LABORATORY TECHNIQUES

BALANCES ELECTRONIC BALANCES are generally more precise and give a digital reading. Because of their sensitivity and cost, extreme care is needed to maintain the instruments. NEVER PLACE CHEMICALS DIRECTLY ON THE BALANCE. The procedure for proper use follows: 1. Be sure the balance is level and clean. Report any chemical spills to the instructor. 2. Turn the balance on and allow it to adjust to zero. 3. Check the capacity of the balance. The capacity is the maximum mass the balance can support. Do not exceed the balance capacity. 4. Place the weighing paper or boat on the balance. Record the mass. Alternatively, the tare button can be pushed. This will subtract the weight of the weighing paper or boat from the balance. 5. Transfer small amount of the chemical by gently tapping the spatula. Add the chemical to the weighing paper or boat until it reads the desired mass. 6. Remove the chemical and push the tare button.

Figure 1

HANDLING SOLIDS 1. Solids are usually kept in wide-mouthed bottles. During the transfer of solid, either hold the reagent bottle cover in your fingers, or lay it on the bench top with the top side down to prevent contamination, as shown in Figure 2a. 2. Pour solids by gently tipping the reagent bottle whole slowly rotating it back and forth, as shown in Figure 2a. Just tipping the bottle may cause large lumps of the reagent to drop suddenly into your container possibly causing a spill. 3. Use spatula only to transfer solids from your container, as shown in Figure 2b. Do not put your spatula into a reagent bottle.

Figure 2

4. Return the original cover to the reagent bottle. Interchanging covers of reagent bottles may cause contamination. Do not return unused solids to their reagent bottles; this can cause contamination. TRANSFERRING TO A TEST TUBE: Hold the creased weighing paper or boat over the test tube opening and slowly pour the chemical into a test tube. (Figure 3) Figure 3

USING A MORTAR AND PESTLE 1. A mortar and pestle should be used for grinding only one substance at a time. 2. Never use a mortar and pestle for simultaneously mixing different substances. 3. Place the substance to be broken up into the mortar. 4. Pound the substance with the pestle and grind to pulverize. 5. Remove the powdered substance with spatula.

Figure 4

HANDLING LIQUIDS DROPPING BOTTLE: Most of the chemicals we will be using are dispensed from dropping bottles. Be sure the top is on tightly before inverting the bottle. Dispense the liquid slowly until the desired amount is obtained. BERAL PIPETS: To use a Beral or Pasteur pipet to transfer liquid, first squeeze the bulb to expel air. Still squeezing the bulb, place the tip of the pipet well below the surface of the liquid and keep it there to avoid drawing air into the pipet. Release the pressure on the bulb slowly to draw liquid into the pipet. Position the pipet tip over the appropriate well in the well plate and squeeze the bulb to release the liquid into the well. Store Beral pipets bulb side down. PIPET: Attach a pipet pump to the appropriate size pipet. Be sure you are familiar with the proper use of the pump before you use it. Draw the liquid into the pipet to the desired volume. Remove the pipet from the liquid and dispense the liquid into the appropriate container. (Figure 5) BURET: Figure 6 shows the proper setup for a buret, used for measuring liquid. TRANSFERRING LIQUID TO A TEST TUBE: When you are transferring a liquid to a test tube or measuring cylinder, the container should be held at eye level. The safest way to transfer a liquid from a graduated cylinder to a test tube is shown in Figure 7. Figure 5 Figure 6 The liquid is transferred at arms length with the elbows slightly bent. This position enables you to see what you are doing and still maintain steady control. Figure 7

TRANSFERRING FROM A STOPPERED BOTTLE: When you are pouring a liquid from a reagent bottle into a beaker, the reagent should be poured slowly down a glass-stirring rod (Figure 8a). When you are transferring a liquid from one beaker to another, you can hold the stirring rod and beaker with one hand (Figure 8b).

Figure 8 a Figure 8 b

FILTERING LIQUIDS: Insoluble solids can be removed from a liquid by filtration. 1. Fold a filter paper circle in half and then quarters. Open the folded paper to form a cone with one thickness of paper on one side and three thicknesses on the other (Figure 9).

Figure 9 2. Put the paper cone in a filter funnel. Place the funnel in an iron ring clamped to a ring stand. Moisten the filter paper with a small volume of water, and gently press the paper against the sides of the funnel to give a good fit. (If the correct size of filter paper has been used, the top edge of the cone will be just below the rim of the filter funnel.) 3. Place a beaker beneath the funnel to collect the filtrate. The tip of the funnel should touch the inside surface of the beaker and extend about an inch below the rim. 4. Decant the liquid from the solid (precipitate) by pouring it down a glassstirring rod into the funnel (Figure 10a). Be careful to keep the liquid below the top edge of the cone of the filter paper at all times; the liquid must not overflow. 5. Use a glass rod with an attached rubber policeman to scrape the precipitate from the beaker into the funnel, as shown in Figure 10b. 6. Finally, use a jet of distilled water from a wash bottle to wash the solid (precipitate) into the filter. (Figure 10c) 3

7. When the filtration is complete, wash the solid residue on the filter paper with distilled water to remove traces of solvent. Dry the solid.

Figure 10

MEASURING LIQUIDS: 1. For approximate measurements of liquids, a graduated cylinder is generally used. A pipet or a buret is used for more accurate volume measurements. Pipets are made in many sizes and are used to deliver measured volumes of liquids. A pipet is fitted with a suction or pipet pump used to withdraw air from the pipet while drawing up the liquid to be measured. 2. Since most of the liquids that will be used in the experiments wet the sides of their containers, this property must be taken into account in reading the instrument. Notice that the surface of a liquid is slightly curved, which is called the meniscus. Locate the bottom of the meniscus and read the liquid level. Figure 11 shows the proper way to read a concave meniscus.

Figure 11

USING A GAS BURNER BUNSEN BURNER: A typical Bunsen burner is shown in Figure 12a. The combustible gas flows through a piece of rubber tubing from a gas cock on the laboratory bench to the gas inlet of the burner. Gas passing up the burner barrel mixes with air drawn into the barrel through the air inlets. The gas-air mixture is ignited by holding a burning match just above the top of the barrel (Figure 12 b). The quality of the flame depends on the mixture of air and gas.

Figure 12

Use the following procedure when lighting and using your burner. 1. Be sure your lab area is clear of any combustible materials and flammable liquids. 2. Be sure long hair is tied back. Wear chemical splash goggles and an apron. 3. Be sure your burner is firmly inserted in the gas jet. Do not light the burner if you can detect the odor of gas prior to opening the gas valve. 4. Open the air inlet or collar slowly to admit more air into the barrel. Hold a flint igniter over the top of the burner and turn on the gas. Strike the flint lighter. CAUTION: Shut the gas off at the gas inlet if the burner does not light or if the gas begins to burn inside the barrel. 5. A mixture that is mostly gas with only a little air produces a relatively cool yellow flame, referred to as a reducing or luminous flame (Figure 13 a). Open the air inlet or collar until the flame turns entirely blue with two cones as depicted in Figure 13 b. Turn off your gas burner when finished.

Figure 13

air inlet closed

air inlet open

HEATING LIQUIDS Figure 14 HEATING LIQUIDS IN A TEST TUBE. 1. Check to see that the test tube is heatresistant. 2. Always use a test tube holder or clamp when heating a test tube. 3. Never point a heated test tube at anyone, because the liquid may splash out of the test tube. 4. Never look down into the test tube when heating it. 5. Heat the test tube from the upper portions of the tube downward and continuously move the test tube as shown in Figure 14. Do not heat any one spot on the test tube. Otherwise a pressure build-up may cause the bottom of the tube to blow out. HEATING HOT-WATER BATH

A LIQUID IN A

Figure 15

EVAPORATING SOLUTIONS 1. Figure 16a shows the proper setup for evaporating a solution over a water bath. 2. Figure 16b shows the proper setup for evaporating a solution in a porcelainevaporating dish with a watch glass cover that prevents spattering. 3. Glassware, porcelain and iron rings that have been heated may look cool after they are removed from a heat source, but these items can still burn your skin even after several minutes of cooling. Use tongs, test tube holders, or heat resistant mitts and pads whenever you handle this apparatus. 4. You can test the temperature of the questionable apparatus that had been heated by holding the back of your hand close to their surfaces before grasping them. You will be able to feel any heat generated from the hot 6

surfaces. DO NOT TOUCH THE APPARATUS. Allow plenty of time for the Figure 16a Figure 16b

apparatus to cool before handling. HEATING SOLIDS 1. Porcelain crucibles are commonly used for heating solids to thermally decompose them or to heat them to dryness. Generally, the crucible is first heated to constant mass to drive off any moisture. This way, there is no change in the crucibles mass when it is heated along with the sample. After the crucible is heated to constant mass and cooled, put the solid to be heated into the crucible. 2. To heat the sample so that it does not react with atmospheric oxygen, insert the covered crucible upright in the clay triangle, with the cover on straight as shown in Figure 17a. If the heated solid is to react with atmospheric oxygen, tilt the crucible slightly in the clay triangle and use crucible tongs to position the cover so it is slightly ajar (Figure 17b). Figure 17

DETECTING ODORS SAFELY 1. Test for the odor of gases by wafting your hand over the test tube and cautiously sniffing the fumes as shown in Figure 18. 2. Do not inhale any fumes directly.

Figure 18

3. Use a fume hood whenever poisonous or irritating fumes are evolved. DO NOT waft and sniff poisonous or irritating vapor.

THERMOMETERS 1. Store in an upright position to prevent separation of fluid. 2. Do not stick thermometer directly in a flame or on a hot plate. 3. Remove the plastic cap on the end if present. 4. Thermometers should be placed in the center of the substance that you are measuring. GLASSWARE 1. Use the specific type and smallest size possible to increase your accuracy. In general the precision of the instrument decreases as the size increases. 2. Do not cross contaminate chemicals a. Use one piece of glassware per chemical b. Use soap and water and rinse thoroughly before using another chemical 3. Use only the glassware detergent on the glassware this prevents buildup that may mess up future labs. 4. Rinse all glassware thoroughly and hang on pegs or set in dish drainer to dry.