Chromic acid removal

Chromic acid removes amorphous regions of the polymer morphology, leading to the formation of complex (labyrinthine) cavities on the plastic surface. Some surface oxidation takes place. Improved wettability and bond strength have been ascribed to the topography of etched plastic surfaces rather than the polarity of the surface. ... 

CAUTION. Ethers that have been stored for long periods, particularly in partly-filled bottles, frequently contain small quantities of highly explosive peroxides. The presence of peroxides may be detected either by the per-chromic acid test of qualitative inorganic analysis (addition of an acidified solution of potassium dichromate) or by the liberation of iodine from acidified potassium iodide solution (compare Section 11,47,7). The peroxides are nonvolatile and may accumulate in the flask during the distillation of the ether the residue is explosive and may detonate, when distilled, with sufficient violence to shatter the apparatus and cause serious personal injury. If peroxides are found, they must first be removed by treatment with acidified ferrous sulphate solution (Section 11,47,7) or with sodium sulphite solution or with stannous chloride solution (Section VI, 12). The common extraction solvents diethyl ether and di-tso-propyl ether are particularly prone to the formation of peroxides. 

Copper and Copper-Containing Alloys. Either sulfuric or hydrochloric acid may be used effectively to remove the oxide film on copper (qv) or copper-containing alloys. Mixtures of chromic and sulfuric acids not only remove oxides, but also brighten the metal surface. However, health and safety issues related to chromium(VT) make chromic acid less than desirable. 

When a potential is appHed across the ceU, the sodum and other cations are transported across the membrane to the catholyte compartment. Sodium hydroxide is formed in the catholyte compartment, because of the rise in pH caused by the reduction of water. Any polyvalent cations are precipitated and removed. The purified NaOH may be combined with the sodium bicarbonate from the sodium dichromate process to produce soda ash for the roasting operation. In the anolyte compartment, the pH falls because of the oxidation of water. The increase in acidity results in the formation of chromic acid. When an appropriate concentration of the acid is obtained, the Hquid from the anolyte is sent to the crystallizer, the crystals are removed, and the mother Hquor is recycled to the anolyte compartment of the ceU. The electrolysis is not allowed to completely convert sodium dichromate to chromic acid (76). Patents have been granted for more electrolytic membrane processes for chromic acid and dichromates manufacture (86). 

The technology is primarily applicable to the removal of inorganic fumes, vapors, and gases (e.g., chromic acid, hydrogen sulfide, ammonia, chlorides, fluorides, and SOj) volatile organic compounds (VOC) and particulate matter (PM), including PM less than or equal to 10 micrometers ( m) in aerodynamic diameter (PM,q), PM less than or equal to 2.5 m in aerodynamic diameter (PMj 5), and hazardous air pollutants (HAP) in particulate form (PM ap)-... 

While keeping the collected deuterioammonia at dry ice-isopropyl alcohol temperature, lithium wire (10 mg) is added, followed by a solution of 3/3-hydroxy-5a-cholest-7-en-6-one (161 50 mg) in anhydrous tetrahydrofuran (4 ml). The reaction mixture is stirred for 20 min, the cooling bath is then removed and the ammonia is allowed to boil under reflux for 40 min. A saturated solution of ammonium chloride in tetrahydrofuran is added dropwise until the deep blue color disappears and then the ammonia is allowed to evaporate. The residue is extracted with ether and the organic layer washed with dilute hydrochloric acid and sodium bicarbonate solution and then with water. Drying and evaporation of the solvent gives a semicrystalline residue which is dissolved in acetone and oxidized with 8 N chromic acid solution. After the usual workup the residue is dissolved in methanol containing sodium hydroxide (0.2 g) and heated under reflux for 1 hr to remove any deuterium introduced at C-5 or C-7. (For workup, see section II-B). 

A constant problem in the use of selenium dioxide is the removal of selenium-containing contaminants in the above example it was found necessary to treat the product with chromic acid to remove materials which otherwise poisoned subsequent hydrogenation steps. 

Sorm" " found that when cholesterol acetate (67) is oxidized by chromic acid in acetic acid-water at 55°, crystalline keto seco-acid (69) is obtained in 25-30 % yield from the mother liquors after removal of successive crops of 7-ketocholesterol acetate (68). Reaction of keto acid (69) with benzoyl chloride in pyridine gives a dehydration product, shown" to be the )5-lactone... 

Acid (69)." To a well-stirred mixture of 108 g (0.232 mole) of cholesterol acetate and 1.2 liters of glacial acetic acid is added over a period of 2 hr, a solution of 70 g of chromium trioxide in 200 ml of 50 % glacial acetic acid. The reaction mixture is maintained at a temperature of 55°. Upon completion of the addition, the mixture is stirred for an additional 2 hr at 55°. Excess chromic acid is destroyed by addition of 60 ml of methanol, and then 800 ml of acetic acid is removed by distillation under reduced pressure at a bath temperature of 40°. The remaining liquid is diluted with 50 ml of water and allowed to stand for 12 hr. The crystalline 7-ketocholesterol acetate which separates is removed by filtration and washed with 80 % acetic acid to yield 33.3 g (35%) of (68) mp 149-152°. 

Chromate ions, when used as inhibitors in aqueous solutions, passivate by maintaining a coherent oxide film on the metal surface. Passivation is maintained even in a boiling concentrated chromic acid solution, in which many of the oxides in bulk form are soluble. The passivity breaks down rapidly, however, once the chromate is removed. 

Acid pickles Some of the acid pickles used to clean and etch aluminium alloy surfaces and remove oxide and anodic films, such as the chromic/ sulphuric acid pickle (method O of DEF STAN 03-2) and other chromic-acid bearing pickles (App. Foi DEF-151) probably leave on the surface traces of absorbed or combined chromate which will give at least some protection against mild atmospheres. 

Note in making up the chromic acid solution it is advisable to dissolve the silver nitrate separately and add it to the boiling chromic acid to prevent excessive crystallisation of the silver chromate. The chromic acid must be free from sulphate to avoid attack on the zinc. Immerse each specimen for 15 s in a 6% solution of hydriodic acid at room temperature to remove the remaining corrosion products. Immediately after immersion in the acid bath, wash the samples first in tap water and then in absolute methanol, and dry in air. This procedure removes a little of the zinc and a correction may be necessary. 

Hydrocarbons and carbonized or coke deposits can be removed by chromic acid. The chromic acid oxidizes the binders holding the deposits together. Use a 10 to 20% solution for 12 to 24 hours at 190 to 200 °F. Chromic acid cannot be effectively inhibited and is not suitable for cleaning copper, brass, aluminum, zinc, or cast iron because these are all rapidly attacked. 

Oxidation of isopropyl alcohol (H2R) by chromic acid has been studied in det ai by Westheimer and Novick , and it was found that acetone (R) is formed nearly quantitatively. The reaction proved to be first order with respect to hydrogen chromate and second order with respect to hydrogen ions. Measurements using 2-deutero-2-propanol under identical conditions as those for the oxidation of ordinary isopropyl alcohol showed the rate of reaction to be of that with the hydrogen compound. This fact is considered to prove that the secondary hydrogen atom is removed in the rate-controlling step and that the assumption of hydride-ion abstraction can be excluded. The data are consistent with the following mechanism... 

---