CHAPTER II
Easy Examples of Laboratory Glass-Blowing—Cutting and Sealing Tubes for Various Purposes; Test-Tubes, Pressure-Tubes, Tubes for High Temperature Experiments—Thermometer-Bulbs, Bulbs of Special Glass, Pipettes, Absorption-Bulbs or Washing-Bulbs—Joining Tubes; Branches, Exhaustion-Branches, Branches of Dissimilar Glass—Blowing Bulbs; A Thistle Funnel; Cracking and Breaking Glass; Leading and Direction of Cracks—Use of Glass Rod or Strips of Window-Glass; Joining Rod, Feet and Supports—Gripping Devices for use in Corrosive Solutions—The Building Up of Special Forms from Solid Glass.
Perhaps the most common need of the glass-blower whose work is connected with that of the laboratory is for a sealed tube; and the sealing of a tube is an excellent preliminary exercise in glass-blowing.
We will assume that the student has adjusted the blowpipe to give a flame similar to that shown in d, Fig. 1, and that he has learned to maintain a steady blast of air with the bellows; further, we will assume that the tube he wishes to seal is of moderate size, say not more than half an inch in diameter and with walls of from one-tenth to one-fifth of an inch thick.
Fig. 4
A convenient length of tube for the first trial is about one foot; this should be cut off from the longer piece, in which it is usually supplied, as follows:—lay the tube on a flat surface and make a deep cut with the edge of a file. Do not "saw" the file to and fro over the glass. If the file edge has been ground as shown in a, Fig. 3, such a procedure will be quite unnecessary and only involve undue wear; one movement with sufficient pressure to make the file "bite" will give a deep cut. Now rotate the tube through about one-eighth of a turn and make another cut in continuation of the first. Take the tube in the hands, as shown in a, Fig. 4, and apply pressure with the thumbs, at the same time straining at the ends. The tube should break easily. If it does not, do not strain too hard, as it may shatter and cause serious injuries to the hands, but repeat the operation with the file and so deepen the original cuts. In holding a tube for breaking, it is important to place the hands as shown in sketch, as this method is least likely to cause shattering and also minimises the risk of injury even if the tube should shatter. To cut a large tube, or one having very thick walls, it is better to avoid straining altogether and to break by applying a small bead of intensely heated glass to the file cut. If the walls are very thin, a glass-blower's knife should be used instead of a file. The tube and glass-blower's knife should be held in the hand, and the tube rotated against the edge of the knife; this will not produce a deep cut, but is less likely to break the tube. A bead of hot glass should be used to complete the work.
The next operation is to heat the glass tube in the middle; this must be done gradually and evenly; that is to say the tube must be rotated during heating and held some considerable distance in front of the flame at first; otherwise the outer surface of the glass will expand before the interior is affected and the tube will break. From two to five minutes, heating at a distance of about eight inches in front of the flame will be found sufficient in most cases, and another minute should be taken in bringing the tube into the flame. Gradual heating is important, but even heating is still more important and this can only be obtained by uniform and steady rotation. Until the student can rotate a tube steadily without thinking about it, real progress in glass-blowing is impossible.
When the tube is in the flame it must be held just in front of the blue cone and rotated until the glass is soft enough to permit the ends to be drawn apart. Continue to separate the ends and, at the same time, move the tube very slightly along its own axis, so that the flame tends to play a little more on the thicker part than on the drawn-out portion. If this is done carefully, the drawn-out portion can be separated off, leaving only a slight "bleb" on the portion it is desired to seal. This is illustrated by b, Fig. 4.
To convert the seal at b, Fig. 4., into the ordinary form of test-tube seal, it is only necessary to heat the "bleb" a little more strongly, blow gently into the tube until the thick portion is slightly expanded, re-heat the whole of the rounded end until it is beginning to collapse, and give a final shaping by careful blowing after it has commenced to cool. In each case the glass must be removed from the flame before blowing. The finished seal is shown by c, Fig. 4. If desired, the open end may now be finished by heating and rotating the soft glass against the large turn-pin, as illustrated in d, but the turn-pin must not be allowed to become too hot, as if this happens it will stick to the glass. After turning out the end, the lip of glass must be heated to redness and allowed to cool without coming in contact with anything; otherwise it will be in a condition of strain and liable to crack spontaneously. The finished test-tube is shown by e.
When it is necessary to seal a substance inside a glass tube, the bottom of the tube is first closed, as explained above, and allowed to cool; the substance, if a solid, is now introduced, but should not come to within less than two inches of the point where the second seal is to be made. If the substance is a liquid it can more conveniently be introduced at a later stage.
Now bring the tube into the blowpipe flame gradually, and rotate it, while heating, at the place where it is to be closed. Allow the glass to soften and commence to run together until the diameter of the tube is reduced to about half its original size. Remove from the flame and draw the ends apart, this should give a long, thick extension as shown by f, Fig. 4. If any liquid is to be introduced, it may now be done by inserting a thin rubber or other tube through the opening and running the liquid in. A glass tube should be used with caution for introducing the liquid, as any hard substance will tend to scratch the inside of the glass and cause cracking. The final closure is made by melting the drawn-out extension in the blowpipe flame; the finished seal being shown by g, Fig. 4.
If the sealed tube has to stand internal pressure, it is desirable to allow the glass to thicken somewhat more before drawing out, and the bottom seal should also be made thicker. For such a tube, and especially when it has to stand heating, as in a Carius determination of chlorine, each seal should be cooled very slowly by rotating it in a gas flame until the surface is covered with a thick layer of soot, and it should then be placed aside in a position where the hot glass will not come in contact with anything, and where it will be screened from all draughts.
Joining Tube.—We will now consider the various forms of join in glass tubing which are met with in the laboratory. First, as being easiest, we will deal with the end-to-end joining of two tubes of similar glass. a, b, and c, Fig. 5, illustrate this. One end of one of the tubes should be closed, a lip should be turned out on each of the ends to be joined, and both lips heated simultaneously until the glass is thoroughly soft. Now bring the lips together gently, until they are in contact at all points and there are no places at which air can escape; remove from the flame, and blow slowly and very cautiously until the joint is expanded as shown in b, Fig. 5. Reheat in the flame until the glass has run down to rather less than the original diameter of the tube, and give a final shaping by re-blowing. The chief factors of success in making such a join are, thorough heating of the glass before bringing the two tubes together, and avoidance of hard or sudden blowing when expanding the joint. The finished work is shown by c, Fig. 5.
Fig. 5
To join a small glass tube to the end of a large one, the large tube should first be sealed, a small spot on the extreme end of the seal heated, and air pressure used to expand the heated spot as shown in d. This expanded spot is then re-heated and blown out until it bursts as shown in e, the thin fragments of glass are removed and the end of the small tube turned out as shown in f. After this the procedure is similar to that used in jointing two tubes of equal size.
When these two forms of joint have been mastered, a T piece will present but little difficulty. It is made in three stages as shown in Fig. 5, and the procedure is similar to that used in joining a large and small tube. Care should be taken to avoid softening the top of the "T" too much, or the glass will bend and distort the finished work; although a slight bend can be rectified by re-heating and bending back. Local re-heating is often useful in giving the joint its final shape.
An exhaustion branch is often made by a totally different method. This method is shown by g, h, and i, Fig. 5; g is the tube on which the branch is to be made. The end of a rod of similar glass should be heated until a mass of thoroughly liquid glass has collected, as shown, and at the same time a spot should be heated on that part of the tube where it is desired to make the branch. The mass of hot glass on the rod is now brought in contact with the heated spot on the tube and expanded by blowing as shown by h. The air pressure in the tube is still maintained while the rod is drawn away as shown by i. This will give a hollow branch which may be cut off at any desired point, and is then ready for connection to the vacuum pump.
If the rod used is of a dissimilar glass, the branch should be blown much thinner. Such a branch will often serve as a useful basis for joining two tubes of different composition, as the ordinary type of branch is more liable to crack when made with two glasses having different coefficients of expansion.
Blowing Bulbs.—A bulb may be blown on a closed tube such as that shown by c, Fig. 5, by rotating it in the blowpipe flame until the end is softened, removing it from the flame and blowing cautiously. It is desirable to continue the rotation during blowing. In the case of a very small tube, it is sufficient to melt the end without previous sealing, rotate it in the flame until enough glass has collected, remove from the flame and blow while keeping the tube in rotation.
Thermometer Bulbs.—If the thermometer is to be filled with mercury, it is desirable to use a rubber bulb for blowing, as moisture is liable to condense inside the tube when the mouth is used, and this moisture will cause the mercury thread to break. In any case, a slight pressure should be maintained inside the thermometer tube while it is in the flame; otherwise the fine capillary tube will close and it will be very difficult to expand the heated glass into a bulb.
Large Bulbs.—When a large bulb is needed on a small or medium sized tube, it is often necessary to provide more glass than would be obtained if the bulb were blown in the ordinary way. One method is to expand the tube in successive stages along its axis, as shown by a, Fig. 6. These expanded portions are then re-heated, so that they run together into one hollow mass from which the bulb is blown; b and c, illustrate this. Another method, and one which is useful for very large bulbs, is to fuse on a length of large, thick-walled, tubing. The heat reflector, g, Fig. 3, should be used, if necessary, when making large bulbs. It consists of a sheet of asbestos mounted in a foot, and is used by being placed close to the mass of glass on the side away from the blowpipe flame while the glass is being heated.
Fig. 6
Bulbs of Dissimilar Glass.—These may be made by the second method given under "Large Bulbs," but the joint should be blown as thin as possible. Further instructions in the use of unlike glasses are given on page 94.
A Bulb in the Middle of a Tube.—Unless the bulb is to be quite small, it will be necessary to join in a piece of thick glass tubing, or to draw the thin tube out from a larger piece, thus leaving a thick mass in the middle as shown by d, Fig. 6. This mass of glass should now be rotated in the blowpipe flame until it is quite soft and on the point of running together. Considerable practice will be necessary before the two ends of the tube can be rotated at the same speed and without "wobbling," but this power must be acquired. When the glass is thoroughly hot, remove from the flame, hold in a horizontal position, and expand by blowing. It is essential to continue the rotation while this is done. Should one part of the bulb tend to expand more than the other, turn the expanded part to the bottom, pause for about a second, both in rotating and blowing, in order that the lower portion may be cooled by ascending air-currents; then continue blowing and turning as before.
Absorption Bulbs or Washing Bulbs.—These are made by an elaboration of the processes given in the last paragraph, g, h, and i, Fig. 6, illustrate this.
A Thistle Funnel.—This is made by blowing a fairly thick-walled bulb on a glass tube, bursting a hole by heating and blowing, and enlarging the burst-out part by heating and rotating against a turn-pin.
Bending Glass Tube.—Small tubing may be bent in a flat flame gas burner and offers no special difficulty. Large or thin-walled tubing should be heated in the blowpipe flame and a slight bend made; another zone of the tube, just touching the first bend, should now be heated and another slight bend made. In this way it is possible to avoid flattening and a bend having any required angle can gradually be produced. A final shaping of the bend may be made by heating in a large blowpipe flame and expanding slightly by air pressure.
Glass Spirals.—If a tube is heated by means of a long, flat-flame burner, the softened tube may be wound on to an iron mandrel which has previously been covered with asbestos. The mandrel should be made slightly conical in order to facilitate withdrawal. It is desirable to heat the surface of the asbestos almost to redness by means of a second burner, and thus avoid undue chilling of the glass and the consequent production of internal strain.
Fig. 7
A Thermo-Regulator for Gas.—Fig. 7, a-e, shows an easily constructed thermo-regulator. The mercury reservoir, a, and the upper part, b, are made by joining two larger pieces of tubing on to the capillary. The gas inlet passes through a rubber stopper, in order to allow of adjustment for depth of insertion, and the bye-pass branches, d and e, are connected by a piece of rubber tubing which can be compressed by means of a screw clip, thus providing a means of regulating the bye-pass.
Use of Glass Rod.—Apart from its most common laboratory use for stirring; glass rod may be used in building up such articles as insulating feet for electrical apparatus or acid-resisting cages for chemical purposes. Such a cage is shown by f, g and h, Fig. 7. Further, by an elaboration of the method of making an exhaustion branch, given on page 18, blown articles may also be constructed from rod. Note the added parts of e, Fig. 9.
A Simple Foot.—The form of foot shown by Fig. 7, k, is easy to make and has many uses. First join a glass rod to a length of glass tubing as shown (the joint should be expanded slightly by blowing), cut off the tube and heat the piece remaining on the rod until it can be turned out as shown by i. This should be done with the large turn-pin, and care should be taken not to heat the supporting rod too strongly, otherwise the piece of tube will become bent and distorted; it is better to commence by heating the edge of the piece of tube and turn out a lip, then extend the heating by degrees and turn out more and more until the foot looks like that shown by i.
We now need to make three projections of glass rod. These are produced as follows:—Heat the end of the glass rod until a thoroughly melted mass of glass has accumulated (the rod must be rotated while this is being done, otherwise the glass will drop off); when sufficient melted glass has been obtained, the edge of the turned-out foot should be heated to dull redness over about one-third of its circumference, and the melted glass on the rod should be drawn along the heated portion until both are so completely in contact as to form one mass of semi-fluid glass. The rod should now be drawn away slowly, and, finally, separated by melting off, thus producing a flat projection. A repetition of the process will give the other two projections, and the finished foot may be adjusted to stand upright by heating the projections slightly and standing it on the carbon plate mentioned on page 7. After the foot is adjusted it should be annealed slightly by heating to just below the softening point of the glass and then rotating in a smoky gas flame until it is covered with a deposit of carbon, after which it should be allowed to cool in a place free from draughts and where the hot glass will not come in contact with anything. The finished foot is shown by k, Fig. 7.
Building up from Glass Rod.—A glass skeleton-work can be constructed from rod without much difficulty, and is sometimes useful as a container for a substance which has to be treated with acid, or for similar purposes. The method is almost sufficiently explained by the illustration in Fig. 7; f shows the initial stage, g the method of construction of the net-work, and h the finished container. It is convenient to introduce the substance at the stage indicated by g. The important points to observe in making this contrivance are that the glass rod must be kept hot by working while it is actually in the flame, and that the skeleton must be made as thin as possible with the avoidance of heavy masses of glass at any place. If these details are neglected it will be almost certain to crack.
Stirrers.—These are usually made from glass rod, and no special instructions are necessary for their construction, except that the glass should be in a thoroughly fused condition before making any joins and the finished join should be annealed slightly by covering with a deposit of soot, as explained on page 16. The flat ends shown in a, Fig. 8, are made by squeezing the soft glass rod between two pieces of carbon, and should be re-heated to dull redness after shaping. Fig. 8 also shows various forms of stirrer.
In order to carry out stirring operations in the presence of a gas or mixture of gases other than air, some form of gland or seal may be necessary where the stirrer passes through the bearing in which it runs. A flask to which is fitted a stirrer and gas seal is shown in section by b, Fig. 8. The liquid used in this seal may be mercury, petroleum, or any other that the experimental conditions indicate.
Fig. 8
If the bearing for a stirrer is made of glass tube, it is desirable to lubricate rather freely; otherwise heat will be produced by the friction of the stirrer and the tube will probably crack. Such lubrication may be supplied by turning out the top of the bearing tube and filling the turned-out portion with petroleum jelly mixed with a small quantity of finely ground or, better, colloidal graphite, and the bearing should also be lubricated with the same composition. Care should be taken not to employ so soft a lubricant or so large an excess as to cause it to run down the stirrer into the liquid which is being stirred.
Leading a Crack.—It sometimes happens that a large bulb or specially thin-walled tube has to be divided. In such a case it is scarcely practicable to use the method recommended for small tubes on page 12, but it is quite easy to lead a crack in any desired direction. A convenient starting point is a file cut; this is touched with hot glass until a crack is initiated. A small flame or a bead of hot glass is now used to heat the article at a point about a quarter of an inch from the end of the crack and in whatever direction it has to be led. The crack will now extend towards the source of heat, which should be moved farther away as the crack advances. In this manner a crack may be caused to take any desired path and can be led round a large bulb.
Cutting Glass with the Diamond.—Slips of window-glass can be used in place of glass rod for some purposes, and as cutting them involves the use of the glaziers' diamond or a wheel-cutter, they may well be mentioned under this heading.
In cutting a sheet of glass with the diamond, one needs a flat surface on which to rest the glass, and a rule against which to guide the diamond. The diamond should be held in an almost vertical position, and drawn over the surface of the glass with slight pressure. While this is being done the angle of the diamond should be changed by bringing the top of the handle forward until the sound changes from one of scratching to a clear singing note. When this happens the diamond is cutting. A few trials will teach the student the correct angle for the diamond with which he works, and the glass, if properly cut, will break easily. If the cut fails it is better to turn the glass over and make a corresponding cut on the other side rather than make any attempt to improve the original cut. The diamond is seldom used for cutting small glass tubes.
The use of the wheel-cutter calls for no special mention as it will cut at any angle, although the pressure required is somewhat greater than that needed by most diamonds.