Titanous chloride

Titanium Phosphates. Titanium(III) phosphate [24704-65-2] (titanous phosphate) is a purple soHd, soluble ia dilute acid, giving relatively stable solutions. It can be prepared by adding a soluble phosphate to titanous chloride or sulfate solution and raising the pH until precipitation occurs. 

Reduction. Triaryknethane dyes are reduced readily to leuco bases with a variety of reagents, including sodium hydrosulfite, 2inc and acid (hydrochloric, acetic), 2inc dust and ammonia, and titanous chloride in concentrated hydrochloric acid. Reduction with titanium trichloride (Knecht method) is used for rapidly assaying triaryknethane dyes. The TiCl titration is carried out to a colorless end point which is usually very sharp (see Titanium COMPOUNDS, inorganic). 

In some cases, a simple solvent extraction is sufficient to remove a particular impurity. For example, traces of gallium can be removed from titanous chloride in hydrochloric acid by extraction with diisopropyl ether. 

Redox (reduction-oxidation) titrimetry is used primarily for nitrate detns. Five systems are in current use ferrous sulfate—dichromate, io dome trie, periodic acid oxidation (NaOH titrant), K permanganate, and titanous chloride-ferric ammonium sulfate. The ferrous sulfate— dichromate system is used for MNT DNT detns (Vol 2, C162-Lff Vol 6, F17-Rff Ref 17). In the iodometric procedure, the sample (ie, NG) is treated in a C02 atm with a satd soln of Mn chloride in coned HC1, the vol reaction products are bubbled thru a K iodide soln, and the liberated iodine is titrated with standard thiosulfate soln (Refs 1 17). The periodic... 

The prescribed analytical method for determining nitrogen content in PETN is the MIL-STD-286 Method 209.3. The ferrous chloride-titanous chloride method described for NG in Vol 6, G106-7 is also applicable to PETN... 

Assay Methods. A Na carbonate fusion prod is currently used for assay of mil grade AP (see below under Specifications), but recently attempts have been made to replace it with a method which is faster and simpler to carry out. Two procs have been proposed a) Titanous Chloride Titration. A measured excess of Ti trichloride is added to a known weight of AP which reacts according to the equation ... 

The ease of N determination in PVN samples appears to be a function of the degree of polymerization. The nitrometer method gives consistent results, but are about 0.6% lower than the true values (Ref 6). Difficulty is experienced with high viscosity PVN. These products dissolve slowly in sulfuric acid, and give scattered results. Analytical methods based on titanous chloride,... 

The Polymerisation of Styrene by Titanic Chloride, Part I. Kinetics, P.H. Plesch, Journal of the Chemical Society, 1953, 1653-1658. 

Titanous chloride (titanium trichloride) is applied in aqueous solutions, sometimes in the presence of solvents increasing the miscibility of organic compounds with the aqueous phase [199, 200]. Its applications are reduction of nitro compounds [201] and cleavage of nitrogen-nitrogen bonds [202] but it is also an excellent reagent for deoxygenation of sulfoxides [203] and amine oxides [199] (Procedure 38, p. 214). 

In 1910 M. A. Hunter (28) obtained the metal 99.9 per cent pure by a modification of Nilson and Pettersson s method in which pure titanic chloride and sodium were heated in a 1000-cc. machine steel bomb capable of bearing 40,000 kilograms of pressure. The lid, which rested on an... 

Determination of TNT — Titanous Chloride Method. Hot melt is present in the TNT wax filtrate obtd in 4.4.3.3.I. This filtrate is used in the TNT detn by the titanous chloride method. Hot melt does not interfere with the TNT detn... 

Standardization of0.2N Titanous Chloride Solution. Sweep the air from a 300-ml reduction flask with a current of nitrogen or carbon dioxide gas for 5 mins. Continue to pass the current of gas thru the flask until the titration is completed... 

Pipette 20.00ml of the 0.200N p-Nitroaniline soln into the reduction flask. Pipette 25ml of titanous chloride approx 0.2N into the same flask. Add 25ml of 6N HC1 (by cylinder), and a few glass beads. Connect the reduction flask to a reflux condenser and boil for 15 mins. Cool the flask to RT without disconnecting the condenser (lift the flask and condenser, remove the heater, and let the flask down into a pan of cold water)... 

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... 

Determination of the Normality of the Ferric Ammonium Sulfate Solution. Using the value of R and the value of the normality of titanous chloride detd in 4.4.3.5.11 and 4.4.3.5.12, calculate the normality of the ferric ammonium sulfate soln... 

HH) M. Roth R.E. Wegman, AnalChem 30, 2036(195 8). A soln containing NGu is analyzed for the NGu content by addition to excess deaerated titanous chloride followed by back titration with standard ferric ammonium sulfate... 

March i960 (Following are some accomplishments a) Modification of DuPont nitrometer by introducing a 2-part bulb. This bulb is recommended for use with PETN and Nitro-guanidine (NGu) (abbr NQ by Roth) This modification is described by M. Roth et al in PATR 2579(1958) b) Introduction of "titanous chloride-buffer method" for detn of NGu in propellants. This method is described by M. Roth R.F. Wegman in Anal-Chem 30, 2036(1958) (See Addnl Ref HH) c) Improved method for detn of stabilizer content. The method is described by M. 

It may alternately be detd by the method described on p 1394 of Ref 10a under "Nitrogua-nidine by Buffered Titanous Chloride Reduction" Picatinny Arsenal Method. The following titration method developed at PicArsn as a culmination of many years work involving the Ti(III ) titrant for nicro and nitrate species in general. 

M.I. Fauth H. Stalcup, AnalChem 30,1670— 72(1958) Be CA 53, 2929(1959) [Evaluation of six methods for detn of nitrogen in NGu. (Nitro N methods tested are modified nitrometer — greatest precision of the six acetate-buffered titanous chloride transnitration with sulfuric acid and Bowman-Scott). Total N methods are modified Kjeldahl and micro-Dumas — better of these two. The titanous chloride and trans-nitration methods are satisfactory]... 

N = normality of ferric alum soln Note Illustration of Apparatus for Storing and Using Titanous Chloride Solution is on p D1647 of Vol 5. On p D1646-L is stated that Mr N,... 

Reduction of ammonium chlororuthenate with titanous chloride gives a solution containing divalent ruthenium which will absorb ethylene or propylene to give a 1 1 ruthenium-olefin complex which was not isolated (108). Ethylene was previously reported not to form stable complexes on treatment with ruthenium halides (97). 

Two ammino-derivatives of titanic chloride, namely, octammino-titanic chloride, [Ti(NH3)8]Cl4, and hewammino-titanic chloride, [Ti(NH3)6]Cl4, are described.1... 

Octammino- titanic Chloride, [Ti(NH3)8]Cl4, is obtained by passing dry ammonia gas into a suspension of titanic chloride in ether ammonia is rapidly absorbed, and a dark yellow powder formed of composition TiCl4.8NH3. The substance loses ammonia very readily, and is immediately decomposed by moist air, but not if kept over freshly prepared anhydrous calcium chloride. 

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