Chamber crystals 601 process

Formed as an intermediate in the Pb chamber process for sulfuric acid by the reaction of sulfur dioxide, nitrogen trioxide, oxygen and w (chamber crystals) (Refs 1 2). Can be prepd from Ag acid sulfate and nitrosyl bromide (Ref 4)... 

Free nitrosylsulphuric acid actually occurs in the lead chambers only under abnormal conditions of working its separation as chamber crystals is most undesirable from the manufacturer s point of view, as not only does it indicate improper regulation of the process, but it also causes the lead walls of the chambers to be attacked unduly. A solution of violet acid is sometimes obtained at the bottom of the Gay-Lussac tower. 

Nitrosulphonic Acid, Nitrosylsulphuric Acid or Nitroso-sulphuric Acid, NQ2.S02.0H.—In 1806, Clement and Desormcs, during the manufacture of sulphuric acid by the lead chamber process, observed the formation of a crystalline solid, to which the names nitrosulphonic acid and nitrosylsulphuric acid were later given the term chamber crystals, however, is still commonly applied to this acid.6 The composition and nature of the acid were first investigated by Weber,7 and by Michaelis and Schumann.8... 

In the lead chamber process for the manufacture of sulfuric acid, nitric oxide, oxygen (from the air), sulfur dioxide, and water (steam), interact. The nitric oxide acts as the catalyst, and is present at the end of the action, with the sulfuric acid. It acts as oxygen carrier. One of the intermediate compounds which is formed contains nitrogen peroxide (NO2), sulfur dioxide, and water. It may be obtained in crystalline form, known as chamber crystals which have the composition HSQ3NO2, nitro-sulfonic acid, under certain conditions. This substance is decomposed in the presence of an excess of steam or water vapor into sulfuric acid and nitric oxide, or better, nitrogen trioxide, N2O3. While the exact formulation of the intermediate compounds is not simple under the various conditions, the evidence at hand is sufficient to make the existence of at least one intermediate compound certain. 

Nitrosyl sulfuric acid in industry it is also called lead chamber crystals because of its occurrence as an impurity in the chamber process for manufacture of H3SO4. 

Figure A2.1 Waters ProMonix On-Line HPLC analyzer. The upper compartment door contains a keypad for programming and operation of the analyzer. The upper window allows viewing of indicator lights and a liquid crystal display that provides the operator with analyzer interface, programmed parameters, and instrument status results. The lower chamber contains the pumps, valves, injector, and detector(s) required for the chromatographic separation. The sample conditioning plate for online process monitoring is to the right of the analyzer. This is a typical process HPLC. (From Cotter, R.L. and Li, J.B., Lab Rob Autom., 1, 251,1989. With permission of VCH Publishers.)...

---