Test-tube

At lower temperatures, the crystals increase in size, and form networks that trap the liquid and hinder its ability to flow. The pour point is attained which can, depending on the diesel fuel, vary between -15 and -30°C. This characteristic (NF T 60-105) is determined, like the cloud point, with a very rudimentary device (maintaining a test tube in the horizontal position without apparent movement of the diesel fuel inside). 

Antirust properties (inhibited mineral oils) NFT 60-151 ISO 7120 ASTM D 665 Spots on a test tube after agitation with oil water... 

Before starting the realisation of silicium coils, we construct a simpler probe with a 27 mm long excitation coil and 16 wired coil sensors, with 1 mm diameter and 1 mm long. We cannot hope any reconstruction with such a probe, but this allows to validate the whole approach. We tried it with test tubes with longitudinal or circonferential notches, external or internal, 100 pm wide, 100%, 60%, 40%, 20% and 10% deep. Our attention has been especially focused on circonferential notches, which are difficult to detect with usual probes. For example, the measurement signals at 240 kHz standard frequency are shown figure 6 7. 

Students frequently attempt to seal liquids in test-tubes the latter are, however, usually too fragile for this purpose. 

General Considerations. With liquids and solutions the most serious losses are due to (a) transference from spherical flasks and difficulties of drainage, (b) retention by filter-papers, (c) absorption by large corks. As containers for small quantities of liquids it is therefore often convenient to use pear-shaped flasks A and conical test-tubes or centrifuge-tubes B (Fig. 29). (In this and subsequent figures, approximate dimensions are given to indicate a convenient size.)... 

A skilled worker can use a micro-Bunsen burner for most types of heating. Nevertheless, as there is a tendency for a liquid to shoot out of a small test tube when heated, it is preferable to place the tube in a hot water-bath or in a metal heating block. A small glycerol bath is suitable for distillations and heating under reflux, the glycerol being subsequently easily removed from flasks, etc., by washing with water. 

When the correct solvent for recrystallisation is not known a procedure similar to that given on pp. 15-16 should be followed, but on the semi-micro scale not more than 10 mg. of the solid should be placed in the tapered-end test-tube (Fig. 29(B)) and about o i ml. of the solvent should be added from the calibrated dropping-pipette (Fig. 30(B)). If the compound dissolves readily in the cold, the solvent is unsuitable, but the solution should not be discarded. [In this case recourse should be had to the use of mixed solvents (p. 18). For example if the substance is very soluble in ethanol, water should be added from a calibrated pipette with shaking to determine whether crystallisation will now take place, indicated by a cloudiness or by the separation of solid.]... 

The liquid becomes progressively darker in colour, and then effervesces gently as ethylene is evolved. Allow the gas to escape from the delivery-tube in T for several minutes in order to sweep out the air in F and B. Now fill a test-tube with water, close it with the finger, and invert the tube in the water in T over the delivery-tube so that a sample of the gas collects in the tube. Close the tube again with the finger, and then light the gas at a Bunsen burner at a safe distance from the apparatus. If the tube contains pure ethylene, the latter burns with a clear pale blue (almost invisible) flame if the ethylene still contains air, the mixture in the test-tube ignites with a sharp report. Allow the... 

The oxime is freely soluble in water and in most organic liquids. Recrystallise the crude dry product from a minimum of 60-80 petrol or (less suitably) cyclohexane for this purpose first determine approximately, by means of a small-scale test-tube experiment, the minimum proportion of the hot solvent required to dissolve the oxime from about 0-5 g. of the crude material. Then place the bulk of the crude product in a small (100 ml.) round-bottomed or conical flask fitted with a reflux water-condenser, add the required amount of the solvent and boil the mixture on a water-bath. Then turn out the gas, and quickly filter the hot mixture through a fluted filter-paper into a conical flask the sodium chloride remains on the filter, whilst the filtrate on cooling in ice-water deposits the acetoxime as colourless crystals. These, when filtered anddried (either by pressing between drying-paper or by placing in an atmospheric desiccator) have m.p. 60 . Acetoxime sublimes rather readily when exposed to the air, and rapidly when warmed or when placed in a vacuum. Hence the necessity for an atmospheric desiccator for drying purposes. 

Hydrolysis of Ethyl Bromide. Add -a few drops of pure freshly distilled ethyl bromide to 2-3 ml. of aqueous silver nitrate solution in a test-tube and shake. Only a faint opalescence of silver bromide should be formed. -Now carefully warm the mixture in a small Bunsen flame, with gentle shaking silver bromide soon appears as a white suspension which rapidly increases in quantity and becomes a heavy precipitate. The ethyl bromide is thus moderately stable in cold water, but rapidly hydrolysed by hot water. 

Reactions of Aspirin, (i) Distinction from Salicylic acid. Shake up with water in two clean test-tubes a few crystals of a) salicylic acid, (0) aspirin, a very dilute aqueous solution of each substance being thus obtained. Note that the addition of i drop of ferric chloride solution to (a) gives an immediate purple coloration, due to the free —OH group, whereas (b) gives no coloration if the aspirin is pure. 

Place a few drops of nitromethane in a test tube, add about 3 times as much concentrated hydrochloric acid, and then a piece of granulated tin. The tin dissolves in the acid and the nascent hydrogen produced reduces the nitromethane to monomethylamine ... 

Dissolve a small portion of the sodium derivative in a few mi. of water in a test-tube, and add one drop of ferric chloride solution. A deep red coloration is produced, but rapidly disappears as the iron is precipitated as ferric hydroxide. The sodium (derivative (A) of the nitromethane wh dissolved in water undergoes partial hydrolysis,... 

Dissolve 5 g. (5 ml.) of aniline in 50 ml. of warm dilute sulphuric acid in a conical flask and add 50 ml. of water. Place a thermometer in the solution, immerse the flask in a mixture of ice and water, and cool until the temperature of the stirred solution falls to 5°. Dissolve 4-5 g. of powdered sodium nitrite in 20 ml. of water, and add this solution in small quantities (about 2-3 ml. at a time) to the cold aniline sulphate solution. Keep tne latter well shaken and maintain the temperature at about 5° (see p. 183). When all the sodium nitrite solution has been added, transfer about 5 ml. of the cold solution to a test-tube for each of the following reactions. The remainder of the diazonium hydrogen sulphate solution must be kept in ice-water until required, and then when all the reactions have been carried out, the solution should be poured down the sink. 

Add 2 -3 drops of phenylhydrazine to about 2 ml. of Fehling s solution in a test-tube and shake the mixture vigorously nitrogen is evolved and reddish-brown cuprous oxide is precipitated. The reaction proceeds rapidly on gentle warming, more slowly in the cold. 

Place about i g. of the base in a test-tube, and cover with concentrated (about 20%) sodium hydroxide solution. Bring the mixture gently to the boil, keeping the test-tube lightly closed with the finger meanwhile to prevent undue escape of vapour.. A.s the solution boils a strong fishy odour of dimethylamine is detected, and white fumes form when the test-tube is held near an open bottle of concentrated... 

To 2 ml. of the ester in a test-tube add slightly more than the same volume of a cold saturated aqueous copper acetate solution. The blue colour of the latter turns immediately to a pale green. Now shake the tube vigorously in order to produce an emulsion of the ester in the aqueous layer. Scratch the sides of the tube with a rod, and shake vigorously as before. Crystallisation may be delayed for about 5 minutes, but, when once started, rapidly gives a copious precipitate... 

Sodium benzoate,—Burns with great difficulty, and after prolonged heating leaves a white infusible residue of NajCOj. Scrape this residue into a test-tube, and test for carbonate in the usual way. Typical of alkali salts of carboxylic acids. 

Sodium mlphanilate.—Burns with difficulty, leaving a residue of (chiefly) sodium sulphide. Add dil. HCl, and confirm without delay the evolution of HjS by means of a filter-pa per moistened with lead acetate solution. Typical of salts of the sulphonic acids. Acetone sodium bisulphite.—Almost non-inflammable, leaving a colourless residue of sodium sulphite and sulphate. Transfer residue to a test-tube, add dil. HCl, warm, and confirm the SO2 evolved. 

The sodium fusion and extraction, if performed strictly in accordance with the above directions, should be safe operations. In crowded laboratories, however, additional safety may be obtained by employing the follow ing modification. Suspend the hard-glass test-tube by the rim through a hole in a piece of stout copper sheet (Fig. 69). Place 1 -2 pellets of sodium in the tube, and heat gently until the sodium melts. Then drop the organic compound, in small quantities at a time, down — =. the tube, allowing the reaction to subside after each addition before the next is made. (If the compound is liquid, allow two or three small drops to fall at intervals from a fine dropping-tube directly on to the molten sodium.) Then heat the complete mixture as before until no further reaction occurs. 

Sulphur. THE LASSAIGNE SODIUM TEST. The sodium fusion will have converted any sulphur present in the original compounds to sodium sulphide. Dissolve a few crystals of sodium nitroprusside, Na8[Fe(CN)5NO],zH20, in water, and add the solution to the third portion of the filtrate obtained from the sodium fusion. A brilliant purple coloration (resembling permanganate) indicates sulphur the coloration slowly fades on standing. Note, (i) Sodium nitroprusside is unstable in aqueous solution and therefore the solution should be freshly prepared on each occasion, (ii) This is a very delicate test for sulphides, and it is essential therefore that all apparatus, particularly test-tubes, should be quite clean. 

Proceed as follows for both solid and liquid compounds. By means of a test-tube holder, hold the tube in a horizontal position, and by means of a small flame gently heat the mixture at the open end. Increase the size of the flame gradually until the mixture is red-hot at this end. Now slowly and cautiously extend the heating towards the closed end until the whole of the mixture is red-hot. (If during the extension of the heating, the mixture tends to be pushed out of the tube by the evolution of gas, stop the heating momentarily, and rotate the... 

Now heat the tube very gently at first and then more strongly. A non-conden-sible product such as hydrogen or methane is best detected by collecting a sample of the gas in a test-tube as shown in Fig. 71(A). A condensible product such as benzene or phenol should be collected by twisting the delivery-tube downwards and collecting the liquid in a few ml. of water in a test-tube as shown In Fig. 71(B). 

There is no satisfactory chemical way of distinguishing betn een ethane and methane, both of which burn with an almost non-luminous flame this fact however is quite unimportant at this stage of the investigation. Hydrogen also burns with a non-luminous flame and w hen the open end of a test-tube full of the gas is placed in a Bunsen flame, a mild explosion with a very characteristic report takes place. 

These compounds require a more concentrated NaOH solution (e.g., 30%) for a quick reaction on a test-tube scale. 

Hydrolyses to ethanol and acid on being heated for a few minutes. Cool, add a few ml. of water and then cone. HCl, and cool again. Crystals of benzoic acid separate out. Complete hydrolysis cannot be carried out effectively on a test-tube scale. ( ec p. 355). 

Place about 5 ml. of NagCOj solution in (p. 318) a test-tube, add a few fragments of unglazed porcelain, and boil gently to ensure complete absence of bicarbonate and of free carbon dioxide. Cool the solution, add about 01 g. of the substance to be tested, and... 

Place a small quantity (t.e., about o-i g.) of the following substances (finely powdered) in a clean dry test-tube and add about I ml. of cone. H2SO4. Note any reaction in the cold, and then warm gently. Note any effervescence and any pronounced blackening (as distinct from mere darkening in colour). 

Take two test-tubes A and B in A place about 5 ml. of neutralised tartaric acid solution and in B place 5 ml. of distilled water. To each solution add 3-4 drops of ferric chloride solution. Place a piece of white paper under the tubes, look down their length and note that A is definitely yellow compared with the control tube B. This yellow colour is given by a-hydroxy-carboxylic-acids, lactic acid, tartaric acid, citric acid. 

Dinitrobenzoylation. To 0 5 g. of powdered 3,5-dinitro benzoyl chloride (preparation, p. 240) in a dry test-tube, add 2 ml. of dry methanol and warm the mixture until a clear solution is obtained. Cool and filter off the solid ester which separates. Recrystallise from petroleum (b.p. 60-80 ), and take the m.p. (M.ps., pp. 536, 537.)... 

Glycol gives the non-volatile oxalic acid. After heating the mixture under reflux for 10 minutes, transfer 2 ml. of the cold product to a test-tube and add 4 ml. of cone. H2SO4. Note the production of carbon monoxide and carbon dioxide on heating (p. 350). 

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