C3 Platinum fuse wire, 300 cm 4 43A3 Combustion capsules, fused silicaAny of the above items can also be purchased sepa-rately.

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513A Quartz Liner with 514A Cover for 1108 Oxygen Bomb

Procedure For Installing The Liner

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 termi-nal 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 pointed outward and tighten the lock nut gently; then turn the loop electrode to its center posi-tion and tighten the lock nut. Bring the loop electrode to its fi nal position by gentle pressure in the loop itself, but remember that platinum is soft and the threads on the electrodes can be damaged by tightening lock nuts more than nec-essary. Also, it may be necessary to bend the loop electrode slightly to allow the cover to slide freely on the electrodes and still remain concen-tric 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 the wire into a running loop around the periph-ery 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 fl ame 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 fi lter paper for this purpose.

5. When fi ring the 26 ga. fuse do not hold the fi ring button down more than one or two seconds. A longer ignition period will melt the wire. If the wire melts, use the 7 cm terminals on the igni-tion unit to obtain a lower fi ring voltage; or add a heavy, one-ohm resistor to the 10-cm fi ring circuit to lower the voltage.

6. To assemble the bomb, slide the quartz cup into the cylinder and lower the head and quartz cover into the bomb gently so as not to break the cover.

7. For zinc and cadmium determinations, the 230A synthetic rubber sealing ring on the bomb head should be replaced with a similar ring made of Viton, Part No. 230AJV.

8. Handle the quartz cup and cover carefully as these parts are easily broken. And, although quartz is noted for its good resistance to thermal shock, these parts can be broken by a non-uniform burn or other unusual conditions in the bomb. Breakage can be minimized by always leaving as much moisture in the sample as possible (up to 40% in some cases) to avoid the sometimes explosive reaction which may result from burning a bone dry sample.

1108 Oxygen Bomb with 513A Quartz Liner

Analytical Methods for Oxygen Bombs

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1. Adam. J., J. Chem. Met. Mining Soc. S. Africa, 39, 1 (1938).

2. Adam, J., “The Use of the Calorimetric Bomb for the Determination of Carbon in Coal”, J. Chem. Met. Mining Soc. S. Africa 39, 69-70 (1938).

3. Agruss, M.S., Ayers, Jr., G.W. and Schindler, H., “Organic Halogen Compounds in Mineral Oils, Detection, Determination & Identifi cation”, Ind. Eng. Chem., Anal. Ed. 13, 69-70 (1941).

4. Anduze. T. A., “Calorimetric Determination of Titanium in Polyethylene”, Anal. Chem. 29, 90 (1957).

5. Bailey, J.J. and Gehring, D.G., “Determination of Traces of S, F and B in Organic Materials by Oxygen Bomb Combustion”, Anal. Chem. 33, 1760 (1961).

6. Barthel, J., Herglotz, H. and Lissner, A., “Rapid Method for the Determination of Total Sulfur in Solid Fuels”, Chem. Tech. (Ger.) 2, 179-81 (1950).

7. Borchardt, L.G. and Browning, B.L., “An Oxygen Bomb Method for Determining Mercury in Pa-per”, Tappi 41, 669 (1958).

8. Bradford, H. R., “Fluorine in Western Coals”, Min-ing Eng. 9, 78-9 (1957).

9. Burke, W.M., “Boron Determination in Volatile Organic Compounds Using the Parr Oxygen Bomb”, Ind. Eng. Chem., Anal. Ed. 13, 50-1 (1941).

10. Buss, H., Kohlschutter, H.W. and Preiss, M., “De-termination of Phosphorus in Organic Materials After Decomposition with Sodium Peroxide or Compressed Oxygen”, Z. Anal. Chem. 214 (2), 106-9 (1965).

11. Callan, T.P. and Toennies, G., “Determination of Sulfur in Organic Compounds”, Ind. Eng. Chem., Anal. Ed. 13, 450-5 (1941).

12. Carey, F.P., Blodgett, G. and Satterlee, H.S., “Preparation of Samples for Determination of Arsenic – Oxygen Bomb Combustion Method”, Ind. Eng. Chem., Anal. Ed. 6, 327-30 (1934).

13. Conrad, Anne L., “Modifi cation of the Parr Bomb Method for the Combustion of Petroleum Prod-ucts”, Mikrochemie ver. Mikrochim. Acta. 38, 514-20 (1951).

14. Conrad, Anne L. and Vigler, M.S., “Determination of Boron in Borine Compounds”, Anal. Chem. 21, 585 (1949).

15. Dye, W.B., Bretthauer, E., Seim, H.J. and Blincoe, C., “Fluorometric Determination of Selenium in Plants and Animals with 3,3’-Diamino-benza-dine”, Anal. Chem. 35, 1687 (1963).

16. Edwards, A.H. and Pearce, A.O., “Determination of Sodium and Potassium in fuels”, Nature 154, 463 (1944).

17. Fujita, M., Terao, M., Takeda, Y., Hoshino, O. and Ukita, C., Abstract Papers at the 24th Annual Meeting of the Pharmaceutical Society of Japan, p. 552 (1967).

18. Fujiwara, S. and Narasaki, H., Bunseki Kagaku 10, 1268 (1961).

19. Fujiwara, S. and Narasaki, “Determination of Trace Elements in Organic Material by the Oxygen Bomb Method”, Anal. Chem. 40, 2031-3 (1968).

20. Herrig, H.J., Brennstoff-Chem. 42, 355 (1961).

21. Hicks, J.F., Fleenor, J. F. and Smith H., Anal. Chim. Acta. 68, 480-3 (1974).

22. Hill, W. H., Seals, J. and Montiegel, Ethel, “De-struction of Animal and Vegetable Tissue by Combustion in a Parr Oxygen Bomb”, Am. Ind. Hyg. Assoc. J. 19, 378-81 (1958).

23. Hill, W.H. and Smith, R.C., “Analysis of Blood for Boron”, Am. Ind. Hyg. Assoc. J. 20, 131-3 (1959).

24. Huggler, N., “Sohio Modifi cation of ASTM D-129, Sulfur in Petroleum Products and Lubricants by the Bomb Method”. Standard Oil Co. (Ohio), March, 1956.

25. Intoni, R. and Gargiulo, M., “Determination of Halogens in Organic Substances by Means of the Bomb Calorimeter”, Rend. Ist. Super. Sanita (Rome) 11, 731-42 (1948).

26. Johnson, H., “Determination of Selenium in Solid Waste”, Environmental Science & Technol-ogy 4, 850-2 (1970).

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27. Kuck, J.A. and Grim, E.C., Microchem, J. 3, 35 (1959).

28. Lambris, G. and Boll, H., “A New Method for the Rapid and Exact Determination of Carbon Con-tent of Solid and Liquid Fuels”, Brennstoff-Chem. 18, 61-6 (1937).

29. Lindahl, Peter C., “An Oxygen Bomb Combus-tion/Atomic Absorption Spectrophotometric Method for the Determination of Trace Elements in Coal”, Exxon Production Research Company, Houston, Tx 77001. Reprints available from Parr Instrument Company, Moline, IL 61265

30. Longo, B., “Determination of Halogens, Espe-cially Iodine, in Organic Compounds Using the Calorimetric Bomb”, Atti. X° congr. Intern. Chim. 3, 427-8 (1939).

31. Mehta, R.K.S., “Determination of Carbon and Hydrogen by Calorimeter Bomb”, J. Sci. Ind. Re-search (India) 13B, 195-203 (1954).

32. Monsanto Co., Organic Chemicals Div., St. Louis, Mo., “Determination of Chlorphenols and Their Salts in Impregnated Materials”, Technical Bulle-tin 0-24 (March 15, 1945).

33. Nishioka, S. and Miwa, M., “Determination of Carbon and Hydrogen with a Bomb Calorimeter”, J. Chem. Soc. Japan, Ind. Chem. Sect. 55, 377-9 (1952).

34. Nadkarni, R.A., “Determination of Volatile Ele-ments in Coal and other Organic Materials”, Am. Lab., August, 1981.

35. Piercy, G.T., Plant, E.K. and Rogers, M.C., “Rapid Determination of Phosphorus in Linseed Oil by Oxygen Bomb”, Ind. Eng. Chem., Anal. Ed. 12, 165 (1940).

36. Przybylski, E., “A New Application of the Calori-metric Bomb for Quantitative Analysis”, Roczniki Pantswowego Zakladu Hig. 5, 170 (1954).

37. Randall, M. and Stevenson, H.O., “Rapid Volu-metric Method for the Determination of Sulfate Ion”, Ind. Eng. Chem., Anal. Ed. 14, 620-1 (1942).

38. Selig, W., “Fluorine Analysis of Viton and Viton Containing Explosives”, Univ. Calif. Radia. Lab. Bul. 14875 (1966).

39. Selig, W., “Fluorine Analysis of Plastic-Bonded Explosives and Plastics”, Univ. Calif. Radia. Lab. Bul. 70156 (1966).

40. Sheppard, H. and Rodegker, W., “Determina-tion of H3 and C14 in Biological Materials Using Oxygen Bomb Combustion”, Anal. Biochemistry 4, 246-51 (1962).

41. Siegfriedt, R.K., Wiberley, J.S. and Moore, R.W., “Determination of Sulfur after Combustion in a Small Oxygen Bomb”, Anal. Chem. 23, 1008-11 (1951).

42. Thomas, M., “Rapid Method for Determination of Carbon in Explosive Materials”, Mem. poudres 34, 402-11 (1952).

43. Toennies, G. and Bakay, B., “ Photonephelomet-ric Microdetermination of Sulfate in Organic Compounds”, Anal. Chem. 25, 160-5 (1953).

44. Ukita, T., Osawa, T., Imura, N., Tonomura, M., Sayato, Y., Nakamuro, K., Kanno, S., Fukui, S., Kaneko, K., Ishikura, S., Yonaha, M., and Naka-mura, T., “A Novel Quick Determination of Mer-cury”, The Jour. Of Hygienic Chem. 16, 258-66 (1970).

45. U.S. Environmental Protection Agency, “IERL-RTP Procedures Manual: Level 1, 2nd Ed., Inter-agency Energy/Environment R&D Program Re-port”, EPA-600/7-78-201, Industrial Environmental Research Laboratory, Research Triangle Park, NC 27711.

46. Whitaker, J.W., Chakravorty, R.N. and Ghosh, A.K., “Oxygen Determination by combustion in a Bomb”, J. Sci. Ind. Research (India) 15B, 72-7 (1956).

47. Wreath, A.R., J. Assoc. Offi cial Agr. Chemists, 31, 800 (1948).

48. Zhokovskaya, M.D., “A New Method for the De-termination of Hydrogen in Solid Fuel by Com-bustion in a Bomb Calorimeter”, Chem. Zentr. II. 952-3 (1947).

Revision 05/31/12