Barium Hydroxide Solution Research Articles

Determination of organic acids in silage by silica gel chromatography

AbstractA method is described for the separation of butyric, propionic, acetic, formic, succinic and lactic acids from silage extracts by chromatography on columns of silica gel eluted with mixtures of benzene and n‐butanol. Separated acids were estimated by titration with barium hydroxide solution. The method has been applied to silages made from pure species of herbages at different stages of growth and receiving different treatments before ensilage.Lactic acid concentrations up to 11.5% of the dry matter were recorded, giving rise to low pH values. Butyric acid concentrations of up to 5% raised the pH and under these conditions only small amounts of lactic acid were present; propionic acid concentrations rose to 1–2% in some cases and trace amounts of formic acid could be detected. Acetic acid was present in all silages at concentrations of up to 7% of the dry matter, and appeared to fall off as the nitrogen content of the crop decreased. As the herbage matured, the total acid concentration of the silage decreased.

Acid of Krypton and Its Barium Salt

An acid of krypton is formed when krypton tetrafluoride is slowly hydrolyzed by ice at -30 degrees to -60 degrees C. The yield is 2 to 3 percent (mole). A barium salt of this acid, thermally stable at room temperature, is formed by the hydrolysis of krypton tetrafluoride with a 0.35N solution of barium hydroxide at O degrees to 5 degrees C in a yield of approximately 7 percent by weight.

Studies on the 2-phenylglycine derivatives having antispasmodic activity and their related compounds. IV. Syntheses of 1-2-alkylaminoethyl)-5-arylhydantoins

A number of 1-(2-alklaminoethyl)-5-phenylhydantoins were synthesized by the amination of 1-(2-bromoethyl)-5-phenylhydantoins. Some new N-substituted 2-phenylglycines were obtained by their hydrolysis with barium hydroxide solution under high pressure.

Die analytische anwendung der kohlendioxyddestillation: Destillations- und titrationsmethode zur bestimmung des sich bei der totalen oxydation von organischen stoffen bildenden kohlendioxyds

Organic materials in aqueous solution are determined by the carbon dioxide formed by complete oxidation. This is distilled in a special apparatus into barium hydroxide solution covered with pentane and the excess of alkali titrated, 0.06–6 mg of organic carbon can be determined.

Synthesis of 1-Amino-2-hydroxyanthraquinone

1-Amino-2-hydroxyanthraquinone was synthesized from ammonolysis of 1-chloro-2-hydroxyanthraquinone. 1-Chloro-2-aminoanthraquinone in conc. sulfuric acid was diazotized with sodium nitrite and decomposition by heating for 30min. at 150°C yielded 87% of theory of 1-chloro-2-hydroxyanthraquinone, mp 226.9-7.6°C. Ammonolysis of 1-chloro-2-hydroxyanthraquinone was completed by heating for 6 hrs. at 100°C in 15 times of its weight of 28% aqueous ammonia and 0.1 mole copper sulfate catalyst. Alkali insoluble portion and aqueous barium hydroxide solution insoluble portion were removed and recrystallization of the product from 50% aqueous solution of ethanol gave red needles. However, this was not a pure 1-amino-2-hydroxyanthraquinone but contained yellow colored 1-chloro-2-hydroxyanthraquinone and others as impurities from the result of examinations by alumina column chromatography, paper chromatography, and spectrometric analysis. The purity was found to be 93% by spectrometric analysis and this can be utilizable for synthesis of intermediate of anthraquinone-oxazole dyes.

Determination of carbon on non-conducting catalysts by induction heating-conductometric method

A method is described for the determination of carbon in non-conducting synthetic catalysts. Carbon is oxidized in a high frequency induction furnace and the evolved carbon dioxide is absorbed in a solution of barium hydroxide. The change in conductivity of this solution is directly proportional to the carbon burned. The method is rapid and reasonably precise at the 0.05% carbon level. Une méthode est décrite pour le dosage rapide du carbone dans des catalyseurs. On procède par combustion dans un four à induction, à haute fréquence. L'anhydride carbonique obtenu est absorbé dans une solution d'hydroxyde de baryum. La variation de conductibilité de cette solution est proportionnelle à la quantité de carbone brûlée. La méthode est rapide et d'une précision satisfaisante au niveau de 0.05% de carbone. Beschreibung einer Schnell-methode zur Bestimmung des Kohlenstoffs in Katalysatoren durch Verbrennung in einem Hochfrequenz-Induktionsofen. Das gebildete Kohlendioxyd wird in Barytlauge absorbiert und die Änderung der Leitfähigkeit gemessen; diese ist dem Kohlenstoffgehalt direkt proportional. Die Exaktheit der Methode ist bei 0.05% Kohlenstoffgehalt zufriedenstellend.

松柏類および近縁植物の成分 (第35報)

Decomposition of sciadopitysin trimethyl ether by boiling in methanolic barium hydroxide solution afforded xanthoxylin, anisic acid, and a substance B, all of which were isolated in fair yield. This fact would be difficult to explain by the structure (I) assumed for sciadopitysin proposed earlier and a new formula (II) was proposed for its trimethyl ether. It was considered that the substance B is a biphenyl derivative (III).

Corrosion of silicate glasses by alkaline solutions Communication 5. Effect of alkali concentration on the degree of destruction of glass

1. An increase in concentration of sodium hydroxide solutions from 0.5 to 10 N affects the degree of corrosion of silicate glasses variously: glasses rich in silica are attacked proportionally to the alkali concentration, the destructive action on glasses rich in lead, zinc, cadmium, or magnesium is at first increased and then retarded as a result of the accumulation in the solution of anion-inhibitors and the formation of protective layers of magnesium hydroxide, and glasses rich in calcium, strontium, or bariumare attacked to the same extent by all solutions in the concentration range investigated. 2. An increase in the concentration of strontium or barium hydroxide solutions leads to a decrease in the corrosion of silicate glasses as a result of the formation on the surface of the glass of alkali-stable compounds.

海人草有効成分ならびに関連化合物の研究 第73報

Ethyl 2-oxo-5-isopropyl-4-piperidineacetate (Ia) was derived to its 3, 3-dichloride (IIa), boiled with barium hydroxide solution, and 2-oxo-3-chloro-5-isopropyl-3-piperideine-4-acetic acid (VIa) was isolated from its reaction product. Catalytic reduction of (VIa) afforded both DL-α- (VIIIa) and DL-β-dihydroallokainic acid (IXa) at the same time. (VIIIa) was also obtained by retrokainin inversion of (IXa) and its kainin inversion afforded DL-N-acetyl-β-dihydroallokainic anhydride (X). DL-N-Acetyl-β-dihydro allokainic acid (XI), formed by treatment of (X) with water, was also obtained by treatment of (IX) with acetic anhydride and water. L- and D-α-Dihydroallokainic acids (XVI and XVII) were obtained by optical resolution of (VIIIa) with d- and l-ephedrine.Treatment of ethyl 2-oxo-5-propyl-4-piperidineacetate (Ib) with barium hydroxide, same as (Ia) afforded 5-propyl analog (VIb) of (VIa) and two kinds of stereoisomers (VIIIb and IXb) of 2-carboxy-4-propyl-3-pyrrolidineacetic acid. The structure of pyrrolinecarboxylic acid derivatives (Va, b) as precursor of these products was presumed.

海人草有効成分ならびに関連化合物の研究 第75報

Ethyl 2-oxo-5-(2-dimethylaminopropyl)-4-piperidineacetate (I) was derived to its 3, 3-dichloride (III) by the application of sulfuryl chloride and thionyl chloride and a pyrrolinecarboxylic acid derivative (IV) was obtained by boiling (III) in barium hydroxide solution. Ethyl 1, 2-diethoxycarbonyl-4-(2-dimethylaminopropyl)-3-pyrrolidineacetate (VI) was obtained from a proline derivative formed by reducution of (IV). Treatment of the methiodide of (VI) was found to effect rapid betainization and pyrolysis of this betaine under a reduced pressure was found to result in the formation of a mixed basic methyl and ethyl esters (VII) and a mixed unsaturated methyl and ethyl esters (VIII). Reaction mechanism of this new pyrolysis of betaine was presumed. Saponification of (VIII) afforded 2-carboxy-4-allyl-(and -propenyl)-3-pyrrolidineacetic acids.

The Effect of Cold Work and Heat Treatment On the Rate of Dissolution of Pure and of Impure Aluminum in Acids and Bases

Abstract The rate of dissolution of a 99.99 percent pure, one way cold rolled aluminum sheet as received was determined in 1 N hydrofluoric acid, and compared with the rates obtained with a 400 to 575 C recrystallized aluminum specimen of the same quality. No significant differences in rates could be detected. There also was no difference in the dissolution rates of surfaces cut under different angles with respect to the direction of cold rolling. The same dissolution behavior was observed with 99.998 percent pure aluminum in 0.5 N barium hydroxide solutions; there was no difference in rates of the cold rolled and recrystallized samples, except for cold hammered samples, which showed higher rates. Differential heat treatment of aluminum alloys (with 1 and 2 percent copper), however, produced different rates; the samples heat treated at 200 C exhibited lower rates of dissolution. The conclusion reached is that cold work itself evidently does not influence the rates of dissolution of aluminum in hydrofluori...

New Volumetric Determination of Sodium Content in Crude Industrial Salt

There has been no satisfactory direct method so far for the determination of the content of sodium in industrial salt and the practical method available at present necessitates an indirect calculation of all components to as certain the content of sodium. The present study was undertaken to establish a new process for determining sodium contents in industrial salt by a direct and rapid quantitative analysis. As a step in the process, the crude industrial salt is dissolved in a small quantity of distilled water, to which a solution of barium hydroxide is added, the solution is boiled, and filtered in order to eliminate all traces of sulfate ion as barium sulfate. Silver carbonate and silver oxide are then added to the filtrate, boiled, filtered again to eliminate chloride as silver chloride, and magnesium, calcium and the excess barium ions are elimated as carbonate and hydroxide. In this manner, the resulting filtrate containing only carbonate and hydroxide of sodium (including potassium) is directly determined by usual titration with 1/5N nitric acid. The results of blank tests by this method on a synthetically mixed salt consisting of an extra pure sodium chloride and known percentages of impurities as sulfate, magnesium and barium ions were highly satisfactory even for those with greater amount of added impurities than are found in commercial grades of industrial salts. The new process made possible to determine sodium content in industrial salts more accurately than the usual method practiced at present. Also, the process requires less than two hours in the analytical procedure.

Electrolyte balances following total body x-irradiation.

One of the prominent features of irradiation sickness is the attendant upset of salt and water metabolism. Depending upon the species, this may be manifested in the forms of vomiting, diarrhea, and diuresis. An exact determination of the changes in electrolyte balance following total body x-irradiation is, therefore, of interest.Methods. Twenty 250 g male white rats (Rolfsmeyer Co., Madison, Wisconsin) were placed in metabolism cages over siliconized glass funnels, and allowed free access to distilled water and a diet containing 60% sucrose, 18% lactalbumin, 16.9% Crisco, 4% modified Wesson salt mixture (minus its Na+, K+, and Cl), 1% liver extract (Wilson Co., liver fraction D. Lot 41863), 0.1% choline hydrochloride, with supplements of thiamine, pyridoxine, riboflavin and calcium pantothenate. Roughly 5% of the Na+, K+, and Cl intake was furnished by the diet; coming largely from the liver extract. The remainder of the sodium and potassium chlorides was administered daily by intraperitoneal injection. In the control period the average total electrolyte intake was 1.55 meq of sodium. 2.37 meq of potassium, and 2.54 meq of chloride per 48-hour period. Under these conditions the electrolyte intake was largely independent of the level of food intake. Each 48 hours, the food intake and body weight were recorded, and the excreta were removed for analysis. The excreta were collected quantitatively in barium hydroxide solution, evaporated to dryness, and ashed at 500°C for 12 hours. Sodium and potassium determinations were made on food, injection solutions, and excreta, with a flame photometer attachment to the Beckman DU Spectrophotometer. Chlorides were determined on the same samples by the Volhard method.

The Thyroxine Content of Thyroactive Iodinated Proteins as Determined by a Radioactive Isotope Dilution Technique

Sumamry A procedure is described for the determination of thyroxine in thyroactive iodinated proteins by an isotope dilution technique employing radioactive thyroxine. It is shown that during hydrolysis in 40% barium hydroxide solution and subsequent isolation no significant exchange of iodine occurs between radioactive thyroxine and iodide. Analyses on seven different samples yielded an average true thyroxine value of 1.04 ± 0.049%. The average apparent thyroxine content (n-butanol soluble fraction) was 3.24 ± 0.429%. The “true” thyroxine thus comprised roughly one-third of the apparent thyroxine value.

ニトロベンゼンスルフォンアミド誘導体の転位反応 (第1報)

It was found that when N-acetoactyl-p- or -o-nitrobenzenesulfonamide in aqueous solution of sodium hydroxide, carbonate, or bicarbonate, magnesium, calcium, or barium hydroxide, ammonia, or sodium cyanide, is allowed to stand at a room temperature or heated at 80-90°, a conversion reaction unknown to date in literature occurs, with liberation of sulfurous acid. It was confirmed that p- or o-nitrophenylacetamide is obtained in 73-92% yield. This reaction did not occur with compounds with substituents other than the nitro radical.

A microrespirometer for simultaneous measurement of O 2-consumption and CO 2-production and its use in determining the respiratory quotient of tissue cultures

Summary o I. A microrespirometer was described with the following characteristics: 1. O 2 -consumption and CO 2 -production may be measured simultaneouslyand independent of each other. O 2 -consumption is measured volumetrically. CO 2 -production is measured by determining the change in electric conductivity of a bariumhydroxide solution. 2. Measurement sensitivity is 0.001 mm 3 for O 2 , and 0.01 mm 3 for CO 2 . II. The Respiratory Quotient of proliferating fibroblasts in vitro was measuredand it appeared to be 1.0.

MICRO METHOD OF DETERMINING CARBON IN PORCELAIN AND THE TRANSLUCENCY OF PORCELAIN

The carbon content in porcelain was determined by the application of the micromethod proposed by M. H. Kalina and T. L. Joseph (Blast Furnace and Steel Plant, 1939, 345-351) for carbon in steel. Specimens of porcelain were powdered to pass 130 mesh per inch and fused with red lead in a platinum boat in a current of oxygen. The carbon dioxide evolved was absorbed with barium hydroxide solution. Excess barium hydroxide was titrated back.As a measure of translucency, the extinction coefficient of porcelain thin plate was measured by a Hartmann microphotometer.A few examples of the measured results are shown in the following.Specimens were taken out from several parts of a working tunnel kiln. The water absorption and the carbon content of these specimens were measured. The results are shown in Fig. 3 (I&II). It was shown that the carbon content of specimens fired the range of 900° to 1000°C was about 0.03%, and it was reduced to about 0.01% before the beginning of the vitrification.

The Saponin of Fenugreek Seeds

THE presence of a saponin in the seeds of Trigonella Foenum graecum (Leguminosae) was first reported by Wunschendorff1, who had subjected the defatted seeds to a process of extraction with alcohol. He obtained from the alcoholic extract a gelatinous precipitate which was afterwards dissolved in alcohol and reprecipitated with ether. Wunschendorff described the product so obtained as a white semicrystalline powder, m.p. 214–215°, which gave a yellow colour test with concentrated sulphuric acid, and a white precipitate with barium hydroxide solution. However, he could not assign a definite formula to the saponin, but showed that it gives by hydrolysis a reducing sugar and water-insoluble sapogenin.

The preparation of oxygen by electrolysis of baryta

Morley, in his classical researches, pointed out that various impurities were present in the gases produced by electrolysis of sulphuric acid and potassium hydroxide solutions. Using the latter method, Lord Rayleigh, by addition of a small quantity of baryta, attempted to minimize the amount of hydrocarbons present in the hydrogen as impurity, derived from the carbonate present in the alkali. Baker pointed out that the action of baryta on potassium carbonate is a reversible one, particularly in the presence of such a large excess of potash, and concluded that Rayleigh's precaution might not be particularly effective. Baker recommended the electrolysis of pure barium hydroxide solution, in which barium carbonate is insoluble, and which consequently must give hydrogen tree from hydrocarbons. He also noted that, with the use of pure baryta solution, the oxygen is apparently free from ozone and hydrogen peroxide. It is to be noted that Baker gave no details concerning the shape and material of his electrodes, or of the currents employed in the electrolysis. The method of electrolysing baryta, using nickel electrodes has become a standard method of preparing small quantities of pure oxygen. The present author has employed the apparatus shown in fig. 1 for this purpose during the past few months. The apparatus consists of two vessels, A and B, constructed from 1-inch internal diameter tubing, carrying nickel electrodes, the upper ends of which are welded to platinum wires sealed through the glass, the seals being sufficiently strong to allow currents up to 2 amperes to pass without cracking the glass. The use of nickel is justified owing to its low hydrogen and oxygen over-voltages. The electrodes are constructed from 18 S. W. O. pure nickel wire, 3 feet of which is coiled up as shown. These electrodes have a fairly large surface area—approximately 34 sq cm. The baryta solution was saturated at room temperature and a layer of pure barium hydroxide was allowed to settle on the bottom of the outer jar. The electrolysis was carried out, using a current of 1 ampere, which kept the temperature of the solution at about 60°C. The oxygen was used in experiments, and was found at first to be highly satisfactory.

Colorimetric Detection of Barbital and its Applications

Barbital and other barbituric acid derivatives are usually detected by recrystallization (Bachem), and only few chemical tests for their identity have been described. Most of these tests are obviously crude and unsatisfactory, or at least not specific. One cannot test for the presence of barbital with Millon's reagent, Denigès' reagent, phenylhydrazine and sodium nitroprusside, or sulphuric acid and naphthol (Parri). The murexide test of Handorf is likewise not sufficiently specific. Parri, Zwikker, and Bodendorf used cobaltous salts for the detection of barbiturates, but proved neither the specificity of their tests, nor did they attempt to make them sensitive beyond 1 part in 2000. We devised the following test for the determination of barbiturates. We acidulate the unknown solution with hydrochloric acid, and shake with 10 volumes of chloroform in a separatory funnel. Six cc. of the chloroform extract are divided into 3 equal parts, A, B, and C. To A we add 0.05 cc. of a 1% solution of cobalt acetate in absolute methyl alcohol; to B, 0.1 cc.; and to C, 0.2 cc. of the same. This gives no color beyond a dilution of the original color of the cobalt acetate solution. Then to A we add 0.1 cc. of 1% barium hydroxide solution in absolute methyl alcohol; to B we add 0.2 cc., and to C 0.4 cc. of the same. If malonyl urea derivatives are present in the extract, a blue color always appears in A, may appear in B, or even in C, according to the amount of barbiturates contained therein. This step gives us an approximate idea of the concentration of barbiturates in the solution, for we have found that small amounts of barbital react only to small amounts of the reagents.