Water detn

K. Mehlhose, Explosivstoffe 20 (3-4), 37-70 (1972) CA 78, 113513 (1973) Methods developed for detn of H20 in gun and rocket propints are column distn with n-PrOH and gas-chromatographic analysis of the distillate, corrected for continuous formation of water in decompn reactions and photometric methods, both based on the reaction of CoCl2 with water. Choice of the methods is based on a critical review (117 refs) of the usual methods of water detn by chemical and physical methods. A theoretical and exptl analysis of the new methods was made and their results compared with those of older methods. Application to mono-, di-, and tribasic and to double-base NC and poly (vinyl nitrate) propints is discussed... 

This technique calls for drying the sample in a liq drying column using Linde 4A molecular sieves (water detn), and then using the near IR spectrum between 2.2 and 1.7 micrometers to determine the ratio of UDMH to diethylenetriamine] 5) H.N. Voltrauer, Hydrazine Analysis Using Chemiluminescence , SAM-76-37, Aero Chem Res Lab, Princeton, Contract F41609-76-C-0029 (1976) [A procedure is reported using the chemiluminescent reactions of ozone with monomethylhydrazine and Aero-zine-50 (UDMH/hydrazine in 50/50 wt %) to... 

Detonation, Water Plexiglos Induced Shock Wove Velocity in. Cook et al (Ref 2) applied the "aquarium technique in the exptl detn of the equation of state for water Lucire. The results for water are compared with similar results by other methods. Measurements of the peak pressures in the deton wave are presented for RDX, RDX/salt, TNT HBX-1. Peak pressures were found to be the CJ or deton pressures of the thermohydro-dynamic theory. There was no evidence whatever for the "spike of the Zel dovich-von Neumann model even though conditions were such that this spike would have been detected by the method employed if it were present, at lease in the large diam, nonideal expls of max reaction zone length Refs.T) C. Fauquignon, CR 251, 38 (I960) 2) M, A. Cook et al, JAppl... 

The term (C—RD) should be zero. If the value lies outside the range +0.10 and —0.10, either R is incorrect, or the acetic acid is contaminated. Repeat the detn of R. Continued high or low values for (C—RD) probably mean impure acetic acid If normality of Ti(III) soln falls outside of the range 0.19—0.22, add 20% titanous chloride soln or water as required to bring normality to approx 0.2N. Then repeat the detn of R and repeat the detn of the normality... 

CAUTION Keep soln well agitated at all times. When soln begins distilling, position flask so that an air space is between the flask and hot palte. This is to prevent a hot spot from building up in the chunk explosive. Sample should not be left unattended during the moisture detn. Care must be taken that the cold water condenser is operating properly at all times. If the condenser should fail to trap the toluene and the flash were to boil dry, there could be a possibility of overheating the expl... 

L.A. Chen el, MP 23, 4-6(1928) CA 22, 3531(1928) (Detn of alcohol, ether and water in solvent eliminated from propellant during drying)... 

In Ref 2 is described analysis of industrial EtAcet liable to contain water, ethanol and ethyl formate with traces of acidity, whereas in Ref 3 is described a precise method for detn of acidity in EtAcet... 

Procedure Assemble the apparatus (Fig Et 15) for the ethoxy detn. Grind approx 1 g of the specimen to pass thru 149 micron (No 100) sieve conforming to Spec RR-S-366 and dry it at I00°t5° for 2 hrs. Fill the trap T by pouring a small amt of aq suspension of red phosphorus thru the cup C above. Follow with a water rinse, using sufficient liq to make the trap... 

OB to C02 —37.4% colorless, somewhat volatile liquid, with faint aromatic odor sp gr 1.348 at 20/4°, fr p below —20°, bp 91—2° in a vacuum of a water jet pump and decomp at atm pressure miscible with w and sol in ale, eth chlf dissolves in coned sulfuric acid with considerable evolution of beat, so that in the detn of die nitrogen concent by Nitrometer Method (See Vol 1 of Encycl, pp A373—A378)... 

By means of a pipette, transfer a portion of approx lOg of the sample to a tared 250 ml beaker, rewelgh and dissolve in 100ml of benzene. Move the soln to a 250-ml separatory funnel and shake the contents of it with a 50-ml portion of neutral distilled water. After separation of layers run die water layer into the above 250-ml beaker. Repeat the operation using another 50ml of discd w and transfer the bottom layer to the same beaker. Add to beaker several drops of bromomethyl blue indicator. If the soln turns yellow titrate immediately with standard 0.01N NaOH. soln and if hlue titrate immediately with standard 0.0IN sulfuric acid. The change of color is taken as end point. Run a blank detn on 100ml of benzene alone and correct die volume alkali of acid required for titration. Calculate the percentage of acidity as nitric acid or alkalinity as Na carbonate as follows ... 

Note As NG is appreciably soluble in water, care should be taken not oo use too much water. In order to hajre comparable results, the same quantity of water should be used for all detns (Ratio 1 1)... 

It can also be used for rapid detn of small amts of water in miscellaneous materials. The KF reagent consists of sulfur dioxide-iodine in pyridine-methanol solution. It is available in commerce in strength equivalent to 5—6 mg water per 1 ml of reagent. It can also be prepd... 

Excess pyridine, iodine, and methanol are required for quantitative consumption of water. Sulfur dioxide reduces iodine quantitatively in the presence of excess water. The excess iodine present in the mixt makes a visual detn of the end point difficult. Therefore, the endpoint can be detnd electrometri-... 

Chimlnd, Bruxelles, Belgium 3(1954) CA 50, 7479(1956)(Detn of N content in NC) 26)J. Tranchant, Ibid 3(1954) CA 51, 1607(1957) (Titanometric detn of N content in NC) 27)P. Miaud, MP 37, 465-97( 1955)(Detn of water in NC cakes by means of high-frequency current) 27)H.Stalcup R.Williams, AnalChem 27, 543-6 (1955)(Volumetric detn of NC NGu by transnitration of salicylic acid) 28)Ott vol 5, part 3(1955), 1394(Detn of viscosity of NC) 1407(Detn of N content) 1411-13(Stability tests) 1414-15(Detn of impurities, such as ash, acidity, alkalinity, sulfur chlorides in NC) 14l6(Detn of density) 29)T.C.Castorina, PATR 2107(1955XRadiometric method for detn of sulfate in crude NC) 30)E.Thonert F.Lobato, Explosivst 1955, 109-13 CA 51, 9160(1957)... 

The phase-stabilized AN is prepd by mixing 90 parts AN, 10 ps K nitrate some water, heating the mixt to 140°F, drying and grinding to 40 micron size particles. The proplnt is compressed into grains. Example of compn AN 82.95, K nitrate 9.22, petroleum pitch 4.11 90/10 copolymer of l,3-butadiene/2-methyl-5 -vinyl pyridine 1.76 Amm dichromate 1.96%] EE)R.MacDonald A.M.Bedard, "Methods of Chemical Analysis of Cardeplex Propellant No 4760/A5 and Its Ingredients", CARDE TR426/63 (1963) (Cardeplex No 4760/A5 is a composite ammonium perchlorate-polyurethane proplnt. Analysis of fully cured product includes detns of Amm perchlorate, Al, ferric acetylacetonate, phenyl-/3 -naphthylamine, lithium fluoride total iron) FF)Anon,... 

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