Ground glass joint
Ground glass joints are used in laboratories to quickly and easily fit leak-tight apparatus together from commonly available parts. For example, a round bottom flask, Liebig condenser, and oil bubbler with ground glass joints may be rapidly fitted together to reflux a reaction mixture. This is a large improvement compared with older methods of custom-made glassware, which was time-consuming and expensive, or the use of less chemical resistant and heat resistant corks or rubber bungs and glass tubes as joints, which took time to prepare as well.
To connect the hollow inner spaces of the glassware components, ground glass joints are hollow on the inside and open at the ends, except for stoppers.
Crude versions of conically tapered ground glass joints have been made for quite a while, particularly for stoppers for glass bottles and retorts. These days, ground glass joints can be precisely ground to a reproducible taper or shape. They are made to join two glassware pieces together. One of the glassware items to be joined would have an inner (or male) joint with the ground glass surface facing outward and the other would have an outer (or female) joint of a correspondingly fitting taper with the ground glass surface facing inward.
Two general types of ground glass joints are fairly commonly used: joints which are slightly conically tapered and ball and socket joints (sometimes called spherical joints).
Conically tapered joints
The conically tapered ground glass joints typically have a 1:10 taper and are often labeled with a symbol consisting of a capital T overlaid on a capital S, meaning "Standard Taper". This symbol is followed by a number, a slash, and another number. The first number represents the outer diameter (OD) in millimeters (mm) at the widest point of the inner (male) joint. if possible - mark on picture The second number represents the ground glass length of the joint in millimeters. The most common US joints are 14/20 and 24/40. These sizes apply only to glassware in the US. There are also European ISO standard joints with common joint sizes of 5/13, 7/16, 10/19, 12/21, 14/23, 19/26, 24/29, 29/32, 34/35, 45/40, 60/46, 71/51 and 85/55. The US and ISO joints differ only in the length, not in the slope, and some can be used in combination. The stopper joints of chemical bottles, volumetric flasks, and separatory funnels often do not use the precision standard taper joints. Stopper joints are designated (if at all) only by the maximum diameter number.
- cones with cone tip
- cones with short cone tip
- cones with angle tip
- cones and sockets, full length with designations ST 5/20, 7/25, 10/30, 12/32, 14/35, 19/38, 24/40, 29/42, 34/45, 40/50 45/50, 50/50 and 55/50
- cones, full length, with cone tip
- tubes with socket and cone
For ball-and-socket joints (also known as spherical joints), the inner joint is a ball and the outer joint is a socket, both having holes leading to the interior of their respective tube ends, to which they are fused. The ball tip is a hemisphere with a ground-glass surface on the outside, which fits inside of the socket, where the ground glass surface is on the inside. Ball-and-socket joints are labeled with a size code consisting of a number, a slash, and another number. The first number represents the outer diameter in mm of the ball at its base or the inner diameter in millimeters at the tip of the socket, in both cases where the diameters are their maximum in the joints.
The second number represents the inner diameter of the hole in the middle of the ball or socket, which leads to the inner diameter of the tube fused to the joint.
If the angle standard taper fittings make with glassware is not perfectly set, the glass is extremely rigid and brittle, presenting a fracture risk on some setups. A ball and socket joining method allows some flexibility in the mating angles of the pieces being joined, which can be particularly important with heavy flasks or long pieces of glassware that would otherwise be difficult to support and potentially snap under bending loads. A common example of this is the collection flask on a rotary evaporator, whose weight increases significantly as it fills. A ball and socket allows the flask to plumb itself without placing a bending load on the joint. Such a socket might also be used on a larger, but more typical, distillation setup at the head and before the condenser. This allows the long span of the condenser, the non-perfect angle of the receiving bend and the filling flask to be supported more easily as their angle with the still head has a few degrees of positioning freedom.
They can also be found as the necks on pilot plant production flasks, where large volumes and masses are present, and on some Schlenk lines, where the long spans of fine glass benefit from a little flexibility between pieces. Generally, when considering smaller glassware, ball and sockets are far outnumbered by standard tapers.
Another type of glass joints uses an O-ring between the parts to form a leak-tight seal. Such joints are symmetric, with a tubular joint on each side having a widened tip with a concentric circular groove into which an elastomer O-ring can be inserted between the two joint pieces. O-ring joints are sized based on the inner diameter of the joint in millimeters. Since they can come apart rather easily, a clip or pinch clamp is needed to hold them together. The elastomer of the O-ring is more limited in high-temperature resistance than other types of glass joints using high-temperature grease.
Glass-to-metal transition joints
Occasionally, it may be desired to fuse a glassware item to a metal item with a tubular pathway between them. This requires the use of a glass-to-metal transition joint. Most glass used in laboratory glassware does not have the same coefficient of thermal expansion as metal, so fusing the usual type of glass with metal is likely to result in cracking of the glass. These special transition joints have several short sections of special types of glass fused together between the metal and the usual type of glass, each having more gradual changes in thermal expansion coefficients.
Round slightly spiral threaded connections are possible on tubular ends of glass items. Such glass threading can face the inside or the outside. In use, glass threading is screwed into or onto non-glass threaded material such as plastic. Glass vials typically have outer threaded glass openings onto which caps can be screwed on. Bottles and jars in which chemicals are sold, transported, and stored usually have threaded openings facing the outside and matching non-glass caps or lids.
Laboratory glassware, such as Buchner flasks and Liebig condensers, may have tubular glass tips serving as hose connectors with several ridged hose barbs around the diameter near the tip. This is so that the tips can have the end of a rubber or plastic tube mounted over them to connect the glassware to another system such as a vacuum, water supply, or drain. A special clip may be placed over the end of the flexible tube surrounding the connector tip to prevent the hose from slipping off the connector.
A number of brands, including Quickfit, have begun using threaded connections for hose barbs. This allows the barb to be unscrewed from the glassware, the hose pushed on and the setup screwed back together. This helps avoid accidentally breaking the glass and potentially doing serious harm to the chemist, as will sometimes occur when pushing the hoses directly onto the glass.
For either standard taper joints or ball-and-socket joints, inner and outer joints with the same numbers are made to fit together. When the joint sizes are different, ground glass adapters may be available (or made) to place in between to connect them. Special clips or pinch clamps may be placed around the joints to hold them in place.
Round-bottom flasks often have one or more conically tapered ground glass joint openings, or necks. Conventionally, these joints at the flask necks are outer joints. Other adapters, such as distillation heads and vacuum adapters, are made with joints that fit in with this convention. If a flask or other container has an extra outer ground-glass joint on it, which needs to be closed off for an experiment, there are often conically tapered inner ground-glass stoppers for that purpose. In some cases, small hook-like glass protrusions may be fused onto the rest of the glass item near a joint to allow an end loop of a small spring to be attached, so the spring helps keep joints temporarily together. The use of a special very small size of conically tapered fitting for glass, plastic, or metal parts called a Luer fitting or adapter has become more widespread. Originally, Luer fittings were used to connect the hub of a needle to a syringe. Where the use of ground glass presents a problem, as in the production or distillation of diazomethane (which may explode on contact with rougher surfaces), equipment with smooth glass joints may be used.
To prevent a joint from separating during a reaction process, various types of plastic or metal clips or springs can be used to secure the two sides together. They are available in a variety of materials for different temperature and chemical environments.
Patented in 1984 by Hermann Keck, plastic joint clips are usually made of polyacetal, and are colored according to joint sizes. Polyacetal melts at a reasonably low temperature (around 175 °C) and begins to soften around 140 °C. As glassware temperatures are recommended up to 250 °C, care needs to be taken that clips made from this material are not being used to hold glass together that will get this hot. Typical problem areas include a flask over the plate (which may drop off the end of the column as it gets hot) and the connection the condenser makes to the still head (which will reach high temperatures and may allow the condenser to fall off). As such, different clips should be used at these points or the glassware should be clamped such that these elements can't slide apart or don't need the clip. Polyacetal clips suffer another problem in that the material is strongly affected by corrosive gases. This effect can be so dramatic that the clip will fall apart in minutes of exposure to minute quantities leaking through even greased, ground tapers. Importantly, this failure mode is sudden and without warning.
PTFE joint clips are sometimes used, as its recommended temperature peak matches that of most practical chemistry work. Its highly inert nature also makes it immune to degradation around the corrosive gases. However, it is both expensive and will begin producing perfluoroisobutylene if heated to beyond its specified temperature; so care must be taken to avoid this, given the level of risk the result presents. The same is true of using Krytox and chemically resistant Molykote (PTFE thickened, fluoro based) oils and greases for glassware seals. High grade stainless steel joint clip is a final option. Naturally, this can withstand the entire temperature spectrum of borosilicate glass and is reasonably inert. Though, lower grades of stainless are still rapidly attacked in the presence of the corrosive gases and the clips themselves are often as expensive as PTFE.
Some glassware features barbs (Devil's horns / Viking helmet) sticking out the sides of the tapers. Small stainless steel springs are used on these to hold the joint together. The use of springs is of particular benefit when dealing with positive pressures, as they apply enough force for the glass to operate, but will open the taper if an unexpected excursion occurs. This method is considered quite old fashioned, but is still used on some of the most well known and high-end glassware available.
For situations where the simple spring action of metal wires or plastic is not strong enough or are not convenient for other reasons, screws can be used to hold joints together. Plastic collars are often used on microscale equipment. Metal clips with strong springs and screws to prevent release are used on larger joints that are subject to mechanical stress.
Extreme consideration must be taken when using clips on glassware that will generate a positive pressure, as it can be very easy for passages to block when using reactive gases and dip tubes. Hydrogen chloride, for example, has a vapour pressure at room temperature that is high enough to burst standard glassware. It is almost ubiquitously the case that only those joints that must be clipped should be clipped. It is safer to have an unclipped joint open and vent some of the corrosive gas than to have the same occur with the addition of the glassware exploding, emptying all of the contents and all of the gas out.
A thin layer of PTFE material or grease is usually applied to the ground-glass surfaces to be connected, and the inner joint is inserted into the outer joint such that the ground-glass surfaces of each are next to each other to make the connection. The use of this helps to provide a good seal and prevents the joint from seizing, allowing the parts to be disassembled easily. Although silicone grease used as a sealant and a lubricant for interconnecting ground glass joints is normally assumed to be chemically inert, some compounds have resulted from unintended reactions with silicones.
Sealing allows chemists to easily see when a taper is leaking, as bubbles can usually be seen flowing through the taper.
Both PTFE tape, bands, and fluoroether-based grease or oils, but not silicone-based, all emit perfluoroisobutylene fumes, as well as multiple other breakdown products, as they approach and exceed their working temperature limits (ca. 300C), which can occur when using a hotplate, mantle, oil bath or flame. Perfluoroisobutylene is about ten times as toxic as phosgene, upon contact with moisture (including tissue) rapidly converts to various reactive compounds including fluorophosgene, and requires immediate medical attention upon exposure.
Sometimes conical ground glass joints can lock together, preventing the user from rotating them - this is known as freezing or locking. Ball and socket-type joints are much less susceptible since they have more degrees of rotation than a conical joint. This may happen for a variety of reasons:
- Lack of lubrication between the two glass surfaces. If organic solvents come into contact with the joint, they can slowly dissolve the grease, leaving a dry glass-glass surface.
- Exposure to a strong base (hydroxide, phosphate, etc.) may dissolve some of the SiO2 surface, generating silicic acid (H4SiO4 / Si(OH)4)
- Solids from reaction mixtures
- Allowing sealed vessels to cool, which creates a pressure difference across the joint
Frozen joints may be removed by working solvent into the joint while rocking the stopper, heating the outer joint, or cooling the inner stopper. The last two methods employ the property of thermal expansion to create a small space between the two surfaces. There are also specialized glassblowing tools to unfreeze the joint.
- "Glassblower's Components: Joints and Stopcocks". East Carolina University.
- US patent 4442572, Hermann Keck, "Clip for fixing male and female parts of ground glass joints", issued 1984-04-17
- "Threaded Ground-glass Joint Tutorial". Sigma-Aldrich. Retrieved January 8, 2012.
- Haiduc, I., "Silicone Grease: A Serendipitous Reagent for the Synthesis of Exotic Molecular and Supramolecular Compounds", Organometallics 2004, volume 23, pp. 3-8. doi:10.1021/om034176w
- Lucian C. Pop and M. Saito (2015). "Serendipitous Reactions Involving a Silicone Grease". Coordination Chemistry Reviews. doi:10.1016/j.ccr.2015.07.005.
- Rob Toreki (2006-12-30). "Glassware Joints". Interactive Learning Paradigms Inc.
- Rob Toreki (2006-06-27). "Glassblowing". Interactive Learning Paradigms Inc.
- "Stuck/Frozen Glass Joints". East Carolina University.
A reflux set-up with conically tapered ground glass joints connecting the coil condenser with an adapter to allow inert gas (nitrogen or argon) to leave the vessel (top) and two-necked flask. Another ground glass joint connects the second neck to another adapter for introduction of an inert gas.