Amount Of Sulphuric Acid Research Articles

Modifications of standard methods for coal analysis for sulphur and nitrogen determinations in oil shales

Investigations were made to determine if methods that are satisfactory for determining total sulphur and total nitrogen in coals are also suitable for determinations when using compounds that contain some organic structures to be expected in oil shale kerogens. Sulphur recoveries in an excess of 98%, and typically better than 99%, were obtained using modifications of ASTM method D3177 (75). It was found that the semi-micro Kjeldahl method in the BS 1016 : Part 6 : 1977 was not suitable for the determination of nitrogen in aromatic nitrogen compounds. For example, the recovery of nitrogen from 8-hydroxyquinoline was increased from approximately 30 to 96% by increasing the digestion time to a minimum of 2 h. Variation in the initial amount of sulphuric acid in the digestion mixture between 3 and 5 ml did not alter the recovery. The use of the modified semi-micro Kjeldahl method for an oil shale sample gave a higher nitrogen recovery and better precision of results than the unmodified standard method.

Alkylation of Phenol with Olefins in the Presence of Sulphuric Acid

Alkylphenols have been synthesised in high yield by the alkylation of phenol with olefins (C6-C8) in the presence of sulphuric acid. The effects of the variation of temperature, molar ratio of phenol to olefin, time of reaction, concentraction and amount of sulphuric acid have also been studied on the reactions.Keywords: Alkylation, Phenol, Sulphuric Aciddoi: 10.3329/bjsir.v44i1.2722 Bangladesh J. Sci. Ind. Res. 44(1), 131-136, 2009

Benzylation of Phenol with Benzyl Alcohol in the Presence of Sulphuric Acid

Benzylphenol has been produced in high yield by the benzylation of phenol with benzyl alcohol in the presence of sulphuric acid. The effect of variation of temperature, molar ratio of phenol to benzyl alcohol, time of reaction, concentration and amount of sulphuric acid have been studied on the reaction. 
 
 Bangladesh J. Sci. Ind. Res. 41(3-4), 257-261, 2006

Factors influencing the mode of thermal decomposition of zirconium sulphate tetrahydrate

The thermal decomposition process of zirconium sulphate tetrahydrate has been studied. Dehydration, which takes place via a crystalline monohydrate phase, is accompanied by the loss of small amounts of sulphuric acid apparently resulting from internal hydrolysis of the compound. This process gives a non-stoicheiometric zirconium sulphate which may exist in several modifications depending on the vapour pressure of the sulphuric acid around the sample during dehydration. The vapour pressure of the sulphuric acid is in turn controlled by such factors as the particle size of the tetrahydrate preparation, the size of sample, and the temperature and technique used during heating. Equilibration experiments have shown that a-Zr(SO4)2 is the stable anhydrous form. The X-ray powder diffraction patterns of a- and γ- Zr(SO4)2 have been indexed. Above 650� all forms of Zr(SO4)2 decompose to cubic ZrO2 which transforms to monoclinic ZrO2 at 800�.

THE RAPID DETERMINATION OF PHTHALODINITRILE

Phthalic anhydride reacts with hydroquinone in sulphuric acid, and changes into quinizarin. Phthalodinitrile can be determined as the yellow benzene solution of quinizarin using this reaction. Though this method is very simple, the temperature of reaction and the amount of sulphuric acid or hydroquinone affect the yield of quinizarin delicately. So the conditions of reaction should be controlled severely.

Über den einfluss der Kristallgitterstörungen von Bleipulver auf dessen Schwefelsäure-Aufnahmefähigkeit

It is established that the quantity of sulphuric acid which is needed for the intimate mixing of lead powder and lead oxide is independent of lattice defects. With technical powders which contain tetragonal lead oxide as well as metallic lead with a disturbed crystal lattice, heating in an inert gas atmosphere reduces the sulphuric acid uptake from 16·6 to 13·0 g H 2SO 4 per 100 g of powder. By contrast, a well formed tetragonal lead oxide submitted to thorough grinding increases its uptake from 9·2 to 18 g H 2SO 4 per 100 g of powder and, after trituration, exhibits a disturbed crystal lattice.

THE RELATION BETWEEN THE SULPHATE AND NITROGEN CONTENT OF UNSTABILIZED CELLULOSE NITRATE

The sulphate and nitrogen contents of cellulose nitrates prepared from mixed acids containing different amounts of sulphuric acid were compared. The sulphate content showed a tendency to decrease with increasing nitrogen, for instance it was 1.96% for 10.54% and 0.44% for 13.31%. Similar results were obtained with a series of wood cellulose nitrates, for instance 2.40% for 11.01% and 0.91% for 12.47%. With practically the same amount of sulphuric acid in the mixed acid, cellulose nitrates were prepared and the sulphate and nitrogen contents were compared. For unstabilized cotton cellulose nitrates, the sulphate content decreased steadily with increasing nitrogen content. Similar results were obtained with wood cellulose nitrates.

I. COMPARISON OF RESISTANCE OF SIX TIMBERS TO SULPHURIC ACID

Summary Part I describes the relative effect of 3.0 per cent sulphuric acid on six timbers. These were tested by the following combination of methods at atmospheric temperature:— 1a. Determination of hardness and lb. crushing strength in comparison with unexposed control timbers and with control specimens immersed in water. 2a. Quantity of sulphuric acid absorbed and 2b the rate of absorption. 3. Temporary and permanent expansion or shrinkage. 4. Loss of weight of timbers after four weeks' exposure. 5. Colour imparted by the timber to acid, and the condition of the test pieces after immersion and drying. In these tests Balau gave the best results from nearly all aspects; South African Pine was the least satisfactory. For four out of the seven tests Balau, Merbau and Pitch Pine are amongst the three best, and for six out of seven tests they are amongst the first four. No wood tested behaved similar to Californian Redwood in all respects.

Determination of iron in small amounts of biological materials.

SummaryA method is described for determining the amount of iron in small amounts of biological materials. A small amount of sulphuric acid is added to the sample, which is afterwards oxidized by addition of relatively small amounts of fuming nitric acid and hydrogen peroxide. After evaporation to dryness the ferric iron is converted to ferrous iron by hydro-quinone. The iron is determined colorimetrically with o-phenanthroline at a pH of about 3 in a final volume of 2.5 ml. in Beckman's quartz spectrophotometer, model D U, at a wavelength of 508 mμ. The method permits determination of 0.5 γ iron with an accuracy of a few per cent. The method was also tested in the presence of an excess amount of phosphates, copper and zinc. It was tried on organic material in increasing quantities (serum + blood from homo). These experiments made it probable that the method permits determination of iron in ordinary biological materials of a wet weight of anything up to at least 100—125 mg.

Some Observations on the Hardening Process used in Felt Manufacture

The hardening of masses of loose wool under various conditions is studied, the effectiveness of the operation being assessed by measuring the air permeability (on a Cambridge instrument) and the breaking load of samples of the hardened material. It is shown that on a Garson plate hardener maximum hardening is effected by processing for 80 sec., prolonged treatment yielding weaker hardened pads. The use of high steam pressures also tends to produce weak pads. Hardening is more effective in presence of acids than under neutral or alkaline conditions, but if the amount of sulphuric acid exceeds about 2%, degradation occurs. Phosphoric, acetic, and formic acids behave similarly to sulphuric acid at the same pH value, but if the pH is less than 2 the strength of the hardened pad falls. Chlorinated wool is more difficult to harden than unchlorinated wool.

Germination and Development of Heather and the Hydrogen Ion Concentration of the Medium

SEVERAL workers1–3 have shown that, in the field, heather (Calluna vulgaris Salisb.) is found most frequently and attains its maximum development on soils the reactions of which are about pH 4. I have examined the germination and the subsequent seedling development of Calluna seeds planted on agar media adjusted to give a range of reactions. A quantity of 1 per cent British agar was prepared with a form of Knop's solution. This was divided equally between nine flasks. The contents of these were adjusted to pH 2, 3, 4, 5, 6, 7, 8, 9 and 10, respectively, by the addition of the requisite quantities of sulphuric acid or caustic soda. After adjustment, the agar in each flask was poured into six 1-in. boiling tubes to give a depth of agar of about 1½ in. The tubes were plugged and the agar allowed to set. A liberal sowing of Calluna seeds was then made in all tubes.

HYDROGEN EXCHANGE REACTIONS OF PHENOL ETHERS IN ACETIC ACID SOLUTION. PROMOTIVE AND INHIBITORY EFFECTS OF STERIC ORIGIN

As a means of avoiding side reactions which were encountered in earlier studies of hydrogen-deuterium exchange of phenol ethers with ethanol-sulphuric acid mixtures, a new procedure has been devised for the study of exchange reactions in acetic acid. The analysis for deuterium in the carboxyl group of acetic acid is performed by adding methyl magnesium iodide solution to the solution of phenol ether in acetic acid, combustion of the methane so produced, and finally, by determining the density of the water formed in the combustion. As compared with the former procedure, which required fractionation of the reaction mixture to recover the pure constituents, advantages in convenience and accuracy are claimed. Results are reported for the following ethers, reacting at 90 °C. in the presence of trace quantities of sulphuric acid: anisole, o-methylanisole, m-methylanisole, 3,5-dimethylanisole, 2-methylcoumarane, veratrole, di-isobutyl catechol ether, and the cyclic mono- (di-, tri-, and tetra) methylene ethers of catechol. The observed variations in rates are interpreted in part according to whether the conditions imposed by structural alterations favor or constrain the formation of an intermediate cation for which a quinoidal configuration of bonds is required. The role of steric factors is most strikingly demonstrated in the series of cyclic ethers of catechol, constraint being evident at a critical ring size (7-membered ring) and largely absent for either smaller or larger rings.

STUDIES IN THE FORMATION OF DDT

In the condensation of chloral and chlorobenzene in sulphuric acid to yield DDT, the yield of DDT is increased and the rate of formation of DDT decreased by (1) decreased sulphuric acid concentration, (2) decreased molar amount of sulphuric acid, and (3) lowered temperatures. Reversible sulphonation of chlorobenzene is the major side reaction; the presence of 4-chlorobenzene-sulphonic acid reduces the extent of this reaction. Increased yields (based on chloral) can be obtained by using excess chlorobenzene. A mechanism is proposed involving 1-(4-chlorophenyl)-2,2,2-trichloroethanol, which has been isolated from the reaction, and 1-(4-chlorophenyl)-2,2,2-tricholorethyl bisulphate, whose barium salt reacts with chlorobenzene in sulphuric acid to give DDT.

The estimation of sulphur compounds in crude and refined benzoles. Part I

AbstractUntil recently the sulphur compounds in crude benzoles were generally considered to be chiefly carbon disulphide and thiophene, although the presence of other compounds such as sulphides, disulphides and mercaptans had been reported. With the exception of carbon disulphide, methods of estimation had not been accurately worked out and knowledge concerning the exact quantities of other sulphur compounds was scanty. Examination of a large number of crude benzoles in these laboratories had shown that normal high‐temperature benzoles contain approximately half their sulphur content as carbon disulphide. It has been customary to regard the remainder as thiophene and its derivatives, an assumption that is justified to some extent since other sulphur compounds, such as sulphides, behave in the same way as thiopheno during refining by sulphuric acid. For example, although a large number of makes and types of acid‐washed benzoic have been tested, it has always been found that the remaining sulphur, other than as carbon disulphide, was the same for a particular yield of benzole irrespective of the concentration and quantity of sulphuric acid used to obtain this yield.

The reduction of the carcinogenic and dermatitic activity of shale oil recovered from the peritoneal cavities of injected mice

1. A carcinogenic Persian spindle grade oil recovered after 4 days from the peritoneal cavities of injected rabbits showed indications of reduced carcinogenic activity for the skins of mice.2. The activity of a carcinogenic shale oil recovered after 7 days from the peritoneal cavities of injected mice was found to be considerably reduced. The reduction in refractive index and potency of the recovered shale oil showed an obvious parallel to that resulting from certain chemical treatments, namely, treatment of the oil with a certain quantity of sulphuric acid or extraction with alcohol.

RESEARCHES ON FORMYL CELLULOSE (XI)

1. Regenerated cellulose from alkali-cellulose is tried for the esterification.2. The effects of the time of duration on the formylation of the cellulose are studied.3. The relation between the amounts of sulphuric acid used and the contents of formic acid in esters are studied.

菅平大明神澤酸性溪流の生物

During the summer of 1935 and 1937, the writer made ecological studies of an acid stream, Daimyozinzawa, which rises near the top of lit. Azumaya-san, a dormant volcano (ca. 2100 m), and runs down the valley, through the Sugadaira Highland from northeast toward southwest, to a locality about 1100 m above the sea level, where it confluences with Karazawa, a neutral stream. The acid reaction of the water of Daimyozinzawa stream is due to the large amount of sulphuric acid, which seems to be derived from the acid soil around the source of the stream. The pH of the water is 4.9 at, Syowa waterfall, about the middle of the stream, 4.4 or more less at the upper part, and 7.0 at its lowest part.In the acid part of the stream there is no algae, which are usually abundant in some of the neighbouring neutral streams, while a moss, Seapania irrigua (NEEs) DuM., as an unique plant, covers the surface of the stones, submerged in the torrential water. Small quantities of algae, such as Nostoc and Sticliococcus, barely appear in the lower neutral part.Larvae of the water insects, Plecoptera (Nemura, Chloroperla, Isogenus), Tricoptera (Diplectrona, Rhyacophila), and Diptera (Simulium), live under the submerged stones of the acid part. Planaria gonocephala also is found there. Among the Scapania-vegetation, a larva of Chironomidae (Orthocladiinae) and a species of Nematoda abound.A striking feature is that nymphs of the ephemerids, which is an important member of the fauna of Karazawa stream, are never found hero not only in the acid part, but also in the neutral waters.

Electrical Precipitation of Solids From Smelter Gases

The fundamental principles of the process in its simplest form are set forth. It is shown why the Cottrell process during recent years has in a large measure supplanted the bag-house and dust chamber in treating smelter gases. The commonly accepted theory concerning the manner in which the dust particles is charged and precipitated is given. It is pointed out that the thing most important to the operating man is how the particles may be enabled to give up their charge to the electrodes under all conditions, rather than the manner in which they receive it. The various types of treaters in common use are described and discussed. The advantages of straight line treaters over those in which the gases are by-passed are emphasized. It is shown that the gas is ionized much more efficiently for a given power consumption and the construction simplified and reduced by arranging the electrodes in the flue so that their electric fields are in series with each other. It is shown that this is accomplished by causing the gas to flow parallel to the electrostatic lines instead of at right angles to them, as in all other types. The factors of lead and copper metallurgy are given which control the amount of sulphuric acid and water vapor in the gases. It is also pointed out that these things are a measure of the successful operation when treating smelter gases.

Scientific Serials

American Journal of Science, June.—Notes from the Bermudas, by Alexander Agassiz. The story of their present condition is practically that of the Bahamas, with the exception that at the Bermudas we have an epitome, as it were, of the physical changes undergone by the Bahamas. The development of the true reef builders, of the massive corals, is insignificant. Subsidence has brought about the existing outlines of the islands, but there is no evidence to show that the original annular coral reef was formed during subsidence. That reef has disappeared, and nothing is left of it except the remnants of the æolian ledges extending to sixteen or seventeen fathoms outside the reef ledge flats, ledges which owe their existence to the material derived from it: the former æolian hills of the proto-bermudian land.—Discovery of Devonian rocks in California, by J. S. Diller and Charles Schuchert. During the field seasons of 1884 and 1893, the U.S. Geological Survey acquired six lots of Devonian fossils, comprising about thirty species, mostly corals. They demonstrate the undoubted presence of middle Devonian deposits in California, where rocks of this age have long been looked for by geologists, more particularly since the recent discovery of Silurian fossils.—New method of determining the relative affinities of certain acids, by M. Carey Lea. This method is based on the principle that the affinity of any acid is proportional to the amount of base which it can retain in the presence of a strong acid selected as a standard of comparison for all acids. When to free sulphuric acid a salt is added in sufficient quantity to cause the whole of the sulphuric acid to saturate itself with the salt base, it is possible by means of the herapathite test to determine the exact point of such saturation. From this we can deduce the exact nature of the resulting equilibrium. A series of equilibria thus obtained with different salts enables us to determine the comparative strength of the affinities of the acids of these salts. The fact that even small quantities of weak acids added to sulphates will set free a certain quantity of sulphuric acid, can be rendered visible to the eye by a well-marked chemical reaction.—A recent analysis of Pele's Hair and a stalagmite from the lava caves of Kilauea, by A. H. Phillips. The stalagmite is of the kind characteristic of the lava caverns of Kilauea, differing very slightly from Pele's Hair in constitution, but widely from ordinary stalagmites formed by undoubted solution. They are suggestive of fused drops, which falling one on the other are at the time sufficiently plastic to be quite firmly welded together and congealed in a slightly drooping position.

1. Remarks on the Behaviour of Mercury as an Electrode

In this paper the author described numerous experiments, serving to show the modification which occurred in the capillary attraction between mercury on the one hand, and various saline and acid fluids forming parts of active voltaic circles on the other. He also described and showed to the Society the undulatory motions which he had observed in mercury, when forming the cathode of a constant voltaic current in solutions of chloride of sodium, containing small quantities of sulphuric acid.