Name: AP Chemistry: Laboratory Techniques Objective Familiarity with the various instruments used for making physical measurements in the laboratory is essential to the study of experimental chemistry. In this experiment, you will investigate the uses and limits of the various types of laboratory balances and volumetric glassware. Part I: The Laboratory Balance and Mass Determinations Mass is a direct measure of the amount of matter in a sample of substance, that is, a direct indication of the number of atoms or molecules the sample contains. There are various types of balances available in the typical chemistry laboratory. Such balances differ in their construction, appearance, operation, and in the level of precision they permit in mass determinations. Simple rules to follow when using a balance: Never put chemicals directly on the pan – always use a weigh boat, weigh paper or glass vessel. Immediately clean up spills on the metal or scale Never put hot objects on the balance Always make sure that the balance gives a reading of 0 grams when nothing is present on the pan. Adjust the tare / zero knob if necessary. Balances can be damaged by moisture. Be careful with liquids used around the scale. The digital electronic balance gives the mass directly when an object is placed on the pan. This balance reads to 2 decimal places, and has a 200-gram capacity. This balance reads to 1 decimal place, and has a 400-gram capacity. Procedures in a laboratory exercise are generally written in such terms as “weigh 0.5 grams of substance…to the nearest milligram.” This does not mean that exactly 0.500 gram of substance is needed. Rather, the statement means to obtain an amount between 0.450 and 0.550 gram. Unless a procedure states explicitly to weigh out an exact amount, you should not waste time trying to obtain an exact amount. However, always record the amount actually taken to the precision of the balance used. For accurate mass determinations, the object to be weighed must be at room temperature. If a hot or warm object is placed on the pan of the balance, the air around it becomes heated. Warm air rises, and the motion of the air might be detected by the balance, giving masses that are significantly less than the true value. Procedure 1: Using Laboratory Balances Materials: small rubber stopper, large rubber stopper, small beaker, balance, weigh paper Directions: Examine the different types of balances provided in the laboratory. Determine the mass of a small beaker that can accommodate the objects whose masses are to be determined. Transfer one of the 1 objects to the beaker. Determine and record the combined mass; determine the mass of the object by the subtraction method. Then determine and record the mass of the object by itself in the accepted value section. Repeat this procedure with the other balances. (The average mass will be the accepted value) Mass of beaker Mass of beaker + stopper DATA TABLE: Massing the small stopper Mass of stopper Mass of (by subtraction) stopper Show work (by weighing) (accepted value) % error (show work) Electronic balance (hundredths) Electronic balance (tenths) Mass of large rubber stopper Mass of beaker + stopper DATA TABLE: Massing the large stopper Mass of stopper Mass of stopper (by subtraction) (by weighing) Show work (accepted value) % error (show work) Electronic balance (hundredths) Electronic balance (tenths) Part II: The Use of Volumetric Glassware This experiment makes use of several types of volumetric glassware, specialized pieces of glassware which are used to measure volumes of liquids very precisely in quantitative laboratory work. Examples of these types of glassware include graduated cylinders, burettes, pipets, and volumetric flasks. These are carefully manufactured and expensive items and should be treated with great care. Ordinary beakers and flasks are not used for accurate volume measurements; the markings on these pieces of glassware are generally only accurate to within 5% 2 Volumetric glassware is usually marked with its total volume, the notation “TD” or “TC”, and a temperature (usually 20°C). The marked temperature indicates the temperature at which the apparatus was calibrated. Since density and volume change with temperature, the volume markings are strictly correct only at the calibration temperature. The notations TD and TC stand for the phrases "to deliver" and "to contain." The TD notation, used on burettes and pipets (and some graduated cylinders), means that the apparatus is calibrated to accurately deliver or transfer the stated volume to another container. The TC notation, used on volumetric flasks and (most) graduated cylinders, means that the markings give an accurate measure of the volume contained, but that pouring the liquid into another container will not necessarily deliver the indicated volume. Procedure 2: The Use of Volumetric Glassware A. Graduated Cylinders The most common apparatus for routine determination of liquid volumes is the graduated cylinder. Although this instrument does not permit as precise a determination of volume as do other devices, it is sufficient for use in the lab. A plastic safety ring is often used to protect the cylinder if it is knocked over. 1. Determine the smallest graduation of volume that can be measured with each cylinder. You should read the instrument to one more decimal place to the right than the smallest graduation mark. This last number will be an estimation on your part. 2. Read the bottom of the meniscus for water and aqueous solutions. 3. Greater precision is possible with smaller cylinders and more divisions. 4. Read at eye level. 5. What do the following graduated cylinders read? A._______ B._________ C. ________ Answers: A: Each of the smaller lines represents 1 mL. The reading will be one place to the right of the decimal. The bottom of the curve is about halfway between the 16 and the 17, so the reading on this graduated cylinder would be 16.5 mL. B: Each line represents 0.1 mL. The reading will be two places to the right of the decimal. The bottom of the curve looks like it is exactly on the line that would represent 3.8. Because it is exactly on the line, the reading would be 3.80 mL. C: The bottom number is 6 and the top number is 8. If each mark is 0.2, the measurement is halfway between 7.4 and 7.6 – which is 7.5. Because each line is equal to 0.2, the measurement will be 2 places past the decimal. The correct way to report this measurement is 7.50 mL. 3 Directions: For each graduated cylinder, determine the smallest graduation mark. Use that graduation mark to correctly measure the volume of the liquid. Data Table: Graduated Cylinders Water Color GREEN Maximum value of graduated cylinder. Smallest graduation mark Volume of liquid BLUE RED B. Pipettes When a more precise determination of liquid volume is needed than can be provided by a graduated cylinder, a transfer pipette may be used. The Mohr pipette is graduated so as to allow the dispensing of varied volumes. The volumetric transfer pipette is made is dispense one fixed volume with high accuracy. Small plastic pipettes may or may not be calibrated; it might be necessary to count the drops to determine the volume of one milliliter. When using a pipette, a pipette filler or a rubber bulb can supply the suction needed to fill the pipette. Never pipette my mouth. Roll the knob up on the pipette to apply suction force. Allow the liquid to be drawn above the calibration mark on the barrel. At this point, release liquid until it reaches the mark. Then, quickly place the pipette filler over a vessel and dispense the measured liquid. Touch the tip of the pipette to the side of the flask to remove the last drop of liquid. Materials: 50mL beaker, plastic pipette, graduated pipette, volumetric pipette, pipette filler, thermometer Directions: 1. Ensure that the graduated and volumetric pipette is clean. Rinse with water. An ultra-clean pipette will not bead up anywhere inside the barrel. 2. If measuring a substance other than water, to prevent dilution of the solution, always rinse the pipette with several small portions of the solution. 3. Practice using each pipette until you feel comfortable with the technique. 4. Starting with the graduated pipette, fill with water close to but under the zero mark. Record the pipette reading in the data table with the proper number of digits (look at the graduation marks!) under pipette volume. 5. Using your balance, tare (zero) a clean, dry 50mL beaker. 6. Empty the contents into the beaker. Record the mass of the water. 7. Obtain the temperature of the water. Record. 8. Using the Density of water table, record the density of the water at that temperature 9. Calculate the volume using the density and mass. 10. Compare the volume to the volume of the pipet as specified by the manufacture. Any significant difference between these two volumes in an indication that you need additional practice in pipetting. 11. Calculate percent error – assume the calculated volume is the actual volume. 12. Repeat the procedure with the remaining pipettes. 4 DATA TABLE: PIPETTES Pipette Initial reading Volume of water dispensed Mass of water Water temp Water Density Calculated volume (show work) % Error (Show work) Calculated volume (show work) % Error (Show work) (10–initial) Graduated pipette Pipette volume Mass of water Water temp Water Density volumetric pipette Plastic pipette C. Burettes When samples of various sizes must be dispensed or measured precisely, a buret may be used. The buret consists of a tall, narrow calibrated glass tube, fitted at the bottom with a valve (called a stopcock) for controlling the flow of the liquid. Buret must be scrupulously clean before use; precision permitted is 0.02mL, but if not completely clean, this level of precision is not attainable. Rinse with tap water, followed by distilled water. Buret does not have to be filled to the 0.00 mark; fill to a level that is comfortable using a small buret funnel. Readings should be made to the 0.02mL; volume of liquid dispensed is obtained by subtraction of the two volume readings. The glass tip of the buret should touch the flask or beaker so that the last drop is accounted for. Materials: Burette, Burette Clamp, Ring stand, Flask, 100mL beaker, thermometer Directions: 1. Obtain a burette and set it up in a clamp on your lab bench as shown. 2. Ensure that the burette is clean using the information given above. 3. Fill the burette to above the zero mark. Examine the burette while the water is running from it. If the burette is clean enough for use, water will flow down the inside of the burette without beading up anywhere. If the burette is not clean, clean again or replace. 5 4. Refill the burette with distilled water to a point somewhere below the zero mark. Record the precise level to the nearest 0.02 mL. 5. Obtain a clean and dry 100mL beaker. Mass the beaker. 6. Place the weighed beaker under the burette. Open the stopcock of the burette and run water into the beaker until approximately 25 mL of water has been dispensed. Determine the precise liquid level in the burette to the nearest 0.02mL and record. 7. Mass the beaker and the water dispensed. 8. Calculate the volume of water that has been dispensed from the burette by subtraction. 9. Take the temperature of the water. Record 10. Determine the density of the water using the chart provided. 11. Calculate the percent error (assuming the calculated volume is the actual volume) BURETTE DATA TABLE Initial Volume Reading Mass of beaker Final Volume reading Mass of beaker and water Volume of water dispensed (show work) Mass of water dispensed. (show work) Temperature of the water Density of the water Calculated volume of the water (show work) Percent Error (show work) D. Funnels Filtration is performed by inserting a paper filter into a glass (or plastic) funnel. Write your period and group number on the filter paper. Weigh and record the mass of the filter paper. The paper must be folded in half twice to form a cone, which is then inserted into the funnel. The paper filter is then moistened with distilled water using a wash bottle. Materials: Beaker, Buchner funnel, filtering flask, stir rod, filter paper, sand, rubber spatula, wash bottle 6 Directions: 1. Weigh and record the value of approximately 5 grams of sand. 2. Make a mixture by adding approximately 25 mL of tap water to the 5 grams of sand into a beaker 3. Mix with a glass stirring rod, and while the mixture is in motion, filter the sand as demonstrated by the teacher. Be sure to remove all the sand from the beaker with the wash bottle. 4. Allow the filter paper (with the sand) to dry overnight. 5. Mass the sand and calculate the percent error. DATA TABLE FUNNEL Mass of Sand before filtration Mass of Sand after filtration Percent error (show work) LABORATORY QUESTION 1. Pipets used for the transfer of samples of solutions are always rinsed with a small portion of the solution before the actual sample is taken. Calculate the percent error likely to arise in an experiment if 1-mL, 5mL, and 10-mL pipets are used for transfer and each pipet contains 5 drops of water adhering to the inside of the barrel. A single drop of water has a volume of approximately 0.05 mL. Show all work; box answers. 7 8