GLASSWARE APPARATUS WITH INTERCHANGEABLE GROUND GLASS JOINTS LABORATORY GLASSWARE basic glossary (on pictures):

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1 Zajęcia dokształcające z języka angielskiego w chemii nr. 4 Zajęcia mają na celu pracę z tekstami dotyczącego nazewnictwa aparatury szklanej - LABORATORY GLASSWARE (przykładowe teksty poniżej). GLASSWARE APPARATUS WITH INTERCHANGEABLE GROUND GLASS JOINTS LABORATORY GLASSWARE basic glossary (on pictures): GLASSWARE (Vogel s Textbook of practical Organic Chemistry 5 th edition p. 30) Glass apparatus should be carefully examined before use and any which is cracked, chipped, flawed or dirty should be rejected. Minute cracks in glassware for use in evacuated systems are particularly dangerous. Many apparently simple manipulations such as the cutting of glass tubing or rod, the insertion of glass tubing or thermometers into rubber bungs or bark corks, or the removal of tight stoppers from bottles, can lead to serious cuts. Care should be taken to adopt the correct procedures (Sections 2.9 and 2.10). All apparatus and clean glassware not in use should be stored away and not allowed to accumulate on benches. Glossary: Glass apparatus aparatura szklana cracked stuknięty, zbity, pęknięty chipped - wyszczerbiony flawed wadliwy, ze skazą minute cracks minimalne, drobne zarysowania in evacuated systems w układach, zestawach pod próżnią cutting of glass cięcie szkła

2 thermometer termometr rubber guma bark kora cork korek tight stoppers from bottles dopasowany korek, zatyczka fabryczny np. na butelce. benches stoły laboratoryjne APPARATUS WITH INTERCHANGEABLE GROUND GLASS JOINTS (Vogel s Textbook of practical Organic Chemistry 5 th edition p. 30) In considering the following typical standard units of equipment fitted with ground glass joints, it must be borne in mind that while a particular piece of glass equipment of certain capacity or dimensions may be fitted with alternative joint sizes, the range is usually restricted in relation to their relative proportions. When equipping a laboratory, it is usually convenient to limit the range of socket sizes thus permitting interchangeability with the minimum number of adapters. For example, with Quickfit, 14/23, 19/26, 24/29 and 34/35 joints are suitable for macro scale experiments, and 10/19 and 14/23 for semimicro scale experiments; a similar selection would be appropriate from the USA coded sizes. In Fig. 2.8(a)-(d), the various designs of flasks are collected. Type (a) is a pearshaped flask, the capacity range being usually 5 m1 to 100ml, the joint sizes are in the range 10/19 to 24/29. Type (b) is a round-bottomed flask (short-necked), the capacity range being 5ml to 10 litres, joint sizes being in proportion; medium- and long-necked designs are also available. Type (c) illustrates a range of wide-necked reaction flasks which are useful in semimicro and in pilot scale experiments and which are fitted with large diameter flat-flange joints, the capacities range from 250 ml to 20 litres, the flange bore being 75 mm to 100mm respectively; the multi-socket lids are illustrated in Fig. 2.18(a) and (b). The advantages of this type of reaction vessel are that (i) the lids are easily detachable, (ii) large stirrers are readily accommodated, (iii) the vessels are cleaned readily and (iv) the removal or addition of solids and viscous fluids is facilitated; the ground flange joints are fully interchangeable.

3 Special clamps are available for the support of such flasks. Type (d) of Fig. 2.8 is a jacketed flange flask which is ideally suited for reactions requiring accurate temperature control. Various types of multi-necked round-bottomed flasks are illustrated in Fig. 2.9(a)-(d); designs with pear-shaped flasks are available. The centre socket is usually the larger and the side sockets are generally smaller; type (d) shows the side socket being employed for the insertion of a capillary tube necessary in a vacuum distillation assembly (see Section 2.27). Ground glass stoppers of all standard sizes are available and may be of the design shown in Fig. 2.10; the flat head is preferred since the stopper may be stood on end when not in use, thus avoiding contamination of the ground surface; an additional refinement is the provision of a finger grip.

4 Often in the assembly of apparatus, joint adapters are required if the joint sizes of the various parts are not compatible. A reduction adapter is illustrated in Fig and an expansion adapter in Fig. 2.12; numerous combinations are of course possible, but it must be emphasised, however, that in a well-designed assembly of apparatus the number of adapters should be reduced to a minimum and, best of all, completely eliminated. Distillation heads (or still-heads) are shown in Fig (a)-(c). Type (a) is a bend ('knee-tube') which is frequently employed for those distillations which merely require the removal of solvent. Type (b) is a simple distillation head; when fitted into a flask with a ground glass socket, the assembly is virtually a distillation flask. For some purposes, a thermometer may be fitted into a one hole rubber stopper of correct taper and then inserted into the socket; the area of rubber which is exposed to the organic vapour is relatively so small that the amount of contamination thus introduced is negligible. If, however, all rubber stoppers must be absent because of the highly corrosive nature of the vapour, a thermometer fitted with an appropriate size cone is employed. Alternatively the socket of a distillation head may be fitted with a screw-capped adapter (see Fig. 2.32) through which a thermometer may be inserted. Type (c) is a Claisen distillation head; the left-hand socket accommodates the capillary tube for use in distillations under vacuum (see Section 2.27) and the right-hand socket a suitable thermometer. Frequently for semimicro and micro work it is more convenient to use the pearshaped flask designs which incorporate the distillation heads (e.g. Fig. 2.14(a) and (b). Multiple adapters provide for additional entries into a single-necked flask when a multinecked flask is not available. Either double-necked or triplenecked adapters (Fig and Fig. 2.16(a) and (b) are commonly used having a range of socket and cone sizes. The 'swanneck adapter' of Fig is useful for vacuum distillations as it permits the insertion of a capillary tube through the screw thread joint. This joint may also be used for insertion of a thermometer or a gas inlet in the narrow neck and a reflux condenser into the ground joint; this device virtually converts a three-necked flask into a four-necked flask.

5 Multiple socket lids for fitment to the flange flasks (illustrated in Fig. 2.8(c)) are shown in Fig. 2.18(a) and (b). These allow for the introduction of a great variety of standard equipment for stirring, temperature measurement, the inlet of gas, etc. The sockets may be vertical or angled at 5, 10 or 15 degrees from the vertical axis. Several types of condensers are widely used (Figs ). An improved form of Liebig's condenser, sometimes termed a West condenser, is shown in Fig. 2.19; it has an inner tube with very thin walls and the space between it and the heavy-walled outer tube is small, consequently there is a rapid heat transfer to the fast-flowing cooling water leading to greater efficiency. The length of the jacket is usually 6 to 50 cm and the design is available in a range of joint sizes. Figure 2.20 (Davies type) and Fig (double coil type) are examples of efficient double surface condensers. Figure 2.22 depicts a 'screw' type of condenser (Friedrich pattern); this highly efficient condenser is employed for both reflux and downward distillation. The ice or dry iceacetone condenser (Fig. 2.23) is useful for volatile liquids. The water inlet and outlet sidearms on the condensers illustrated are of the standard olive all-glass type. Breakage can easily occur, often resulting in serious hand injury, when attaching or detaching rubber or plastic

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7 water hoses. A recent design (Bibby Science Products) incorporates a screw-thread at sidearm ends on to which a plastic hose connector may be screwed to give a watertight seal. Not only is this safer in the hands of less experienced workers, but it allows for more rapid apparatus assembly. Various forms of receiver adapters or connectors for attachment to the end of condensers when used in a distillation assembly are shown in Figs The simplest form (Fig. 2.24) carries glass hooks for securing it to the condenser by means of a rubber band from the side tube to the hook; an improved form, incorporating two glass joints, is shown in Fig A useful adapter is illustrated in Fig. 2.26; when employed at atmospheric pressure, a drying tube may be attached to the side tube, if desired; in a distillation under reduced pressure, the side tube is connected to a vacuum pump. Cone/ rubber tubing adapters ('take-of adapters), shown in Fig. 2.27(a) and (b), fulfil a number of useful purposes in preparative organic operations, for example where very small volumes of solvents need to be rapidly removed. A calcium chloride guard-tube is illustrated in Fig which is widely used for protecting apparatus assemblies from the ingress of moisture. For many operations the globular form of dropping, addition or separatory funnel having a suitable cone joint fitted to the stem is convenient, but when required on either a multiplenecked flask or with a multiple adapter, the cylindrical design (Fig. 2.29) is preferred; this is similarly provided with a cone on the stem and a ground socket. Figure 2.30 illustrates a cylindrical funnel with pressure-equalising tube; this is invaluable for reactions which are conducted in an atmosphere of inert gas. Either funnel may be fitted with an all-glass or a

8 Rotaflo stopcock; the latter gives excellent liquid flow control. Jacketed dropping funnels for use with ice-water or dry ice-acetone slurry coolants are available and are useful when reagents to be added to a reaction mixture need to be kept at low temperatures. Dropping funnels are also available with a design of stopcock which allows infinite control of the rate of addition. The two designs of the Dean and Stark apparatus (Fig. 2.31(a) and (b); available from Bibby Science Products) carry a flask on the lower cone and a reflux condenser on the upper socket. They are used for the automatic separation of two immiscible components in a distillate and the subsequent return of the upper layer (a) or the lower layer (b) to the reaction flask. Glossary: ground glass joints połączenia na szlif glass equipment wyposażenie szklane capacity - przepustowość dimensions rozmiary joint sizes rozmiary szlifów (od np. korków łączników) socket sizes - rozmiary szlifów (od np. kolb) interchangeability zamienność, wymienność adapters łączniki, nasadki flasks kolby pearshaped flask kolba gruszkowa round-bottomed flask kolba okrągłodenna short-necked - krótkoszyjna long-necked z długą szyją wide-necked reaction flasks kolby reakcyjne z szeroką szyją large diameter flat-flange joints łączniki na płaski kołnierz o dużej średnicy flange bore średnica otworu kołnierza multi-socket lids pokrywy z wieloma wejściami (otworami) detachable - zdejmowalny, odłączalny stirrer mieszadło accommodated zamontowane, przystosowane vessel naczynie

9 solid ciało stałe viscous fluids lepkie ciecze clamp łapy accurate temperature control dokładna, ścisła kontrola temperatury multi-necked wieloszyjne centre socket środkowe wejście, otwór side sockets boczne wejścia capillary tube kapilara vacuum distillation destylacja pod próżnią ground glass stoppers korki na szlif design projekt (w sensie wyglądu) ground surface powierzchnia szlifu provision zabezpieczenie assembly of apparatus zestaw aparaturowy reduction adapter reduktor (z większej średnicy na mniejszą) expansion adapter ekspander (z mniejszej średnicy na większą) distillation heads nasadki destylacyjne bend zginać solvent rozpuszczalnik distillation flask kolba destylacyjna thermometer termometr organic vapour - opary organiczne corrosive powodujący korozję screw-capped adapter nasadka z nagwintowaną nakrętką swan-neck adapter nasadka z tzw. łabędzią szyją screw thread joint nagwintowana szyja nasadki gas inlet wlot gazu reflux condenser chłodnica zwrotna vertical or angled pionowe lub pod kątem inner tube wewnętrzna rurka

10 heavy-walled outer tube grubościenna rura zewnętrzna rapid heat transfer szybkie przekazywanie ciepła fast-flowing cooling water - szybko-przepływająca woda chłodząca length of the jacket - długość płaszcza chłodzącego 'screw' type of condenser chłodnica śrubowa ice or dry ice-acetone condenser chłodnica chłodzona lodem lub mieszaniną suchego lodu z acetonem volatile liquids - ciecze lotne injury ciężkie obrażenia water hoses węże od chłodnic receiver adapters - nasadki odbieralnikowe connectors łączniki glass hooks szklane haczyki atmospheric pressure ciśnienie atmosferyczne drying tube rurka ze środkiem suszącym reduced pressure obniżone ciśnienie vacuum pump pompa próżniowa cone/rubber tubing adapters - nasadki typu stożek-rurka gumowa calcium chloride guard-tube rurka z chlorkiem wapnia moisture wilgoć dropping funnel wkraplacz separatory funnel rozdzielacz with a cone on the stem and a ground socket posiadający na nóżce szlifowaną tulejkę cylindrical funnel wkraplacz cylindryczny atmosphere of inert gas atmosfera gazu obojętnego all-glass or a Rotaflo stopcock kran szklany lub typu Rotaflo jacketed dropping funnels wkraplacze z płaszczem coolants mieszaniny chłodzące reaction mixture mieszanina reakcyjna Dean and Stark apparatus aparat Dean a -Stark a immiscible components - składniki niemieszalne ze sobą upper/ lower layer górna/dolna warstwa

11 Laboratory glassware basic glossary (on pictures): Beaker Erlenmeyer Flask Three-Neck Round-Bottom Flask Round-Bottom Flasks Reducing Adapter Buchner funnels Claisen Adapters Vacuum-Distilling Adapter 105 degree bent adapter Straight Connecting Adapters Three-Way Adapters

12 Four-Neck Angled Round-Bottom Flask Three-Neck Vertical Round-Bottom Flask Three-Neck Angled Round-Bottom Flask Two-neck Angled Round-Bottom Flask Two-neck Vertical Round-Bottom Flask Round-Bottom Flask with Septum Inlet Round Flat-Bottom Flasks

13 Condensers Allihn Liebig Grahams West Thermometer Separatory Funnels Dropping Funnels Crucibles Bunsen Burner Meker Bunsen Burner Tripod Stand

14 Funnel Powder Funnel Pestle Mortar 0 Volumetric Flasks Funnels Burette Holder Burette 5 0 Support Stand Trap Filtering Flasks

15 vacuum desiccator

16 Ćwiczenie. Nazwij poszczególne elementy wyposażenia laboratoryjnego: