Nitro-Explosives: A Practical Treatise

elatine Compounds-Ton

ysis of Explosives-Nitr

alinity-Ash and Inorgan

ion and Pellet's, Schult

c Acid and Picrates-Res

drochloric Acid and O

eneral Impurities and

f the Alkaloids-Analysi

-Total Acid Equivalen

Acids-Impurities-Olei

cerine-Waste Acids-S

on-Table for Correction

ure and

s very simple, and may be conducted as follows:-Weigh out about 10 grms. of the substance, and place over calcium chloride in a desiccator for some six to ei

ns of an ordinary aspirator. The air should pass approximately at the rate of 10 c.c. per second. The tube by which the dry air enters the bottle extends to within 1 inch of the crucible containing the dynamite. An empty safety bottle is connected with the inlet, and another with the outlet of the wide-mouthed bottle. The first guards against the mechanical carrying over by the air current of sulphuric aci

eighed filter, drying at 100° C., and weighing. This gives the weight of the kieselguhr. The nitro-glycerine must be obtained by difference, as it is quite useless to evaporate down the ethereal solution to obtain it, as it is itself volatile to a very considerable extent at the temperature of evaporation of the ether, and the result, therefore, will alway

er paper. If it is nitro-glycerine it will make a greasy spot. If the paper is now placed upon an iron anvil, and struck with an iron hammer, it will explode with a sha

ith distilled water, to see that it produces no turbidity), and filtered, on the addition of distilled water, the s

.84) be added, a deep purple colour will be produced. This colour changes to green upon the addition of water. If it is necessary to determine the nitro-glyce

pulp and saltpetre (KNO_{3}) mixed with a thin blasting gelatine. The method of analysis is as follows:-Weigh out 10 grms. of the substance, previously cut up into small pieces with a platinum spatula, and place over calcium chloride in a desiccator for some days. Reweigh. The loss equals moisture. This is generally very small. Or Handy's method may be used. The dried sample is then transferred to a small thistle-headed funnel which has been cut off from its stem, and the open

l (2 ether to 1 alcohol), and allow to stand overnight. Sometimes a further addition of ether-alcohol is necessary. It is always better to add another 300 c.c., and leave for twenty minutes or so a

e precipitated cotton should then be redissolved in ether-alcohol, and again precipitated with chloroform (20 c.c. of ether-alcohol should be used). This precaution is absolutely necessary, if the substance has been treated with ether- alcohol at first instead of ether only, otherwise the results will be much too high, owing to the gelatinous precipitate retaining very considerable quantities of nitro-glycerin

e Soxhlet, the nitro-glycerine will of course be dissolved out first,

ter, and the water decanted some eight or ten times, and the residue finally transferred to a tarred filter and washed for some time with hot water. The residue left upon the filter is wood-pulp. This is dried at 100° C. until constant, and weighed. The solution and washings from the wood are evaporated down in a platinum dish, and dried at 100° C.

O_{3} = 2NaNO_{3}

t. = 1

64) and x =

ue, and d equals the difference in weight of resi

down upon the water bath at 30° to 40° C., and finally dried over CaCl_{2} until no smell of ether or chloroform can be detected, and the nitr

(collodion) 3

ycerine

ulp 16

3} 12

}CO_{

r 0.

t of course be considerably modified. Paraffin, resin, and most of the sulphur will be found in the ether solution if present. The solution should be evaporated (and in this case the explosive should in the first case be treated with ether only, and not ether-alcohol), and the residue weighed, and then treated on the water bath with a solution of caustic so

100 c.c. silver crucible on the water bath with an alcoholic solution of sodium hydroxide, and where the nitro-glycerine is decomposed, the liquid is evaporated to dryness. The residue is fused with 40 grms. of KOH and 5 grms. of potassium nitrate, the mass dissolved in dilute acetic acid and filtered, and the sulphates precipitated in the usual way. If camphor is present, it can be extracted with bisulphide of carbon after the material has been treated with ether-alcohol. In that case the sulphur, paraffin, and re

CaCl_{2} until the CS_{2} has evaporated from them. The camphor evaporates, and leaves the small quantity of nitro-glycerine which had been dissolved with it. The other portion is the nitro-glycerine, now free from CS_{2}. The two are weighed and their weights added together, and equals the nitro- glycerine present. There is a loss of nitro-glycerine, it being partly evaporated along with the CS_{2}. Captain Hess has s

ly, and the residue warmed gently on the water bath with 5 c.c. of ammonium sulphide solution, and 10 c.c. of alcohol until the nitro-glycerine is decomposed, after which about 250 c.c. of water and sufficient hydrochloric acid to render the liquid strongly acid, are added, and the liquid filtered. The precipitate is washed free from acid, and then washed through the filter with strong alcohol and chloroform into a weighed platinum dish, which is dried to constant weight at 50° C. The contents of the dish are now transferred to a silver crucible, and the sulphur determined. This amount of sulphur, deducted from the weight of the contents of the platinum dish, gives the quantity of substances soluble in chloroform with the exception of the nitro-glycerine, moisture, and sulphur. The amount of the former substances plus the moisture and sulphur, deducted from the total loss on extraction with chloroform

the Analysis of Explosi

1, 23 [8]

atinum dish. Dry and weigh. This equals the Ba(NO_{3})_{2}. If the sample is tonite No. 3, and contains di-nitro-benzol, treat first with ether to dissolve out this substance. Filter into a dish, and evaporate off the ether, and weigh the di-nitro-benzol, and afterwards treat residue with water as before. The residue is dried and weighed, and equals the gun-cotton present. It should then be treated with a solution

shed with a little ether, pressed, and dried at 40° C., and weighed. It equals the gun-cotton. The solution contains the nitro-glycerine, soluble cotton, and vaseline. The cotton is precipitated with chloroform, filtered off, dried, and weighed. The two ether-alcohol solutions are mixed, and carefully evaporated down in a platinum dish upon the water bath at a low temperature. The residue is afterwards treated with strong 80 per cent. acetic acid, which dissolves out any

ried out as follows:-The cordite or other explosive is prepared in the manner laid down for the Abel heat test, that is t say, it is ground in a small mil

-MARSHALL'S APPARATUS F

curately weighed, and is then placed upon a metal plate heated by steam from a water bath. It is left upon the bath until all the moisture has been driven off, then it is allowed to cool for about half-an-hour in a desiccator and is weighed. The loss in weight gives accurately the m

ground finer than stated, else some of the moisture will be lost in the grinding and sieving operations, and the result will be too low. In order to be able to drive off all the moisture in the times mentioned, it is essential that the glass cone shall not fit too closely on the aluminium dish, consequently

ion of Moisture in Nitro

Soc. Chem. Ind., Fe

matter when heated for 12 hours on the water bath, and should have a specific gravity of 0.87 at 100° F., and a melting point of 86° F.

ation of wood, and many other organic compounds. Crude wood spirit, which has been freed from acetic acid, consists in the main of a mixture of acetone and methyl- alcohol. The two substances may be roughl

ever, by the dry distillation of

Ca = CH{3}.CO.C

es on standing, is well pressed, to free it from impurities, decomposed by distillation with dilute sodium carbonate, and the aqueous distillate of pure acetone dehydrated over calcium chloride.

ture of cordite should conform

ATION FO

n evaporation at 212° F. On distillation, four-fifths by volume of the quantity taken must distil over at a temperature not exceeding 138° F. The residual

f potash, added to 100 c.c. of the acetone, must retain its distinctive colour f

ethod must not show more than 0.005 per

on (1 gramme to 1,000 c.c. of 50 per cent. alcohol) added as an indicator, add from a burette N/100 sodi

r acidity, and the pipettes used for measuring should not be blown out, as

Zeit., 1895, xix., p. 1384), which consists in shaking together equal volumes of acetone and petroleum e

, 19, 316- 320) has improved Squibb's modification of Robinea

t. solution of h

l solution of so

ade up to a litre; dissolving 257 grms. of sodium hydroxide (by alcohol) in water, likewise made up to a

a hot solution of 120 grms. of crystallised sodium carbonate in 400 c.c. of water. After cooling, the clear liquid is decanted, the

f the acetone, containing

arch with 5 c.c. of cold water, then adding 20 c.c. of boiling water, b

ure is then acidified with the hydrochloric acid solution, and while agitated, an excess of sodium thiosulphate solution is added, the mixture being afterwards allowed to stand a few minutes. The starch indic

Testing of Acetone," C

March 1900,

metric method for the estimation of acetone, depending on the formation of bromoform, and

2}H_{5}OH = 3CO + C_{2

ally suitable for this purpose for several reasons. It is very readily formed by the action of bromine and potash on acetone, and although very volatile in steam, it is not liable to loss due to its own evaporation. Furth

ot rid of by boiling for a minute or two with a little more caustic potash. The mixture is then distilled until the distillate is free from bromoform, halogen being tested for in the usual manner. Water is added to the contents of the flask if necessary. It may be here observed that no acetone can be detected in the distillate by means of the mercuric oxide test, and free bromine is also absent. The condenser having been washed out with a little alcohol, in order to remove any traces of bromoform which may have collected, the distillate and washings are mixed with 50 c.c. of alcohol and sufficient solid caustic potash to make an approximately 10 per cent. solution. The mixture is then heated on the water bath under a reflux condenser until the bromoform is

ng 9.61 per cent. acetone gave 1.7850

0.96 per cent. acetone gave 0.5847 gr

It is best done by weighing out about 1,000 grms. upon a paper tray, which has been previously dried in the oven at 100° C. for some time, and become constant in weight. The trayful of cot

_{2} to remove camphor. | |_______________________________________________________________________| | | | ~B.~ | | | | Add phenol-phthalein and titrate with alcoholic potash, 1 c.c. normal | | KHO = .330 grm. resin, and add considerably more KHO. Evaporate, | | dissolve residue in water, shake with ether, and separate. | |_______________________________________________________________________| | | | Ethereal Solution evaporated leaves paraffin. | |_______________________________________________________________________| | | | Aqueous Solution- | | Add bromide, acidify with HCl, separate any resin and precipitate, | | filtrate with BaCl_{2} BaSO_{4} x .1373 = Sulphur. | |_______________________________________________________________________| | | | Residue- | | Dry, weigh, and exhaust with water preferably in Soxhlet. | |_______________________________________________________________________| | | | | Solution- | Residue- | | Contains metallic | Dry, weigh, and agitate an aliquot part with | | nitrates, chlorates, | with H_{2}SO_{4} and H

It is better, therefore, to extract some of the original substance with water, a

r to 1 alcohol). The flask is then corked and allowed to digest, with repeated shaking, for two or three hours. The whole is then transferred to a linen filter, and when the solution has passed through the filter, is washed with a little ether, and pressed in a hand-screw press between folds of filter paper. The sample is then returned to the flask, and the previous treatment repeated, but it will be sufficient for it to digest for one hour the second time. T

shakings, in a 200 c.c. stoppered measure for six hours; 75 c.c. of the clear solution are then drawn off by the aid of a pipette and evaporated in a dish on the water bath, and finally in the water oven at 120° F

= 4.6 in 50 =

of ether are then added, and the mixture is stirred for several minutes. After removing the stirrer, the cup is lightly covered with an aluminium lid, and is then placed in the steel cup of a centrifugal machine, which is gradually got up to a speed of 2,000 revolutions per minute, the total centrifugal force at the position occupied by the cups (which become horizontal when in r

washing process is then repeated until all soluble matter has been removed. This may require about seven or eight (or for samples with much insoluble matter ten or twelve or more) washings, but as the extraction proceeds, the period of rotation may be somewhat reduced. After extraction is completed, the insoluble matter is transferred to a Gooch crucible with the usual asbestos pad,

sample are boiled with a saturated solution of sodium sulphide, and then allowed to stand for forty-eight hours, and afterwards filtered or decanted, and again boiled with fresh solutions of sulphide, and again filtered

cellulose, but decomposes nitro-cellulose with the formation of a reddish brown compound, which is soluble in water. In the determination, 5 grms. of gun-cotton are heated to 40° or 50° C. on the water bath with 150 c.c. of the reagent, the liquid being shaken at intervals for twenty to thirty minutes; or the mixture may be allowed to stand for a few hours at the ordinary temperature. The brown-red solution is decanted from the undissolved residue, and the latter washed with alcohol and with water, by decantation, and then on the filter with hot water, to which a little hydrochloric acid is added for the final washings. For ordinary work this cellulose is dried immediately and weighed, but in ex

N/2 hydrochloric acid, and diluted with water to about 250 c.c., and shaken for about fifteen minutes. The liquid is then decanted, and washed with water unt

le, he then moistens it with a mixture of alcohol and ether, in which paraffin has been dissolved to saturation, and filtered and mixed with one-fourth of its volume of water. Some fragments of solid paraffin are then added, and the ether set on fire. Whilst this is in progress the crucible is kept in an oblique position, and is rotated so that the gun-cotton may absorb the paraffin uniformly. The partially charred residue is now rubbed down with a rounded glass rod, and the crucible is covered and heated

blue colour becomes less intense, and here and there grey fibres can be observed, though not in proportion to the increase in the nitrogen. Below 12.4 per cent. of nitrogen, the fibres show a grey lustre, which usually appears yellow when the top light is cut off. Below 10 per cent. of nitrogen, the structure is invariably partially destroyed and no certain observations possible.

erally give the analyst a very fair idea of the composition of his sample. If we regard gun-cotton as the hexa-nitro-cellulose, the theoretical amount of nitrogen required for the formula is 14.14 per cent., and in the same way for collodion-cotton, which consists of the lower nitrates, chiefly, however, of the penta- nitrate, th

on has entirely dissolved to a clear solution, raise the pressure tube of the nitrometer so as to bring the mercury in the measuring tube close up to the tap. Open the tap in order to allow of the escape of any air bubbles, and clean the surface of the mercury and the inside of the cup with a small piece of filter paper. Now close the tap, and pour the solution of the nitro-cotton into the cup. Rinse out the bottle with 15 c.c. of sulphuric acid, contained in a pipette, pouring a little of the acid over the stopper of the weighing bottle in case some of the solution may be on it. Now lower the pressure tube a little, just enough to

41.-ORDINARY FORM

ved to assume the temperature of the room. A thermometer should be hung up close to the bulb of the measuring tube. At the end of the twenty minutes, the levels of the mercury in the pressure and measuring tubes are equalised, and the final adjustment obtained by slightly opening the tap on the measuring tube (very slightly), after first adding a little sulphuric acid to

COLLODIO

suring tube = 114.6 c.c. NO. Baro

m. is enough in the

amme N, and correcting for tempe

= .003665), for tempe

h

6272)/(801.7 x. 6) = 1

: See Table

etter to take a much smaller quantity of the substance. From 0.1 to 0.2 grm. is quite sufficient. This

AM

en gave 32.5 c.c. NO. Baromete

ref

01.78 x.1048) = 18.46 per cen

ened out in the middle to a bulb, and is graduated above and below into 1/10 c.c. The capacity of the whole apparatus is 130 c.c.; that of each portion of the tube bein

2. FIG. 43. SOME NEW

ighed quantity of the powder is dropped bodily into the bulb K. From 4 to 5 c.c. of sulphuric acid which has been heated to 30° C. are then added through the funnel T, the tap H being immediately closed. When the powder has dissolved-a pr

n place, the gas being transferred from the one to the other by joining them by means of indiarubber tubing, and then driving the

gas at 0°

milligrammes

" nitr

(HNO_{3})

aNO_{3}) sod

NO_{3}) pota

nd which dips under a solution of caustic soda contained in a trough, and the end placed under a graduated tube, also full of caustic soda. From 0.12 to 0.16 grm. cotton dissolved in 5 to 6 c.c. of sulphuric acid is allowed to flow into the flask, which contains the ferrous chloride and hydrochloric acid, and in which a vacuum has been formed by boiling, and then closing the taps. The s

ask, acidified with hydrochloric acid, and its surface covered with a layer of petroleum oil. About .5 grm. of the nitro-glycerine is then introduced, and the flask heated on the water bath. When the sample is completely decomposed, the l

e. To fill the apparatus with the soda solution, the gas burette is put on the indiarubber stopper of basin W, and firmly clamped down. Then the taps A and C are opened, and B closed. When the burette is filled with soda solution half-way up the funnel Y, A and C are closed, and B opened. The arrows

g. 44. SCHULTZE-T

lution of protochloride of iron and 10 to 15 c.c. concentrated hydrochloric acid are poured, which are sucked up into the developing flask f by opening clip E, air being carefully kept from entering. The clip E is now closed, and tube i is put underneath the burette, and the development of NO gas is commenced by heating the contents of the flask f. When the pressure of the gas in the flask has become greater than the pressure of the atmosphere, the connecting tube begins to swell at i, whereupon clip D is opened, and the boiling continued with frequent shaking of the bulb, until no more nitrous gas bubbles rise up into

Decomposition Flask for

a paper filter, and acidify filtrate with a few drops of HCl. The soda solution used has a sp. gr. of 1.210 to 1.260; equals 25° to 30° B. The nitro-cellulose is dried in quantities of 2 grms. at 70° C. dur

Chenel, of the Laboratoire Centrale des Poudres, whose method of procedure is as follows:-0.5 grm. of the finely powdered substance is digested in the cold with a solution of 1.2 grm. of phenol and 0.4 grm. phosphoric anhydride in 30 c.c. of sulphuric acid. The mixture is kept well shaken until the solution is complete. From 3 to 4 grms. of zinc-dust is then cautiously and

, Zeitschrift Anal. Chem

ntralblatt, 1886, pp. 434-484. See al

-phenol becomes fixed in the state of ammonia. M. Chenel is perfectly satisfied with the results obtained, but he points out that the success of the operation depends upon the complete conversion of the phenol into the mono-nitro derivatives. This takes p

| | | | 13.96 | | Ammonium nitrate | 35.00 | 35.31 | | | | 34.90 | | | | 34.96 | | Barium nitrate | 10.72 | 10.67 | | | | 10.62 | | Nitro-glycerol | 18.50 | 18.45 | | Di-nitro-benzol[A] | 16.67 | 16.78 | | | | 16.57 | | Para-nitro-phenol | 10.07 | 10.03 | |

r cent. for picric acid and 16.54 per cent. for

ly added to a solution of 2 grms. of phosphorus in about 15 or 20 c.c. of bisulphide of carbon, this solution being contained in a flask of 250 c.c. capacity. The flask and its contents are heated on the water bath at 100° C. with constant attention, until the last traces of the carbon bisulphide have distilled away. It is then cooled, and the iodide of phosphorus is detached from the sides of the flask by shaking, but not expelled. The next step is to add about 0.5 to 0.6 grm. of the substance that is to be analysed, after whi

gun-cotton. Personally, I have never been able to obtain satisfactory results with this process in the analysis of nitro-cellulose, and

ages of Nitrogen and Oxi

sed in or as

UL? NITRO

nt. pe

{3}H_{5}(ONO_{2})

C{12}H_{14}O_{4}(ONO_

e C{6}H_{8}O_{5}(ONO

C{6}H_{5}NO_{2

C_{6}H_{4}(NO_{2}

C{6}H_{3}(NO_{2}

C{7}H_{7}NO_{2

e C_{10}H_{7}NO_

e C_{10}H_{6}(NO_{2

6}H_{7}(NO_{3}){

}H_{8}O_{4}(HNO_

ric

C_{6}H_{2}OH(NO_{

e C{6}H_{3}Cl(NO_{2

rate NH{4}NO

rate NaNO_

itrate KNO_

id HNO_{3

te Ba(NO_{3}

To prevent interference from camphor, the following treatment is suggested by H. Zaunschirm (Chem. Zeit., xiv., 905). Dissolve a weighed quantity of the celluloid in a mixture of ether- alcohol, mixed with a weighed quantity of washed and ign

eep red liquid is produced, owing to the formation of potassium iso-purpurate, which crystallises in small reddish-brown plates with a beetle-green lustre. This, by reaction with ammonium chloride, gives ammonium iso-purpurate (NH_{4}C_{8}H_{4}N_{5}O_{6}), or artificial murexide, which dies silk and wool a beautiful red colour. On add

insoluble on dissolving the sample in boiling water. The separation is

e solutions of the picrates of barium, silver, and calcium. These salts are readily made by boiling picric acid with the carbonates of the

the red fumes evolved on warmin

s of Potash and Sodium~, &c., lea

acid, 50 c.c. of warm benzene may be advantageously substituted for ether. Sugar may be separated from the other impurities by treating the residue insoluble in ether or benzene with rectified spirit, in which sugar and boric acid alone will dissolve. If boric acid be present, the alcoholic solution will burn with a green flame. Mono- and di-nitrophenic acids lower the melting point (122° C). Their calcium salts

sed by carbonate of potash, this salt is thrown down in yellow crystalline needles, which require

above, and sodium picrate is readily soluble in water

d a solution of sulphate of cinchonine acidulated with H_{2}SO_{4}. The precipitated picrate of cinchonine [C_{20}H_{24}N_{2}O(C_{6}H_{2}N_{3}O_{7})_{2}] is washed with cold water, rinsed off the fi

inimum specific gravity of 1.261 at 15° C. This can be determined, either by the aid of a Sartorius specific gr

lman and Berry, Analyst,

nic Analysis," v

the glycerine, and evaporate it at a temperature of about 160° C. in a platinum basin, and finish in an air

r cent. is not always prejudicial to th

r of its bulk of N/10 silver nitrate solution added to it, then shake it, and place in a dark cupboard for fifteen minu

t, 1 c.c. of glycerine heated to boiling with 1 c.c. of ammonia solution and three drops

tor, and allowed to stand for some time. It should, if the glycerine is a good one, have separated from the mixed acids in ten minutes, and the line of demarcation between the nitro-glycerine and the acid should be clear and sharp, neither should there be any white flocculent matter suspended in the liquid. The excess of acids is now drawn off, and the nitro-glycerine shaken once or twice with a warm solution of carbonate of soda, and afterwards with water alone. The nitro-glycerine is then drawn off into a weighed beaker, the surface dried with a piece of filter paper, and weighed; 100 parts of a good glycerine should yield about 230 of nitro

d to 300 c.c. in a beaker, a few drops of a 1 per cent. solution of phenolphthalein and 10 c.c. of normal caustic soda solution are

s of alcoholic phenolphthalein[A] are titrated with hydrochloric acid or sodium hydroxide; not more than 0.3 c.c. normal hydrochloric acid o

and Berry prefer l

her washed with three separate lots of water. The water must have been recently boiled, and be quite free from CO_{2}. All the free fatty acid is now in the ether, and no other soluble aci

dded to it, and enough dilute H_{2}SO_{4} to render it distinctly acid. It is well shaken. All the fatty acids go into the ether. The aqueous solution is then removed, and the ether well washed to remove all H_{2}SO_{4}. After

hides, cyanogen compounds, organic acids (especially oleic acid and fatty acids[A]), rosin products, and other organic bodies. It is also said to be

ouble in nitrating, white flocculent matter

n a test tube with alcohol and sulphuric acid, when, if present, compound ethers, such as ethylic

through the diluted sample, when a white flocculent precipitate of elaidic acid, which is less soluble than oleic acid, will be thrown down. By agitating glycerol with chloroform, fatty acids, rosin oil, and some other impu

little water, neutralised with sodium carbonate, and then titrated with a d

ht but distinct excess, and the mixture well agitated. The formation of an abundant precipitate, which rapidly subsides, is an indication of considerable impurity in the sample. To ascertain its amount, the precipitate is first washed by decantation, and then collected on a tared, or preferably a double counter-poised filter, where it is further washed, dried at 100° to 1

itating with basic lead acetate as already described, and determining the nitrogen by the Kjeldahl

der an upright condenser for one and a half hours. After cooling, 50 c.c. of water are added, and the mixture heated until all the triacetin has dissolved. The liquid is then filtered into a large flask, the residue on the filter is well washed with water, the filtrate quite cooled, phenolphthalein is added and the fluid exactly neutralised with a dilute (2 to 3 per cen

of the glycerine to triacetyl is imperfect. Triacetin in contact with water gradually decomposes. After acetylation is complete, therefore, the operations must be conduc

er substances as might injuriously affect the results, and that the heating of the mixture takes place in an air bath free from carbonic acid. The increase in weight in the litharge, minus the weight of substance not volatilisable from 2 gr

gen by the permanganate method described under nitro-glycerine. Now determine the total acidity of the mixture by means of a tenth normal solution of sodium hydrate, and calculate it as n

per cent. HNO_{3} = 86.39 per cent., then (

is of sampl

cid = 67.20

07 " |- Specific

= 12

trometer. Two c.c. is a convenient quantity in the above case, then 2 x 1.7075 (specific gravity) = 3.414 grms. taken, gave 145 c.c. NO (barometer =

on (gives about 123 c.c. gas); grind very fine, and dissolve in a very little hot water in the cup of the nitrometer; use about 15 c.c. concentrated H_{2}SO_{4}. One cu

sure to the air in open vessels the hydrogen sulphide is for the most part dissipated. The solution is then titrated with potassium hydroxide (KOH), as well as another quantity of hydrochloric acid, equal to that used with the fulminate. As the mercury chloride is reconverted into hydrochloric acid by the hydrogen sulphide, and as the hydroxylamine does not neutralise to litmus the hydrochloric acid

ry, titrated by iodine for hydroxylamine, gave nitrogen equal to 9.85 per cent., and when evaporated with hydroxyl ammonium chloride equal to 9.55 per cent. A solution of 2.6665 grms. fulminate in HCl of know

I. I

0.42 70.4

9.86 9.85

.45 ...

1.27 ...

__

0.

and to estimate these substances in the presence of each other by ordinary analytical methods is a difficult process. Since the separation of antimony sulphide and mercury fulminate in the presence of potassium chlorate necessitates the treatment of the mixture with hydrochloric ac

as, and that chlorate of potash and sulphide of antimony were insoluble in pure acetone saturated with ammonia; these observations at once afforded a simple method of separating the three ingredients of cap composition.

ectly on to the filter paper and is then covered with the solution of acetone and ammonia and allowed to stand thirty-four hours. It is then washed repeatedly with the same solution until the washings give no coloration with amm

ht of compo

filter

er first

second e

= weight of

= " "

sulphide o

uld be finely groun

his method of two mixtures of kn

nd. | Taken. | Found. | |____________________|____________|____________|____________|____________| | | | | | | | Antimony Sulphide | 36.47 | 36.25 | 37.34 | 37.22 | | Potass

osition well stirred from the bottom. After the addition of 0.5 grm. of pure sodium, thiosulphate, the contents of the dish, is well stirred for two and a half minutes. One drop of methyl orange is then added, and the solution titrated with N/20 sulphuric acid, which has been standardised against weighings of 0.05-0.1 grm. fulminate to which 25 c.c. of water is added in a porcelain dish, then 0.5 grm. of thiosulphate, and after stirring for two and a half minutes, titrated with N/20 sulphuric acid. The small amount of antimony sulphide present does not interfere with the recognition of the end point. After titration, the solution is filtered through a small 5-1/2 cm. filter paper, which retains the antimony sulphide. The f

these are uniform within a negligible error, it does not affect the value of the result

0.0001 | | 0.0074 | 0.0071 | -0.0003 | | 0.0068 | 0.0066 | -0.0002 | |____________________|___________________|___________________| | | | | | Stibnite Taken. |Sb_{2}S_{3}, Found.| Error. | | Grm. | Gr

OF GASES FOR TEMPERATURE, GIVI

+ dt)) (d = 0.003665)

804.0093 .3 | 777.5480 | .1 | 790.9179 | .9 | 804.2879 .4 | 777.8266 | .2 | 791.1965 |16.0 | 804.5664 .5 | 778.1051 | .3 | 791.4750 | .1 | 804.8449 .6 | 778.3836 | .4 | 791.7536 | .2 | 805.1235 .7 | 778.6622 | .5 | 792.0321 | .3 | 805.4020 .8 | 778.9407 | .6 | 792.3106 | .4 | 805.6806 .9 | 779.2193 | .7 | 792.5892 | .5 | 805.9591 7.0 | 779.4978 | .8 | 792.8677 | .6 | 806.2376 .1 | 779.7763 | .9 | 793.1463 | .7 | 806.5162 .2 | 780.0549 |12.0 | 793.4248 | .8 | 806.7947 .3 | 780.3334 | .1 | 793.7033 | .9 | 807.0733 .4 | 780.6120 | .2 | 793.9819 |17.0 | 807.3518 .5 | 780.8905 | .3 | 794.2604 | .1 | 807.6303 .6 | 781.1690 | .4 | 794.5390 | .2 | 807.9089 .7 | 781.4476 | .5 | 794.8175 | .3 | 808.1874 .8 | 781.7261 | .6 | 795.0960 | .4 | 808.4660 .9 | 782.0047 | .7 | 795.3746 | .5 | 808.7445 8.0 | 782.2832 | .8 | 795.6531 | .6 | 809.0230 .1 | 782.5617 | .9 | 795.9317 | .7 | 809.3016 .2 | 782.8403 |13.0 | 796.2102 | .8 | 809.5801 .3 | 783.1188 | .1 | 796.4887 | .9 | 809.8587 .4 | 783.3974 | .2 | 796.7673 |18.0 | 810.1372 .5 | 783.6959 | .3 | 797.0458 | .1 | 810.4175 .6 | 783.9544 | .4 | 797.3244 | .2 | 810.6943 .7 | 784.2330 | .5 | 797.6029 | .3 | 810.9728 .8 | 784.5115 | .6 | 797.8814 | .4 | 811.2514 .9 | 784.7901 | .7 | 798.1600 | .5 | 811.5299 9.0 | 785.0686 | .8 | 798.4385 | .6 | 811.8084 .1 | 785.3471 | .9 | 798.7171 | .7 | 812.0870 .2 | 785.6257 |14.0 | 798.9956 | .8 | 812.3655 .3 | 785.9042 | .1 | 799.2741 | .9 | 812.6441 .4 | 786.1828 | .2 | 799.5527 |19.0 | 812.9226 .5 | 786.4613 | .3 | 799.8312 | .1 | 813.2011 .6 | 786.7398 | .4 | 800.1098 | .2 | 813.4797 .7 | 787.0184 | .5 | 800.3883 | .3 | 813.7582 .8 | 787.2969 | .6 | 800.6668 | .4 | 814.0368 _____|_____________|_____|_____________|_____|_____________ ___________________________________________________________ | | | | | t. | 760x(1+dt). | t. |