Concentrated Ammonium Hydroxide Research Articles

Rapid screening and confirmation of amphetamine, methamphetamine, methadone, and methadone metabolite in urine by gas/thin layer chromatography.

A method suitable for large scale screening and confirmation of urine speciments for amphetamine, methamphetamine, methadone, and its primary metabolite (2-ethylidene-1,5-dimethyl-3,3-diphenlypyrrolidine) is described. The drugs are extracted from alkaline urine into an organic solvent. The amphetamine drugs are then back-extracted into a small volume of acid and identified by gas chromatography both as free bases on a 10% Apiezon L-10% KOH column and as their trifluoracetamide derivatives on a 3% OV-17 column. The organic layer, which still contains methadone and its primary metabolite, is analyzed by split-sample thin-layer chromatography using two solvent systems: ethyl acetate: methylene cloride: concentrated ammonium hydroxide (90:10:0.7) and methanol: chloroform: concentrated ammonium hydroxide (74:25:0.8). These solvent systems separate methadone from its primary metabolite without interference from other drugs or urinary substances.

Electron spin resonance studies of interactions of ammonia, copper, and cupriammonia with cellulose

The electron spin resonance spectra (ESR) of complexes of copper with fibrous cotton cellulose under various experimental conditions were determined. Cupric ions dissolved in solutions of strong bases, such as concentrated ammonium hydroxide, sodium hydroxide, and potassium hydroxide, formed complexes with fibrous cotton cellulose. These complexes had paramagnetic resonance properties and generated characteristic ESR spectra. Cupric ions dissolved in solutions of highly ionized neutral salts, such as sodium chloride, formed complexes with cellulose. These complexes also generated the same characteristic ESR spectra as the complexes formed in solutions of strong base. The reaction between cupric ions and cellulose was evidently very rapid and reversible. When the concentration of ammonia was decreased in, or ammonia was removed from, the cupric ion–ammonium hydroxide–cellulose complexes, the paramagnetic resonance properties of the complex were decreased or lost. Similar results were received when potassium hydroxide was removed from the complexes. The compositions of the complexes evidently are variable, that is, under different experimental conditions the relative intensities of the lines of the ESR spectra of the complexes varied, although the hyperfine splittings of the lines were constant. It was concluded that reactions of cupric ions to form complexes with adjacent hydroxyl groups on the cellulose molecule depended on an optimum spatial arrangement of the hydroxyl groups, that is, distance between the groups. Evidently, wetting of cotton cellulosic fibers with solutions of strong bases or neutral salt allowed rotation about the C2–C3 bond to yield this optimum arrangement. When the base or salt was removed, rotation occurred to give less favorable positions of the hydroxyl groups for complexing with cupric ions.

Quantitative determination of lysolecithin and sphingomyelin in phospholipid mixtures by thin-layer chromatography as applied to the thymus of the fmfm mouse

Lysolecithin and sphingomyelin may be readily separated from other phospholipids on thin-layer plates impregnated with silver nitrate using the solvent system chloroform-methanol-concentrated ammonium hydroxide 65:35:8. Quantitation is carried out by determining the phosphorus content of the developed bands. The minimum amount of phospholipid that can be quantitatively determined is that which contains 0.7 micro g of phosphorus. This method has been used for the determination of lysolecithin and sphingomyelin in the tissues of mice having foam-cell reticulosis.

Polarographic analysis based upon solvent extraction with methylisobutylketone

Only few examples of direct polarographic determination of extracted materials in organic solvents are known as yet, because of the difficulty to find a soluble supporting electrolyte in such a solution. Methylisobutylketone (MIBK) containing small amounts of tetraethylammonium hydroxide was distilled using a column packed with helipack and then the distillate at 116°C was further purified by redistillation. The accessible potential range of this distillate in the presence of 0.1 M tetrabutylammonium perchlorate (TBAP) was about +0.7-2.6 volt (vs. SCE). To determine Cu(II), add 5 ml of 30% ammonium citrate, 5 ml of 10% triethanolamine, 15 g of ammonium sulfate and 50 mg of tetraethylammoniumpyrrolidinedithiocarbamate. Adjust the pH to 9.5 with concentrated ammonium hydroxide and dilute to 50 ml with distilled water. Extract the solution with 25 ml of MIBK. Stay for 5 minutes and then add TBAP as the supporting electrolyte. Purge oxygen from the solution with highly purified nitrogen. From the first reduction wave height of Cu(II)pyrrolidinedithiocarbamate, Cu(II) in the range of 5 × 10-58× 10-4 M can be determined successfully. This method can be applied to the determination in ion pair complex system.

Chemical Analysis of the Liquid within a Propagating Stress Corrosion Crack in 70:30 Brass Immersed in Concentrated Ammonium Hydroxide

Abstract Studies were made of the liquid within a stress corrosion crack in 70:30 brass (CDA Alloy No. 260) propagating in 15N ammonium hydroxide containing 8 g/l dissolved copper. The liquid in the crack was isolated for study by removing the sample from the solution, immersing the sample in liquid nitrogen to freeze the liquid within the crack, fracturing the sample, and removing the liquid once it had thawed. Spectrophotometric analysis of the liquid indicated a copper concentration of 14.5 g/l and a zinc concentration of 11.5 g/l after one hour exposure and a crack length of 5 mm. The relative dissolution rates of copper and zinc were 0.57 compared to the 2.3 ratio of these elements in the alloy. The total corrosion rate in the crack was estimated to be 4 × 10−6 g/cm2/min. The corrosion rate of a bulk sample under identical experimental conditions was 5.4 × 10−6 g/cm2/min. The pH within the crack showed no measurable change during crack propagation. The Pourbaix diagram was calculated for pure copper ...

Synthesis of pyrimido[4,5‐e][1,4]oxazepin‐5‐ones

AbstractEighteen novel pyrimido[4,5‐e][1,4]oxazepin‐5‐ones were prepared directly via the reaction of either ethyl 4‐chloro‐2‐phenyl‐5‐pyrimidinecarboxylate (Ia) or ethyl 4‐chloro‐2‐m‐chlorophenyl‐5‐pyrimidinecarboxylate (Ib) with a variety of substituted 2‐(alkylamino)ethanols. A typical example was the preparation of 8,9‐dihydro‐9‐methyl‐2‐phenylpyrimido[4,5‐e][1,4]‐oxazepin‐5(7H)‐one (IIa) from the reaction of Ia with 2‐(methylamino)ethanol. Hydrolytic cleavage of the lactone ring in IIa with sodium hydroxide solution, followed by acidification with hydrochloric acid afforded 4‐[(2‐hydroxyethyl)methylamino]‐2‐phenyl‐5‐pyrimidinecarboxylic acid (IV). Reactions of IIa with concentrated ammonium hydroxide or hydrazine also caused cleavage of the lactone ring, giving the corresponding amide (V) or hydrazide (VI), respectively. Structural assignments were supported by infrared and nuclear magnetic resonance spectra.

Formation of Alkaloid Artifacts in Plant Extracts by the Use of Ammonium Hydroxide and Acetone

Treating plant extracts with ammonium hydroxide and acetone can give rise to the formation of artifacts, which are difficult to distinguish from the actual plant alkaloids. These artifacts give positive reactions with several of the standard qualitative alkaloid test reagents. Similar reactions are also obtained from mixtures of equal volumes of concentrated ammonium hydroxide and acetone.

Ammonia fumigation for reducing green mould wastage in oranges during ethylene degreening

The addition of ammonia to experimental cabinets reduced the development of green mould (Penicillium digitatum) wastage in oranges during ethylene degreening. The treatment consisted of introducing ammonia at a concentration of 6000 p.p.m. (v/v) three times every 24 hours throughout the three or four day degreening period. Ammonia gave excellent control of green mould wastage in wound inoculated oranges in preliminary laboratory tests. In an extensive experiment with Valencia oranges, surface inoculated with spores of P. digitatum, ammonia reduced green mould wastage when fruit was degreened at chamber loads of 25 and 50 per cent. These loads would represent the limits likely to be encountered commercially. The ammonia treatment did not cause rind damage to treated fruit. The evaporation of concentrated ammonium hydroxide solution is a practical and convenient method of adding ammonia to the degreening chamber.

マグロ筋肉の脂質-V

The phosphoaminolipids obtained from cephalins of the muscle of a tuna, Thynnus orientalis, were converted to their dinitrophenyl (DNP) derivatives and applied to the chromatographic separation with a silicic acid/celite (2:1) column and chloroform/methanol to yield a DNP-ethanolamine-containing lipid (I), and amino acid-containing lipids (II), which gave a DNP-serine-containing lipid (II-a) and a mixture of DNP-serine-containing and DNP-threonine-containing lipids (II-b) by rechromatography. Hydrolysis of I with hydrochloric acid yielded DNP-ethanolamine, which gave free ethanolamine by decomposing with concentrated ammonium hydroxide. DNP-serine and-threonine, and free serine and threonine were isolated and identified with the same manner from II-a and II-b respectively. Periodate oxidation of the threonine fraction obtained from DNP-threonine of II-b gave acetaldehyde and glyoxylic acid. Component fatty acids of each fraction were found to be palmitic and oleic acids by paper chromatography. The presence of palmitoyloleoylglycerylphosphoryl esters of ethanolamine, serine and threonine can be supposed.

2‐nitro‐2‐methylpropyl carbamate

2‐Nitro‐2‐methylpropyl carbamate has been prepared by the reaction between 2‐nitro‐2‐methylpropanol‐1 and liquid phosgene followed by amination with concentrated ammonium hydroxide. This new carbamate has been characterized by the formation of certain derivatives.