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BRITISH CHEMICAL ABSTRACTS

B.—APPLIED CHEMISTRY

O C TO B ER 28, 1927.

I.— GEN ERAL; PL A N T ; MACHINERY.

Estimation of the efficiency and dispersive power of emulsifying agents. R . C. S m ith (J.S.C.I., 1927, 4 6 , 345—346 t).—The criteria of a good emulsifying agent are (1) for a given quantity the agent should emulsify as large a fraction of the disperse phase as possible ; and (2) the disperse phase should be in as small globules as possible. Two methods are given for the numerical expression of the results. The

“ emulsifying power ” is the fraction of the disperse phase emulsified, and the “ dispersion power ” is the fraction of the total volume occupied by the emulsion.

To obtain one representative figure the product of these two is taken. This method breaks down when a very small quantity of disperse phase is dispersed throughout the whole of the dispersion medium, so a second method is suggested. If unity represents the volume of disperse phase before emulsifying, then the “ dispersion factor ” represents the total volume occupied by emulsion and remaining disperse phase. In all cases equal quantities of dispersion medium and disperse phase are taken.

Tables are given showing typical results.

Inexpensive and accurate gas chain [hydrogen electrode vessel] for liquids lighter than saturated potassium chloride solution. H. C. Waterman

(J. Assoc. Off. Agric. Chem., 1927, 10, 390—395).—A simple type of sharp-junction hydrogen electrode vessel of the bubbling type is described, which requires only a small volume of the solution under examination and ensures the freedom of the latter from potassium chloride contamination and exclusion of carbon dioxide. The apparatus can also be adapted for use with foaming liquids or those containing sediments. F. It. Ennos.

Works viscosim eter. R. Freund (Farben-Ztg., 1927, 32, 2889—2890).—A simplification of the “ falling sphere ” method of determination of viscosity is de­

scribed. The sphere is attached to a suitably marked fine thread which is allowed to slip loosely through the fingers of the operator, the time taken for the sphere to fall through a given distance being observed. I t is not necessary to transfer the sample of fluid under test to a special vessel, and the sphere may readily be recovered, both points of advantage over the usual method. The accuracy, although decreased, is sufficient for normal

works practice. S. S. Woolf.

Flowmeter for gases. E. II. Riesen feld (Chem.- Ztg., 1927, 51, 678—680).—The apparatus consists of a manometer filled with a suitable liquid and provided with scales to each arm. The two arms are joined at the upper end with a horizontal capillary tube which may be sealed to the manometer, attached by

rubber connexions, or provided with a cooling apparatus.

The upper ends of the manometer tubes are provided with bulbs to prevent loss of liquid, and the tube joining the lower end of the tubes is of small bore to hinder rapid movement of the liquid. The diameter of the capillary tube is adjusted to allow of measurement of rates of flow as low as 0 -1 litre /hr. Details of the method of standard­

ising the scale and of the most suitable liquids for differ­

ent purposes are given. A. R. Po w ell.

Tower absorption coefficients. R . C. C a n te lo , C. W. Simmons, E. M. G ile s , and F. A. B r i l l (Ind. Eng.

Chem., 1927,19, 989— 992).— The rate of dissolution of a soluble gas from a gas m ixture in an absorbing liquid is given b y d m / d t = —K ^ ff ir i) , where m is th e concen­

tration of th e gas in th e gas m ixture and K 2th e dissolu­

tion coefficient. This equation was further investigated for the cases of carbon dioxide and sulphur dioxide, a tower packed w ith R aschig rings being used. W ith carbon dioxide it w as found th at ICZ was scarcely affected by changes in th e gas velocity or com position, the flow of w ater and tem perature being constant. W ith increase in w ater flow K 2decreased rapidly to a critical point and then rem ained constant. Solutions of sulphur dioxide a t higher tem peratures follow H enry’s law closely, though there is deviation at lower tem peratures. Under the conditions of th e experim ent K 2increased linearly with the rate of flow of w ater. In each case th e q uan tity I i 2 is calculated from th e q u an tity relationships of gas and solution, tem perature, vapour pressure, H enry

coefficient, etc. C. I r w in .

Pa ten ts.

Kilns. M. M. Min t e r (E.P. 275,858, 18.6.26).—A n a rra n g e m e n t of flues b y w hich th e h e a t fro m a b u rn in g k iln m a y be u sed to p re h e a t a n eig h b o u rin g one an d b y w hich h e a te d air fro m a cooling k iln ca n be delivered

to th e fire doors. B. M. Ven a bles.

Retort. H . J. and H . C. M c E lv a in (U.S.P. 1,642,457, 13.9.27. Appl., 12.6.26).—Concentric, spaced inner and outer rotary cylinders are mounted within an inclined stationary cylinder provided with peripheral intake and discharge openings. The innermost cylinder is the longest, and means are provided for supplying heat within it. The adjacent surfaces of the rotary cylinders carry longitudinal wir.gs. H . H o lm es.

Grinding and separating apparatus. P. L. Crowe

(U.S.P. 1,639,214, 16.8.27. Appl., 20.10.25).—A grind­

ing cylinder provided with apertures is journalled on a base, and a crusher plate is yieldingly urged toward it.

Means are provided for producing a current of air through the apertures for withdrawing the finely-ground

material. H. Holmes.

a

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B r itis h C h e m ic a l A b s tr a c ts — B .

800 Cl. I.— Gen e r a l; Pl a u t; Machinery,

Mixing or pugging m ill. C. J. Cooper and A. M.

Mason (C. J. Cooper & Co.) (E.P. 276,196, 1.11.26).—

The casing is of frusto-conical shape with axis horizontal and outlet a t the -Rader end, but there are two cones, with incomplete circumferences, joined together, and two

sets of beaters or scrapers the blades of which intercalate and overlap ; provision is also m ad e for scraping the ends of the casing. B. M. Ven a bles.

Dryer. G. K om ahek, Assr. to M a lc o lm so n E n g in ­ e e r i n g & M a c h in e C orp. (U.S.P. 1,641,337, 6.9.27.

Appl., 12.2.24).—The space between an inner rotary cylinder and an outer stationary tubular housing con­

stitutes an annular drying chamber. Heating medium is supplied to one end of the cylinder through a heat- regulating chamber and detachable tubular connexions.

H . Holm es.

Drying and heating apparatus. L. B. West

(U.S.P. 1,641,108, 30.8.27. Appl., 19.3.26).—The mate­

rial to be treated is delivered into the space between an outer dryer casing and an inner superheater, conveyed into the superheater, and discharged therefrom. One end of the superheater extends beyond the casing into a draught chamber communicating with the space between them, and hot gases are admitted from a flue to one end of the superheater. Means are provided for rotating the casing and the superheater.

H . Holm es.

[Waterproofing of] tanks, vats, pits, etc. N.

Sw in d in (E.P. 275,316, 3.5.26).—Rubberised cement of known composition (e.g., Portland cement mixed with latex) is applied to the internal surface of the vessel to be waterproofed, and sheets of rubber are then secured to the cement by means of rubber solution.

B. M. Ve n a b l e s.

Separation of m aterials by [vacuum] flotation.

F. E . Elmore (E.P. 275,778, 16.7.26).—The pulp of mineral, water, and oil or other selective agent is drawn up by a vacuum through a vertical feed pipe in a non- turbulent stream, the velocity of the flow being kept constant by increasing the cross-section of the pipe in proportion to the increase in volume of pulp due to the vacuum. In the separating chamber the outlet of the feed pipe is surrounded by baffles forming louvres, and a t about that level also are radial valves to prevent rota­

tion and disturbance of the froth, but below that level, in the zone which ought to be occupied only by non- floatable mineral or gangue, the pulp is put into rotation by tangential, internal water jets in order that any stray particles of float may get clear and rise. The outlet for gangue is provided with a valve which is intermittently opened and produces pulsations which help to prevent channelling and clogging of the float.

B. M. Ve n a b l e s.

Apparatus for the chemical and mechanical treatment of m ixed liquids and solids. T. St een

(G.P. 440,S00, 30.1.25).—Apparatus suitable for dressing heavy spar, for treating ores with acids, and for processes involving the double decomposition of salts comprises a closed vessel fitted with two pumps of the type used for elevating mixtures of gases and liquids (mammut pumps), one of which, with its base set lower in the vessel than the other, serves to mix the material and

to regulate the pressure in the vessel as soon as the second pump, which removes the material from the vessel, comes into operation. L. A. Co les.

Settling apparatus [jigs] for washing granular m aterials. K. andE. Gr o p pe l, A. Waschkau (Ma sc h in- en f a b r. F . Gr o p p e l, C. Lu h r igs Na c h f.), and W . Scholvien (E.P. 253,139, 4.6.26. Conv., 6.6.25).-—In addition to the vertical motion given by the usual cranks or other means, the tray of a jig is given a horizontal motion by means of guides which may be straight inclined, curved partly inclined, or may follow a closed path so that on the upstroke the forward movement takes place after bedding of the material has taken place.

B . M. Ve n a b l e s.

Manufacture of colloidally dispersed material.

S. Cabot (E.P. 246,874, 1.2.26. Conv., 31.1.25).—A permanent colloidal suspension of solids is produced in non-solvent media by kneading the solid with a proportion of a gel substance so small that it is only sufficient to film-coat the solid particles, the materials being in the form of a stiff, plastic, and sticky paste. A small quantity of the dispersion medium may be added during the kneading if necessary to reduce the gel colloid to a soft condition. E.g., 3 pts. by wt. of a titanium oxide- barium sulphate mixture (“ Titanox ”) are kneaded with 1 pt. of linseed oil jelly containing 30% of turpentine, then to the paste are added 1 pt. of raw linseed oil and enough turpentine and drier to make a workable paint in the form of a permanent suspension.

B. M. Ve n a b l e s.

Centrifugal separating apparatus. Br it. Se p a r a­ to rs, Lt d., and A. G. Cah ill (E.P. 276,268, 7.4.27).—

In a separator for liquids where it is desirable for the heavier liquid to carry off any solid matter, light floccu- lent matter will be carried off through the ordinary outlet passages starting near the circumference, but should these become choked by gummy or heavy solids an alternative route is provided for the heavier liquid starting further inwards, but not as far in as the boundary of the lighter liquid. B. M. Ve n a b l e s.

Evaporation of liquids. E. Morterud (E.P.

263,132, 10.12.26. Conv., 19.12.25).—A number of superposed shallow trays or troughs for the liquid are contained in a common vapour chamber, and are heated by steam tubes or other elements which extend vertically through all the trays. The trays are reciprocated ver­

tically, and are provided with scrapers having a certain amount of freedom which surround the heating tubes and keep their exterior surfaces clean. B . M. Ve n a b les.

Recovering dissolved substances from solutions.

Metallban k u. Metallu rg isch e Ges. A.-G. (G.P.

440,237, 7.8.21).—The liquid is allowed to trickle down a series of heated, inclined surfaces in a tower, the length of the individual surfaces, the rate of heating, and the rate of flow of the liquid being so adjusted that the solid material forms a thin incrustation over the heated surfaces and the liquid is entirely evaporated by the time the lowest plate is reached. When a sufficient thickness of solid has accumulated on the plates in the tower, the liquid supply is stopped and heating is continued from outside the tower, a current of hot dry air being passed through so as to dry the deposited solid. A. R. Po w ell.

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B r itis h C h e m ic a l A b s tr a c ts B .

< X I . — GSKERA*.; Pm s t ; Ma c h in e r y.

Filtering apparatus. J. B. Vernay (E..P. 266,719,

■22.2.27. Conv., 24.2.26).'—l a a filter clement for use in a thickening filter, the filtrate is withdrawn by suction from the lower part of the interior of the element, and the compressed air is admitted at the upper part.

B. M, Yenawbs. Apparatus for filtration. N . C. Ch ristensen

(U.S.P. 1,641,736, 6.9.27. Appl„ 194.21).—A chamber

■closed at the sides and top is provided with suspended vertical partitions of filtering medium, arranged to form spaces which are entirely enclosed except fox openings for the application of vacuum and pressure, and means

■are provided for dipping the lower end of the chamber into the mixture to be filtered. H . Holmes.

Filter. E. J. Sw eetland (E.P. 275,333, 5.5.26).—•

A vacuum filter for removing a small quantity of solids from a large quantity of liquid is arranged so that it is operated in cycles of three stages, viz., collecting the cake, removing the cake by reversal of flow of filtrate, settling ; the cake is thrown off into' the same surround­

ing vessel from which the prefilt is taken, and is removed from it by a pump ox conveyor at the bottom. The action of the filter is one of thickening only, the thick pulp

"being finally treated, if desired, in another filter. The filtering period may be 10 times as long as each of the

■other two, and the vacuum is preferably produced by a wet reversible pump, the discharge pipe being taken up vertically and holding just sufficient filtrate to form tho necessary back-wash. The filter cloths are loose on their supporting members, so that they will distort largely on reversal. B. M. Ven a bles.

Filters. E. J. Sw eetland (E.P. 275,779, 23.7.26).—

A number of disc-shaped filter leaves are attached to a hollow shaft and rotated within a casing, which when in use is pressure-tight, but can be slid on rails to permit inspection of the filter. Connexions for prefilt, wash water, air, and drainage are made to the oasing, preferably through separate valves, but with a common detachable joint. The discs are divided into sectors, which are detachable radially, and each row of sectors is conneoted to a separate passage within the shaft. During the Altering stage the discs are rotated slowly. Disoharge is effected by rotating them quickly in wash water.

B. M. Ve n a bles.

Spray drying. Indu stria l Associates In c. (E.P.

272,859, 4.3.27. Conv., 18.6.26).—A spraying chamber is jacketed round the upper part by the incoming hot air and round the lower part by the outgoing moist air.

A cloud of the liquid enters the inner sprayer chamber at the centre of the top, and is surrounded by a stream of the heated air. They move together downwards, the

•chilled moist air leaving by the lower circumference.

There is also a circulation up the sides of less chilled air.

The dried powder is deposited on the bottom, and is removed, e.g., by rotating rakes. B. M. Ve n a b les.

Apparatus for atomising and drying liquids.

A. Nyrop (E.P. 275,404, 21.7.26).—Air is admitted tangentially and in a downward direction to the upper circumference of the drying chamber, and the liquid is centrifugally sprayed through the centre of the top.

The moist air is withdrawn at the centre of the bottom vthrough a pipe which upstands somewhat. The dried

powder is deposited on the bottom.. The air may be admitted in puffs. B. M. Ven a bles.

Atomiser for [corrosive] liquids. F. E. Martin

(E.P. 271,035, 31.12.26. Conv., 12.5.26).—A mechani­

cally driven centrifugal spraying device stated to be suitable for use in sulphuric acid chambers etc. is de­

scribed. The liquid is flung off from, and the drops caught on the next of, several edges in succession, so that eventually all is reduced to fine mist.

B. M- Ven a bles,

Apparatus for the production of freezing liquid.

N, Dahl (E.P. 275,849, 18-12.26).—Brine is caused to flow down through a column of ice without any splashing ox entrainment of air by supplying the brine above a grating surrounding a hopper which is kept full of ice and forms an upward extension of the ice column suffi­

cient to keep ice sunk below the brine in the wider part of the column. Several columns are connected in series, the point of entry to each being slightly lower than the one before ; by this means the upper level of the brine is automatically kept above the grating, and the final outlet temperature of the brine is very uniform.

B. M. Ve n a b l e s.

Pasteurisation of liquids containing gases. A,/S.

de Forenede Bry g g er ie r (Austr. P , 105,348, 27.6.25).—

Liquids charged with gases are pasteurised by heating them to the desired temperature in vessels with expans­

ible walls ; after cooling, the walls of the vessels are forced baok to their original position by external pres­

sure. Suitable vessels may be made of aluminium, the bottom being of soft aluminium and the remainder of the vessel of hard aluminium. A. R. Po w ell.

Method and device for conditioning gases as regards their temperature and humidity. Ca r r ie r En g in eer in g Co., Ltd., and S, L. Groom (E .P . 276,214, 24.12-26).—The gas is preheated, then humidified by sprays, and the excess liquid from the sprays is recircu­

lated. The conditioned gas passes over a thermostat which regulatos the amount of preheating.

B. M. Ve n a b les.

Apparatus for heating air and/or other gasea.

F . A. Fahrenw ald and H. E. Smith (E.P. 275,706, 6.5.26).—A continuously operating stove, e.g., for heat­

ing the air for blast furnaces, is constructed with the air passing through metallic pipes which in the hotter zones may be of chromium alloys. Provision is made for ex­

pansion and contraction and for the use of the external casing of existing stoves. B. M. Ven a bles.

Deodorising, cooling, and dehydrating fluids and apparatus therefor, H. L. Murray, Assr. to

Te Aroha Da iry Co., Lt d. (U.S.P. 1,641,349, 6.9.27.

Appl., 7.3.24. C onv., 14.8.23).—See E.P. 220,627 ; B„

1926, 74.

[Heat-insulated iron walls for] annular ovens or furnaces with rotary hearths. Trocknungs-, Ver sc h- w elungs- u . Vergasungs-G.m.b.H ., L. Honigmann, and F. Ba r tlin g (E.P. 275,041, 2.10.26).

[Blocks for] furnaces having suspended arches.

L. Mop.ton and J. Hargrove (E.P. 275,008, 7.7.26).

[Automatic, reversible] absorption refrigerating apparatus. J. O. Boving (E.P. 276,088, 21.5.26). _

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B r itis h C h e m ic a l A b s tr a c ts — B .

8 0 2 Cl. I I . — Fu e l; Ga s; De s t r u c t i v e Di s t i l l a t i o n; Mi n e r a l Oi l s.

Absorption refrigerating or heating machine.

SlEMENS-ScnUCKERTWERKE G.M.B.H. (E.P. 251,251, 31.3.26. Conv., 23.4.25).

Absorption refrigerating machines. Sulzicr

F e rre s Soc. An o n. (E.P. 272,865,3.5.27. Conv., 15.6.26).

II.— FU EL

;

G AS; DESTRUCTIVE DISTILLATION;

MINERAL OILS.

Combustion tray for determination of heating value of coal. G. B. Watk ins and J. V. I Iu nn (Ind.

Eng. Cliem., 1927, 19, 1020).—Incomplete combustion, due to loss of sample from the combustion tray, in determinations of the calorific value of coal is avoided by the use of an illium combustion tray \ in. deep, diam. at base f in. and at top 1 in., with holes drilled round the side and half-way up. The coal sample is heaped into a cone in the tray and combustion con­

ducted in the normal way. Oxygen is drawn in through the holes as combustion proceeds. R. Brightm a n.

Propagation of a zone of combustion in powdered coal. III. Composition of the oxidation product.

S. H. Je n k in s and F. S. Sin n a tt (Fuel, 1927, 6, 421—

424 ; cf. B ., 1924, 896).—The loss in weight due to the passage of a zone of combustion through a conical heap of powdered coal varied in different experiments from 5-2 to 12-7% for one coal and from 9-1 to 21-2% for another. In spite of this variation the composition of the oxidation product from the same coal was almost constant. The most marked changes in composition on combustion were the increase in the oxygen content (e.g., from 7-29 to 16-72%, or from 9-51 to 18-31%) and the complete loss of caking power.

A. B. Ma n n in g.

Total carbon in coal determined by analysis of gas from bomb calorimeter. G. B. Wa tk in s (Ind.

Eng. Chern., 1927, 19,1052—1054).—A sample of coal is exploded in a Mahler bomb under an oxygen pressure of 20 atm., and the calorific value determined. The gaseous products of combustion are then expanded into a mercury-sealed gasometer and the carbon dioxide content is determined. The gasometer of 9 litres capacity was constructed of two concentric steel tubes so as to use a minimum quantity of mercury. I t was calibrated to read at 100 c.c. intervals. Tests on standard coal samples, benzoic acid, and sucrose show values for total carbon accurate to 0-1%. C. Ir w in.

Nitrogen as a catalyst in the determination of sulphur in coal by the bomb-washing method.

J. F. Ivohout (Ind. Eng. Chem., 1927,19, 1065—1066).—

I t is shown that increasing the nitrogen content in the gases in a bomb calorimeter from the usual 5% to 10—15% generally caused a slight increase in the apparent sulphur content of the coal tested, as deter­

mined by washing out the bomb and weighing as barium sulphate. This is attributed to the increased catalytic action of oxides of nitrogen in completing oxidation to sulphuric acid, and brings the results more in harmony with the Eschka or sodium peroxide methods.

C. Ir w in.

Resins in coal and their effect upon its properties.

C. Cockram and R. V. Wh e e l e r (Fuel, 1927, 6, 425—

428).—The small yellow rods, varying in length up" to 0-02 in., which appear in the residue from the regulated oxidation of certain coals, e.g., Hamstead vitrain, after removal of the regenerated ulmins by dissolving in dilute sodium hydroxide, are shown by their solubility^in chloroform and their composition to be resin inclusions.

Photomicrographs show that the resin rods exist in the coal in the positions which they had occupied in the woody tissue from which the vitrain was formed. The resin is extracted from the coal by treatment with pyridine and chloroform, and therefore appears in the y-compounds; the yields of y-compounds from a

“ normal ” and a “ resinous sample of Parkgate clarain were 4-9 and 7-2%, respectively. In an assay test at 600° the tar yield from the resinous clarain (16-6%) was much higher than that from the normal clarain (12-1%). Although the coke from the former was highly swollen, the degree of swelling was less than that in an average clarain from the same seam.

A. B. Ma n n in g.

Inherent ash of coal. R. A. Mott and R. V.

Wh e e l e r (Fuel, 1927, 6, 416—420).—The amount and composition of the “ inherent ” and the “ adven titious” ash of a number of samples of clarain and durain from the Parkgate seam, of durain from the Nottingham­

shire Top Hard seam, and two samples of vitrain, have been determined. The coal substance containing the inherent ash was separated from the adventitious ash by suspension of the very finely-ground material in water and flocculation of the coal by the addition of paraffin oil. Comparison of the Si02/Al203 ratios shows a definite difference in composition between the inherent and adventitious mineral matter in the samples. The differences are somewhat greater for the durains than for the clarains, and are, moreover, in the opposite direction. Comparison with analyses of the ash of modern non-flowering plants indicates that these are poorer in silica than their earlier prototypes. The iron present in clarains is probably chiefly adventitious.

The presence of nickel and zinc in the clarain and durain of one seam section has been established. No close relationship could be established between the composition of the adventitious ash in the coal and that of the shale occurring as a dirt band in the seam or composing the floor of the bed. A. B. Ma n n in g.

Determination of the porosity of coke. N. A.

Ross (Gas World, 1927, 87, Coking Sect., 97—98).—

In determining the volume of a piece of coke by immer­

sion in water considerable errors (up to 6%) may be caused by the coke taking up water. More consistent and accurate results are obtained by using mercury (cf. Greenwood and Cobb, J.S.C.I., 1922, 41,181 t). The real sp. gr. must be determined on material so finely ground that no closed pores remain in i t ; on the other hand the degree of subdivision used when determining the sp. gr. of the material plus closed pores must not be such as to affect appreciably the coke structure.

A. B. Ma n n in g.

Lustre carbon as initial mem ber of the black, crystalline carbon series. K. A. Hofm ann and U.

Hofmann (Ber., 1926, 59, 2433—2444 ; cf. Hofmann and Rochling, B., 1923, 1130 a).—Highly lustrous carbon is

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B r itis h C h em ica l A b s tr a c ts — B .

C l. I I . — Fu e l ; Ga s ; De s t r u c t i v e Di s t i l l a t i o n ; Mi n e r a l Oi l s. 803

most certainly prepared by passing the vapours of light petroleum, initial b.p. 90°, mixed with nitrogen, oxygen, water vapour, carbon monoxide, or carbon dioxide into a crucible heated electrically at 750—800°. Decom­

position occurs thermally at the porcelain surface, and formation of soot in the gas is avoided. A uniform, highly lustrous, completely non-transparent, black layer is formed on smooth surfaces of porcelain, quartz, fluorspar, silicon carbide, diamond, zinc blende, gold, or silver, whereas a grey layer is produced on rough surfaces of unglazed porcelain, calcined magnesia or asbestos, electrode retort carbon, or Acheson graphite ; the grey material is also formed on smooth surfaces above 860°. Prolonged exposure of diamond to hydro­

carbon vapours at 700° and 500 atm. does not lead to growth of the crystal. Lustre carbon has d1G 1 •86^ 0-02, the density increasing with increasing temperature of formation. After prolonged heating at 850° in an atmos­

phere of dry hydrogen it appears to be pure carbon. I t is not capable of absorbing phenol, thus resembling graphitic carbon. Towards oxygen, water vapour, carbon dioxide, sodium sulphate, and potassium cyanate lustre carbon is much more stable than sugar carbon prepared at the same temperature, and resembles closely retort graphite. Both varieties are more active than is natural graphite. Röntgen spectrographic observations show that graphite, retort graphite, lustre carbon, and sugar charcoal are all crystalline in structure, and that the size of the crystallites diminishes in the given order.

H . Wr en.

Composition of benzol from carburetted water- gas. W. A. Voss (J.S.C.I., 1927, 46, 373—375 t).—

Benzol extracted from carburetted water-gas by means of active charcoal is compared with the benzol similarly extracted from coal-gas produced in horizontal retorts.

The benzol from carburetted water-gas contained only 0-73% of paraffins, but contained 12% of unsaturated hydrocarbons, which rendered the purification of the spirit difficult. The benzol from coal-gas contained 2-57% of paraffins, but only 5% of unsaturated hydro­

carbons. Rectified benzol from carburetted water-gas is richer in toluene than the benzol from coal-gas. The sample examined contained 32-4% of toluene compared with 17-97% in the water-gas sample. The difficulty in removing the unsaturated compounds from carburetted water-gas benzol is shown graphically, the loss in volume being plotted against the degree of acid washing. With adequate washing a satisfactory benzol can be obtained from carburetted water-gas.

Determination of carbon monoxide, hydrogen, and methane in air containing ethylene, applicable to the analysis of the products of explosion of blasting explosives. J. Thorburn (J.S.C.I., 1927, 46,

355— 358 t).— One litre of the gas to be analysed is automatically displaced by mercury from a pipette and passed through the purification and reaction systems.

Carbon dioxide is removed by caustic potash and ethylene by 20— 25 % oleum. Sulphur trioxide from the oleum is absorbed in caustic potash, and moisture is removed by calcium chloride followed by phosphorus pentoxide.

Carbon monoxide is then oxidised by iodine pentoxide in a U-tube heated at 150° in an oil bath, and the per­

centage determined from the quantities of iodine and

carbon dioxide formed, the iodine being absorbed in a 15% potassium iodide solution and the carbon dioxide in iV/9-barium hydroxide solution. The gas is dried again and the hydrogen is oxidised, by the oxygen present in the sample, over palladium asbestos heated in an electric tube furnace with thermostatic control at 255 ± 5°; the water formed is caught in a weighed tube of special design containing phosphorus pentoxide, and from this the percentage of hydrogen is calculated.

The gas is next passed through N/9-barium hydroxide solution to determine any accidental oxidation of methane at this stage, and after being dried again it is passed over copper oxide heated in a quartz tube to a red heat in a small gas furnace to burn the methane, the percentage of which is calculated both from the amount of water and that of carbon dioxide formed, these substances being absorbed as already indicated. As detailed, the method is applicable to mixtures containing 0—4% of each of the components to be determined, and 01% of ethyl­

ene. It is used when large samples of gas are available if special accuracy is required.

Ignition of gases by hot wires. W . C. F . Shep­

h e r d and R . V . W h e e le r (Safety in Mines R es. Bd., Paper N o. 36, 1927, 26 pp.).—A wide range of m ixtures of m ethane and air can be ignited b y the glowing (tung­

sten) filam ent of a m iners’ electric lamp bulb, w hen the latter is broken in such a w ay as to leave the filament in tact. D eterm inations have been made of th e minimum current which, when caused suddenly to flow through a platinum or tun gsten wire, eventually causes ignition of m ethane-air m ixtures, and of th e tim e interval between com pleting th e circuit and ignition. For a platinum wire of given diameter the m inim um igniting current is constant over the range of ignitable m ixtures, varying from 1-65 amp. for a wire of 0-1 mm. diam. (ignitable range 4-55 to 7-50% of m ethane) to 6-6 amp. for a wire 0-3 mm. diam. (ignitable range 4-30—15-2% of m ethane). Platinum wires less than about 0-1 mm. in diameter fuse before causing ignition of any m ixture.

Some surface com bustion occurs w ith platinum wires in all m ethane-air m ixtures. Other conditions remaining constant, the tim e interval before ignition passes through a m axim um value as th e com position of th e m ixture is varied, th e corresponding com position coinciding with that of th e m ixture of m axim um calorific value (9-45%

of m ethane). The higher tem perature of th e wire due to the greater h eat developed b y surface com bustion in such a m ixture causes an increased convection effect with a resulting m inim um tim e of contact of the gas w ith th e wire. W hen a tungsten wire is heated in an atmosphere containing oxygen it is oxidised, and its tem perature rises until it bum s with a small bright flame, which alw ays ignites an inflammable m ethan e- air m ixture ; th e m ost readily ignitable m ixture con­

tains about 8% of m ethane. I t is therefore recommended th at an autom atic device, which breaks th e electric circuit as soon as th e outer protecting glass is broken, should be incorporated in th e design of a miner’s electric

hand-lamp. A. B . Ma n n in g.

Role of lead sulphide in the sweetening of petroleum distillates and chemistry of the mer- captans. J. C. Mo rrell and W . F . Faragher (Ind.

Eng. Chem., 1927, 19, 1045—1049).—Solutions of pure

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B r itis h C h em ica l A b s t r a c t s —B.

804 C l. H .Fu e l ; G a s ; D e s t r u c t i v e D i s t i l l a t i o n ; M i n e r a l O i l s .

ethyl, n-butyl, tsoamyl, heptyl, and benzyl mercaptans in refined, sulphur-free Pennsylvania naphtha were treated with solutions of sodium hydroxide in various mixtures with lead sulphide and sulphur in a stream of nitrogen or oxygen. Panhandle gasoline (Amarillo, Texas) containing 0-05% of mercaptans and washed free from hydrogen sulphide was similarly treated. With oxygen alone no sweetening occurred, and the mercaptans are not oxidised under the conditions of the test. Agitation with sodium hydroxide and sulphur in a current of nitrogen sweetened the mercaptan solutions, but not the Panhandle gasoline. Sodium mercaptides are formed first and then the disulphide (cf. Holmberg, A., 1908, i, 308) : in the case of i’soamyl mercaptan the use of a current of oxygen in place of nitrogen considerably reduced the time required for sweetening. Lead sulphide suspended in water or in the oil did not effect any sweeten­

ing, and hence lead sulphide does not catalyse the oxidation of mercaptans (cf. Wendt and Diggs, B., 1924, 1002). Mixtures of lead sulphide and sodium hydroxide agitated in a current of oxygen effected sweetening in all cases except those of woamyl mercaptan and the gasoline, lead mercaptides being formed in every case. Sweetening also occurred in a current of nitrogen containing 4% of oxygen, sulphate ions being formed in all cases. Lead sulphide plays a minor part in the stability of lead mercaptide dispersions, functioning similarly to fuller’s earth and charcoal, but being less active. Agitation with a solution of sodium plumbite in either nitrogen or oxygen effected sweetening exactly as in the case of a mixture of lead sulphide and sodium hydroxide, slightly better results being obtained with a current of oxygen. There action, 2(RS)2Pb + 02 ->

2RS-SR + 2PbO, takes place whether the sodium plumbite or the lead sulphide and sodium hydroxide are used. Panhandle gasoline cannot be sweetened unless lead sulphide and oxygen as well as sodium plumbite are present. The nature of the lead sulphide is also a factor. Thus, no sweetening action was observed with galena, and lead sulphide precipitated from lead acetate solution with hydrogen sulphide was less effective than that obtained by passing the gas over lead dioxide, the sweetening activity depending mainly on the rate of oxidation of the sulphide, and the rate of sweetening on the oxygen concentration, being greatest in ozonised air.

No sweetening action occurs in pure nitrogen. In the oxidation of lead sulphide in sodium hydroxide suspen­

sion with oxygen, one mol. of sodium sulphate is formed per mol. of sodium plumbite. Mercury, silver, copper, and nickel sulphides exert a similar sweetening action on benzyl mercaptan, and nickel sulphide in the case of butyl mercaptan also, sulphate being formed in all cases.

Addition of sulphur to the mixture of butyl mercaptan and suspended sulphides in sodium hydroxide produced sweetening in every case, sulphate ion being again formed together with the mercaptide of the metal and subse­

quently the disulphide. R. Brig h t m a n.

Decomposition of waxes. Ma il h e.—See XII.

Pa t e n t s.

Coke oven. C. St il l (E.P. 275,914, 12.5.27).—A combination of the arrangement for the uniform heating of coke ovens described in E.P. 221,697 (B., 1924, 900

with means for withdrawing the gaseous distillation products at or near the bottom of the coking chamber avoids undue cracking of the gaseous products, and at the same time gives a good quality coke. If the ch amber is unevenly heated and the gaseous products are with­

drawn from the bottom, cracking still occurs due to the rapid overheating of the lower part of the charge. In the process now described it is preferable so to dis­

tribute the heating that the temperature of the upper part of the wall is slightly higher than that of the lower

part. A. B. Ma n n in g.

Carbonisation at low temperature of hydro- carbonaceous material. C. Ab-De r-Halden (E.P.

263,197, 20.12.26. Conv., 21.12.25).—A retort for the low-temperature carbonisation of fuels consists of two (or if necessary more) pans fixed to a vertical axis which can be rotated. The material is carbonised in the lower pan, which rotates in an enclosure heated externally by the gases from a fire grate, and is so designed that the combustion gases cannot penetrate into the enclosure.

The hot flue gases then pass through the enclosure in which the upper pan rotates, and in which the material undergoes a preliminary drying. By means of inclined scrapers the material is made to pass along a spiral path from the periphery to the centre of the upper pan, whence it descends through a passage to the lower pan, which it traverses similarly in the reverse direction until discharged through a passage at the periphery. The inclination of the scrapers controlling the circulation of the material can be adjusted from outside the retort.

A. B. Ma n n in g.

Carbonising, distilling, and gasifying solid fuel.

6. W . Wallace (U.S.P. 1,639,390—1 and 1,639,417, 16.8.27. Appl, [a] 18.5.25, [b] 13.1.26, [c] 24.5.26).—

(a) The fuel passes along a horizontal conduit and is met by a stream of hot gases issuing from a jet, whereby sudden local heating is effected. The heating means are adapted to the maintenance of a substantially stationary carbonising zone in the reaction chamber, (b) The fuel is treated in substantially the same manner as in (a),

but a flame of burning gases issues from the jet in place of hot gases, and the material heated thereby is gasified by means of a draught current, (c) Coke and by­

products are produced by a process similar to that described in (b). C. 0. Harv ey.

Distillation and coking of carbonaceous m atter.

L. I Ionigmann and F. Ba r tlin g (U.S.P. 1,640,502, 30.8.27. Appl., 7.1.27. Conv. 26.11.25).—Solid carbon­

aceous material is distilled and coked on annular revolving hearths in a layer less than 1 cm. thick.

C. O. Harv ey.

Production of am m onium nitrate and nitrite etc.

and generation of additional power from the combustion gases in internal-combustion engines.

E. R. Be s e m fe l d e r (G.P. 440,622, 16.4.25).—The combustion chamber is provided with contact material to promote formation of oxides of nitrogen, and the exhaust gases are cooled by the evaporation of a liquid in a closed exhaust system provided with a release valve in connexion with a turbine operated by the escaping gases. The nitrous and nitric acids formed in the process are neutralised with ammonia. L. A. Co les.

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B r itis h C h em ica l A b s tr a c ts —B .

Cl. II .— Fu e l ; Ga s ; De s t k u c t t t e Di s t i l l a t i o n ; Mi k b b a l Oils. 806

Manufacture of active carbon. I. G. Fa r b en in d.

A.-G., Assees. of Fa r b en fa br. vorm. F . Bayer & Co.

(E.P. 251,636, 28.4.26. Conv., 29.4.25).—Cellulose carbonaceous material (wood, peat, lignite, etc.) is treated with sulphuric acid and heated in a furnace at about 750°, the carbon produced being further heated at about 900° while steam is passed through the furnace.

W . G. Ca r e y.

Manufacture of activated carbon. G. W . Wallace

(U.S.P. 1,639,356, 16.8.27. Appl., 13.1.26).—A moving pervious column of material is carbonised by hot flame gases impinging on and moving in counter-current to the material, whereby a stationary zone of carbonisation is maintained. The hot carbonised material is partially oxidised by another draught current. C. 0. Harv ey.

Carbonaceous m aterial and process for making sam e. Roessler & Hasslacher Chem. Co. (E .P.

251,982. 30.4.26. Conv., 9.5.25).— A dense carbon of low porosity and suitable for electrodes etc. is made by m ixing finely-divided graphite w ith a binder and carbonising under pressure. Thus a m ixture of 80%

of graphite and 20% of hard p itch was pressed at 250°

in a steel m ould which was th en heated a t th e tem perature of decom position of the pitch. The carbon was removed from th e m ould and heated a t 1000° ; th e resulting product has an apparent sp. gr. of 1-8 — 1 '9 .

A. C. Monkhouse.

Production of highly-active blood charcoal.

Ch em. Fa b r. a u f Actien (vorm. E. Schering) (G.P.

440,769, 14.8.25).—Blood or blood serum mixed with ammonium sulphate is carbonised in the presence of an excess of alkali carbonate. L. A. Co les.

Process and apparatus for the manufacture of gas from heavy oils. C. Chilovsky (E.P. 255,423, 19.5.26. Conv., 16.7.25).—A process for the continuous complete conversion of oils into combustible gases, in which no fouling of the catalyst occurs, consists in passing the oil (with or without admixture with steam, metallic chlorides in the case of animal and vegetable oils, coal in colloidal suspension, etc.) through a vaporiser, mixing the vapours with heated air (or oxygen) in proportions of about 2 and not more than 3 g. of oil to 5 litres of air, and allowing partial combustion to take place in a heat-insulated cylindrical chamber whereby the mixture attains a temperature of 700—1000°

prior to passing through a catalyst (steel rivets, molten cast iron, etc.). The hot gases produced may be used for preheating the oil and air, and the process may be carried out under partial vacuum. C. 0. Harv ey.

Manufacture of gas from heavy o ils. C. Chilovsky

(E.P. 271,899, 19.5.26. Conv., 16.7.26. Addn. to E.P.

183,828; B., 1924, 46).—The process of the main patent is improved by passing the atomised and gasified heavy oil over a metallic or non-metallic catalyst at 700—900°. The whole of the heat required for the process may be generated in the combustion chamber, or the latter may be maintained at a lower temperature (400—600°) and the heat then required for maintaining the temperature of the catalyst at 700—900° may be produced by the subsequent introduction of additional air and combustion of a further portion of the oil. Steam may be added to the mixture to prevent clogging of the

catalyst. Metallic chlorides are added to vegetable and animal oils, and also, if desired, to mineral oils, before subjecting them to the process. A. B. Man n in g.

Desulphurisaiion of fuel gases. E. Wil l (Austr.P.

105,362, 28.6.23. Conv., 15.5.23).—The gases are passed through strongly heated chambers, fitted completely or partly with chequer work of basic material, between which and the acidic material of the chamber walls there is a layer of magnesite or magnesite brick.

A. B. Ma n n in g.

Gas scrubber. A. C. D . Duchem in (E.P. 263,794, 20.12.26. Conv., 31.12.25).—A horizontal gas scrubber is divided by partitions, slightly inclined in the direction of the gas flow, into a series of chambers containing filling material, and has empty expanding spaces between successive chambers for equalising the gas flow. The scrubbing liquid is pumped from the bottom of each chamber to a spraying device at the top, and at the same time, by the aid of weirs of different heights, is circulated through the lower part of the apparatus in a direction opposite to that of the gas flow.

A. B. Ma n n in g.

Regeneration of contact m asses for the catalytic hydrogenation of carbon oxides. G. Patart (E.P.

252,361, 12.5.26. Conv., 25.5.25. Cf. F .P . 599,588;

B., 1926, 351).—The contact masses containing zinc chromate or tungstate etc. used as catalysts in the synthesis of methyl alcohol, and which have lost activity owing to the accumulation thereon of sulphur compounds, can be regenerated by calcination in an oxidising atmosphere, as, for example, by heating to redness in an open crucible. A. B. Ma n n in g.

Increasing the safety of porous and absorbent materials used for storing explosive combustion gases [e.g., acetylene]. R. He p p n e r (E.P. 264,846, 20.1.27. Conv., 20.1.26. Cf. G.P. 420,150; B., 1926, 230).—Absorbent material used for storing acetylene etc.

is treated with inorganic or organic salts which volatilise at high temperatures, consuming heat and so preventing further decomposition of the gas, or which decompose into gases exerting a fire-choking action. Pumice stone meal, metal oxides, etc. mixed with adhesives such as oils, fats, or resins insoluble in the gas solvent, and incapable of reacting with the gas, are added to the absorbent material to improve its homogeneity.

W . G. Ca r ey.

Production of liquid hydrocarbons and derivatives thereof from coal, tar, etc. I. G. Fa r b e n in d. A.-G.

(E.P. 249,155, 13.3.26. Conv., 14.3.25. Addn. to E.P. 247,217 ; B., 1927, 601).—In the process of con­

verting coal, tar, etc. into liquid hydrocarbons by treatment with reducing gases under pressure and at high temperatures, with or without a catalyst, the hot surfaces of the apparatus which come into contact with the high-pressure gases are made of a metal which does not react with carbon monoxide. Suitable metals are copper, silver, aluminium, chromium, manganese, etc., and special steels containing 1020% of manganese, chromium, tungsten, etc. A. B. Ma n n in g.

Process and apparatus for the cracking of oils.

S. Se e l ig (E.P. 268,323, 11.3.27. Conv., 25.3.26).—

In a process for cracking oils by passage through molten

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B r itis h C h em ica l A b s tr a c ts —B .

806 C l. I I .— Fu e l ; Ga s ; De s t r u c t i v e Di s t i l l a t i o n ; Mi n e r a l Oi l s.

metal, the interior of the vertical cylindrical chamber in which the operation is conducted is protected from fluctuations of temperature by the introduction of a helical tube which may be evacuated or may contain air or steam, and which serves as a heat- insulating medium. The gases passing through the tube may be led into the vapour space above the molten metal, thereby assisting in the removal of the cracking

products. C. 0. Ha r v ey.

Process and apparatus for splitting fluid hydro­

carbons. C. Longhi(E.P. 275,281,1.3.26).—The method of cracking oils by means of an electric arc immersed in the oil (cf. E.P. 248,830; B., 1926, 525) is modified by providing a rotating central electrode, carrying a number of arcing points and a corresponding number of arcing points attached to the body of the apparatus, whereby the arcs are rapidly made, elongated, quenched, and re­

made. When the speed of rotation is great enough, the arcs become in effect a rotating disc, and in such circum­

stances it is advisable to have both electrodes rotatable.

C. 0. Harvey. Treatment of cracking or sludge residues. N. V.

de Bataafsche Petroleum Ma a t s c h a p p ij, and E. R.

Moser (E .P . 270,274, 13.4.27. Conv., 27.4.26).—The residues are treated with small quantities of substances having an acid reaction [e.g., ferrous chloride, aluminium chloride or sulphate, sulphur chloride, organic acid chlorides, etc.) with or without the addition of a little water, and are then heated at temperatures of 100200°, whereby asphaltic and coke-like substances are rendered easily removable by filtration, centrifuging, etc. Viscous residues are diluted with crude oil, fuel oil, or gas oil before treatment. C. 0. Ha r v e y.

Process and apparatus for cracking oil. 6.

Eg l o ff, Assr. to Un iv e r sa l Oil Products Co. (U.S.P.

1,638,115, 9.8.27. Appl., 13.12.20. Renewed 24.3.27).

—The oil to be cracked is passed in a thin stream under pressure through a heating chamber and thence in a substantially liquid state to an expansion chamber, the upper part of which is heated internally, and which carries a reflux condenser whereby less volatile products are returned for retreatment, the vapours being condensed and collected under pressure. C. 0. Ha r v ey.

Method and apparatus for cracking oil. E. M.

He s s (U.S.P. 1,638,335, 9.8.27. Appl., 24.1.23).—The oil flows in a thin stream over inclined heating plates situated in a pressure still, the residual uncracked oil passing to a producer wherein it is converted into a gas rich in hydrogen which is discharged into the still and mixed with the vapours of distillation.

C. 0 . Ha r v e y.

Process for cracking oil. 6. Eg l o ff, Assr. to

Un iv e r sa l Oi l Products Co. (U.S.P. 1,638,093, 9.8.27.

Appl., 20.12.20. Renewed 3.1.27).—The oil passes through a cracking coil to an expansion chamber, the latter being connected with a larger expansion chamber for receiving evolved vapours prior to dephlegmation and condensation. The operation is carried out under

pressure. C. 0. Ha r v e y.

Apparatus for distilling oil. J. W. Coast, jun., Assr. to Doherty Research Co. (U.S.P. 1,639,327, 16.8.27. Appl., 3.11.20).—The interior heated surface

of a horizontal cylindrical still is kept clean by means of a scraping member carried on an endless chain.

C.' 0 . Ha r v ey.

Apparatus for the distillation of oil. E. T. Ma n ley,

Assr. to Te x a s Co. (U.S.P. 1,640,202, 23.8.27. Appl., 26.10.18. Cf. U.S.P. 1,428,338—9 ; B ., 1922, 850 a).—

A horizontal still is provided with a vapour space situated above the level of the oil, external heat being applied around practically the entire periphery of both liquid and vapour spaces, and the latter being lagged in order to avoid overheating of the vapours, while maintaining a uniform cracking temperature. C. 0 . Harv ey.

Art of distilling oils. F. A. Howard and N. E.

Loomis, Assrs. to Standard Develo pm en t Co. (U .S .P .

1,640,938, 30.8.27. Appl., 10.4.22).—The oil passes continuously through the following steps in succession : volatile constituents are removed by heating at ordinary pressure; the residual oil is cracked under pressure and the vapours are removed after reduction of pressure ; the residue is mixed with fresh incoming oil.

0 . 0 . Harv ey.

Continuous treatment of hydrocarbons [with liquid sulphur dioxide]. O. Y. Im ray. From All­ gem. Ge s. p u r Ch e m. Ind. m.b.H. (E.P. 275,884, 2.3.27).—

The process is a modification of that of E.P. 114,845

(B., 1920, 98 a). The oil ascends through a mixer, passing counter-current to the liquid sulphur dioxide, and the resulting extract and raffinate are subjected to a continuous evaporation process divided into a number of pressure stages. In the first stage the sulphur dioxide is removed principally by the action of heat, in the next successive stages by the combined action of heat and reduced pressure, and in the last stage prefer­

ably only by the application of a comparatively high vacuum, so that the gases evolved in the first stage flow into the condenser tank by their own pressure, whilst the gases evolved in the subsequent stages are brought up to the pressure of the tank by compressors. The gases passing from the evaporators are freed before compression from any light hydrocarbons by suitable

cooling. A. B . Man n in g.

Refining hydrocarbon oils. P . McMic h a e l, Assr.

to Hydrocarbon Re f in is h in g ProcessCo., In c. (U .S .P .

1,641,546, 6.9.27. Appl., 25.5.25).—Cracked hydro­

carbon oils are treated with sulphur dioxide and then with an absorbent material. C. O. Harv ey.

Purification of petroleum products. S. J. Dickey

and R . C. Wh e e l e r, Assrs. to Ge n. Petroleum Co r p. of Ca lifo r n ia (U .S .P . 1,639,988, 23.8.27. Appl., 19.4.24).

—The sludge is removed from an acid-treated distillate by filtration through a pack of dried sand, the sand being subsequently cleaned in situ by means of steam and dried by a current of air. C. O. Ha r v ey.

Apparatus for purifying used mineral lubricating oil. R . E. Langston, Assr. to Wayne Co. (U.S.P.

1,640,415, 30.8.27. Appl., 27.9.21).—The oil is purified and freed from volatile matter by being heated to a temperature substantially above 100° in a jacketed vessel heated by means of steam coils, which extend from the jacket into the vessel and open thereinto.

C. 0 . Ha r v e y.

Cytaty

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