Preparation of sulfuric acid
The chamber consists of a 2 or 3 l three-necked Wolff bottle, through the middle neck of which is inserted a two-holed rubber stopper carrying a dropping-funnel and a glass elbow. The other two necks are provided with oneholed rubber stoppers carrying glass tubes of the special form indicated in the figure. Two Liebig condenser jackets filled with broken bits of pumice-stone serve as the Gay-Lussac and Glover towers, respectively. The condenser jackets should have the water-tubes on opposite sides if possible, as otherwise it will be necessary to bend glass tubes to make the proper connections. One of the condensers is clamped in an upright position, its lower end dipping into a small beaker one-third filled with concentrated sulfuric acid. A piece of combustion-tube 25 cm. long is fastened to the lower water-tube of the condenser by means of a rubber stopper, and a small plug of glass wool is thrust into the combustion-tube. A porcelain boat, filled with bits of roll sulfur of such a size as can conveniently pass into the combustion-tube, is inserted part way in the tube. In case the combustion-tube does not remain in a level position, it may be necessary to support it with a ring from the large retort stand.
The upper water-tube of the condenser is connected by a long glass elbow to one of the necks of the Wolff bottle. The second condenser jacket is clamped in a vertical position on the other side of the Wolff bottle, in such a manner that its lower end will be 3 or 4 cm. higher than the upper end of the other condenser. The two condensers are connected by a long, small-bored glass tube, thrust through the corks inserted in the end of the condensers. The glass tube should extend several millimeters below the cork in the top of the lower condenser, and should be just flush with the end of the cork thrust into the lower end of the upper condenser. As this cork is subject to the action of concentrated sulfuric acid, it is best to coat it with paraffin and thrust it, while still warm, into the condenser. Care should be taken in coating the cork that the paraffin does not seal the glass tube by running into it and solidifying. The lower water-tube of the upper condenser is connected with a long glass elbow to the third neck of the Wolff bottle. The upper water-tube is connected with a suction-pump, a gas washing bottle containing water being inserted at some point between the condenser tube and the pump. A one-holed rubber stopper, carrying a dropping-funnel filled with concentrated sulfuric acid, is inserted in the upper end of the upper condenser. Concentrated sulfuric acid is allowed to flow down over the pumice-stone in the upper condenser, which it thoroughly drenches. The acid collects in the bottom of the condenser and flows through the small tube into the lower condenser, trickling down over the pumice-stone, and finally is collected in the beaker. The following arrangement is provided for sending water vapor through the glass elbow in the middle neck of the Wolff bottle. A 100 ml Erlenmeyer flask, one-fourth filled with water, is fitted with a two-holed rubber stopper. A glass elbow, 7 mm. in diameter, is thrust through one hole in the cork, and a small glass elbow, 2 mm. in diameter, is thrust through the second hole. The large elbow carries a piece of rubber tubing and a pinch-cock. The small elbow is connected with the elbow leading into the middle neck of the Wolff bottle. The flask is supported on a stand and gently warmed with a Bunsen burner, the water being kept at or near boiling. The pinch-cock should be moved up on the glass elbow, thus allowing free escape for the water vapor through the large glass elbow and the rubber tube. Steam condenses in one end of the small glass elbow, and the drop clinging to the end of the tube prevents the escape of the steam into the Wolff bottle. When it is desired to introduce steam into the acid chamber, the flame is raised and the water in the flask brought to a vigorous boil. By closing the rubber tube on the large elbow with the pinchcock, the steam forces its way through the small elbow into the acid chamber. On releasing the pinch-cock, the steam issues from the large elbow into the air of the room, as before. A few bits of pumice-stone or glass beads promote the regularity of ebullition. The preparation of sulfuric acid by means of this apparatus is extremely simple. Ten to fifteen drops of fuming nitric acid are allowed to fall into the Wolff bottle, which should be perfectly dry. If the stem of the dropping-funnel has been previously filled with acid, the regulation of the dropping will be much simplified. The boat containing sulfur is then drawn halfway out of the tube, and the sulfur strongly ignited by heating with a lamp. When burning well, the suction is started and air drawn through the combustion-tube over the burning sulfur into the apparatus. After the current of air is started, it is necessary to maintain it at a rate just sufficient to draw the flame of the burning sulfur into the combustion-tube. In this manner a mixture of air and sulfur dioxide is carried into the chamber. After a few moments the walls of the flask will become covered with a deposit of chamber crystals. Water vapor is then admitted, and consequently the chamber crystals are decomposed with the liberation of nitrous fumes. The formation of chamber crystals, being dependent on a certain proportion of water, nitric oxide, and sulfuric acid, is a matter of considerable difficulty, and cannot always be relied on. When the operation is carried out as described, however, the chamber crystals are, as a rule, readily obtained. The yield and concentration are determined by titration of an aliquot with base or by specific gravity. Usually sulfuric acid prepared by the “chamber process” is less than 70% concentration.
Chemical lecture experiments, by F. G. Benedict, 168-173, 1916.
SULFURIC ACID, sulfuric acid, Oil of vitriol, Dihydrogen sulfate, Battery acid, Dipping acid, Mattling acid, Acide sulfurique, Electrolyte acid, Acidum sulfuricum, Vitriol Brown Oil, H2SO4, Schwefelsaeureloesungen, sulfuricacid, Schwefelsaeure, 7664-93-9, Acido solforico, Acido sulfurico, Oil of vitreol, Methanolic H2SO4, Zwavelzuuroplossingen, Sulfuric acid, spent, Sulfuric acid solution, Caswell No. 815, UNII-O40UQP6WCF, Acide sulfurique [French], Acido solforico [Italian], Acido sulfurico [Spanish], Zwavelzuuroplossingen [Dutch], Sulfuric acid standard solution, Schwefelsaeureloesungen [German], CHEBI:26836, HSDB 1811, QAOWNCQODCNURD-UHFFFAOYSA-N, EINECS 231-639-5, UN1830, UN1832, UN2796, Sulfuric acid (NF), Sulfuric acid [NF], EPA Pesticide Chemical Code 078001, Sulfuric acid [Strong inorganic acid mists containing sulfuric acid], BOV, Sulfuric acid contained in strong inorganic acid mists, sulfuric acid (acid aerosols including mists, vapors, gas, fog and other airborne forms of any particle size), suiphuric acid, sulfate ester, sulfate esters, sulfuric esters, sulfuric-acid, Nordhausen acid, suIfuric acid, Matting acid, sulfur-ic acid, Spirit of alum, Vitriol, oil of, Spirit of vitriol, sulfuric acid ester, sulfuric acid esters, tetraoxosulfuric acid, dihydroxidodioxidosulfur, Sulfur oxide (SO4), Sulfuric acid, diluted, Sulfuric acid (1+1), Sulfuric acid (1+2), dihydrogen tetraoxosulfate, Sulfuric acid concentrate, AC1L1ARK, AC1Q7DND, DSSTox_CID_9683, O40UQP6WCF, Dieuropium(3+) trisulphate, DSSTox_RID_78807, hydrogen tetraoxosulfate(VI), NCIOpen2_006177, DSSTox_GSID_29683, hydrogen tetraoxosulfate(2-), KSC378E6L, UN 1830 (Salt/Mix), UN 1832 (Salt/Mix), UN 2796 (Salt/Mix), 40254_ALDRICH, 40306_ALDRICH, 07208_RIEDEL, 30736_RIEDEL, 30741_RIEDEL, 30743_RIEDEL, 319570_ALDRICH, 319589_ALDRICH, 339741_ALDRICH, 35276_RIEDEL, 35347_RIEDEL, 35348_RIEDEL, 35354_RIEDEL, 35355_RIEDEL, 35357_RIEDEL, 35358_RIEDEL, 380075_ALDRICH, 38290_RIEDEL, 38291_RIEDEL, 38292_RIEDEL, 38294_RIEDEL, 38295_RIEDEL, 38308_RIEDEL, 40254_RIEDEL, 40306_RIEDEL, 506516_SUPELCO, CHEMBL572964, O2S(OH)2, Sulfuric acid with >51% acid, 00646_FLUKA, 00647_FLUKA, 03364_FLUKA, 2,4 – dimethoxy – bromophenyl, 30741_FLUKA, 35276_FLUKA, 35347_FLUKA, 35348_FLUKA, 35354_FLUKA, 35355_FLUKA, 35357_FLUKA, 35358_FLUKA, 38291_FLUKA, 38292_FLUKA, 38294_FLUKA, 38295_FLUKA, 38308_FLUKA, 68279_FLUKA, 77239_FLUKA, 84525_FLUKA, 84716_FLUKA, 84722_FLUKA, 84723_FLUKA, 84724_FLUKA, 84727_FLUKA, 84733_FLUKA, 84736_FLUKA, 84741_FLUKA, 93124_FLUKA, CHEBI:26819, CTK2H8265, 319570_FLUKA, 319589_FLUKA, MolPort-003-925-007, [S(OH)2O2], [SO2(OH)2], 07208_SIAL, 30736_SIAL, 30743_SIAL, 84724_SIAL, 84736_SIAL, Sulfuric acid with not >51% acid, 258105_SIAL, 270113_SIAL, 320501_SIAL, 323551_SIAL, 357413_SIAL, 375616_SIAL, 435589_SIAL, 435597_SIAL, ACT13112, NSC38965, EINECS 236-903-3, Tox21_200483, DNC005113, NSC-38965, NSC248648, CCG-221344, LS-3225, MCULE-1504889908, NSC-248648, RL04919, NCGC00248653-01, NCGC00258037-01, E513, SC-65200, CAS-7664-93-9, Sulfate standard concentrate 10.00 g SO42-, Sulfuric acid, spent [UN1832] [Corrosive], C00059, D05963, Sulfuric acid, spent [UN1832] [Corrosive], 3B4-0324, I04-12533, Sulfuric acid with >51% acid [UN1830] [Corrosive], I14-108434, Sulfuric acid with >51% acid [UN1830] [Corrosive], 7370A083-F259-4C3E-A455-B5FA1E3C8CB7, Sulfuric acid with not >51% acid [UN2796] [Corrosive], Sulfuric acid with not >51% acid [UN2796] [Corrosive], Sulfate atomic spectroscopy standard concentrate 10.00 g SO42-, Zinc(2+),1′,1”,1”’-(1,2-ethanediyldinitrilo)tetrakis[2-propanol]]-, sulfate (1:1), 119540-51-1, 127529-01-5, 12772-98-4, 140623-70-7
sulfate, Hydrogen sulfate, Sulfate ion, Unknown Ligand, Sulfuric anhydride, Protamines, sulfates, DIPA, OLEUM, DIISOPROPYLAMINE, Sulfuric acid, fuming, SODIUM SULFATE, 2-Fluoro-4-nitrobenzotrifluoride, CID1118, C033158, 10404-39-4, 13537-15-0, 28831-55-2, 507-18-6, 6202-05-7, 9009-65-8, SO4, UNL