Name Class Period LABORATORY PROCEDURES – Lab Safety and Techniques The best way to become familiar with chemical apparatus is to actually handle the pieces yourself in the laboratory. This experiment is divided into several parts in which you will learn how to adjust the gas burner, use a balance, handle solids, measure liquids, filter a mixture, and observe chemical reactions. Great emphasis is placed on safety precautions that should be observed whenever you perform an experiment and use this apparatus. Several useful manipulative techniques are also illustrated throughout this lab and in A Special Message on Safety. In many of the later experiments, references will be made to these sketches and procedures. You will also be referred to many of the safety precautions and procedures explained in all parts of this experiment. It is important that all students develop a positive approach to a safe and healthful environment in the laboratory. OBJECTIVE After completing this experiment, you should be able to use laboratory equipment safely and skillfully. Safety Take the necessary safety precautions before beginning each part of this experiment. Always wear safety goggles, apron and closed-toe shoes when in the laboratory. Get into the ‘good habit’ of always putting on this standard safety equipment as soon as you enter the lab. It is important that you and your partner observe all safety precautions while conducting experiments. Clean Up At the end of each part of this lab, all glassware and ceramic evaporating dish must be cleaned and given a final rinse with distilled water. All your personal lab equipment must be securely locked in your equipment drawer. All common items must be returned to their original location, either under the hood, or common cabinet as directed by your instructor. PART 1: THE SCALE – Massing solids Apparatus Analytical Scale Weigh paper Spoon Materials Nickel Sulfate 1 Procedure 1. When a scale is required for determining mass, you will use an analytical balance. See Figure 1 below. Analytical balances vary in sensitivity from 0.1gram, 1.01gram to 0.001 gram. For this lab we will be utilizing the scale that is sensitive to 0.100 gram. This means that all your mass readings should be recorded to the nearest 0.001 gram. Figure 1 2. The scale should only be moved by your instructor. 3. Before using the scale, always check to see that the digital readout is at zero. If the pointer is not at zero, gently press the zero button and wait for the balance to zero. Whenever weighing chemicals, always use weighing paper or a glass container, NEVER place chemicals or hot objects directly on the balance pan. They can permanently damage the surface of the balance pan and affect the mass weighing. CAUTION Do not touch chemicals with your hands. Always wear safety goggles, apron and gloves when handling chemicals. Carefully check the label on the reagent bottle or container before removing any of the contents. Never use more of a chemical than directed. You should know the locations of the safety shower and eyewash and how to use them in case of an accident. 4. Make sure that the reading on the scale is set at zero by following procedure 2 a. Gently blow onto the weighing surface of the balance. Record your observation: 5. Zero the balance again. Obtain a piece of weigh paper and place it on the scale pan. Determine the mass of the paper. Record the mass of the weigh paper to the nearest 0.001g. 6. Using a spoon, obtain a spoonful of nickel sulfate from a reagent bottle, under the hood, and place it on a separate piece of weigh paper. Take this back to your lab table to mass. 7. Now slowly pour the nickel from the weigh paper onto the weigh paper on the balance pan, until the scale reads approximately 1.5 grams. 8. Record the mass of the weigh paper and nickel sulfate to the nearest 0.001g. 9. Calculate the mass of the nickel sulfate you have measured out. 10. Take your nickel sulfate sample and weigh paper off of the balance. Zero the balance. 11. Another method of massing can be completed by taring the scale. 12.To tare, means to remove the mass of the weigh paper. Place a piece of weigh paper onto the scale. Press the zero button on the scale. 13.Now slowly pour the nickel sample from the weigh paper, step 8, onto the weigh paper on the scale pan. 14.Record the mass to the nearest 0.001g. 15.What is the mass of the nickel sulfate you have measured out. 3 16.Are the masses in steps 9 and 15 the same or different? Why? 17. Place your massed nickel sulfate sample into a 250ml beaker. 18.Cover your beaker with a piece of parafilm and place into your equipment drawer. We will use this sample in Part 2. CAUTION Never discard chemical or broken glassware important safety precaution against fires, anyone who empties the wastepaper contamination, never pour unused chemicals PART 2: into the wastepaper basket. This is an and it prevents personal injuries to basket. As a precaution against back into their original bottles. MEASURING LIQUIDS Apparatus Graduated Cylinder Buret Clamp and Buret Pipet Ring stand Beakers Materials Water Figure 2 CAUTION Safety goggles, apron and gloves must be worn whenever you measure chemicals. Never pour a liquid directly from its reagent bottle into the buret. You should first pour the liquid into a small beaker that is easy to handle. Then pour the liquid from the small beaker into the buret. This simple method will prevent unnecessary pillage. Never pour any unused liquid back into the reagent bottle. 4 Procedures 1. Burets, fitted with a stopcock, a pinch clamp, or a glass bead, are used for delivering any desired quantity of liquid up to the capacity of the buret. Any burets are graduated in tenths of milliliters, See Figure 2. When using a buret, follow these steps: a) The buret has been clamped into positions on a ring stand and filled with water. See Figure 2. Bring a 50ml beaker with you to the buret. DO NOT move the buret or ring stand. b) Place the 50ml beaker at the bottom of the buret. The beaker serves to catch any liquid that will be drawn off. c) Observe that the surface of the liquid in the buret is slightly curved. It is concave if it wets the glass, convex if it does not wet the glass. Such a curved surface is called a meniscus. If the liquid wets the glass, you read to the bottom of the meniscus as shown in Figure 3. Locate the bottom of the meniscus when reading the volume level in the buret. The volume measurement is read from the BOTTOM of the meniscus. The buret reads from 0.0ml at the top to 50.0ml at the bottom. The buret reading in Figure 3 would be recorded as 15.7ml. Figure 3 d) Record your buret reading. e) Open the stopcock and allow between 8ml and 10ml to dispense into your beaker. Close the stopcock. f) Read and record you final buret reading below. ________ ___ g) Subtract your measurements from d) and f) to obtain the actual amount of water dispensed. Show your work.(Keep this water for the next part) 2. Pipettes are made in many sizes, see Figure 4, and are used to deliver measured volumes of liquids. A pipet is fitted with a suction bulb used to withdraw air from the pipet while drawing up the liquid to be measured. See Figure 4. Always use the suction bulb – NEVER pipet by mouth. Figure 4 5 Use your thumb and forefinger to press on valve "A" and squeeze the bulb with other fingers to produce a vacuum for aspiration. Release valve "A" once the bulb is completely deflated. Hold the pipette close to its upper end and insert into the bottom of the propipette. WARNING: Extreme care should be taken not to place stress on the pipette or it may shatter. Figure 5 Insert the pipette into the beaker of water you dispensed from the buret. Press on valve "S". Suction will draw liquid up into the pipette. Continue pressing valve "S" until the liquid reaches the desired level. Carefully adjust the fluid level so that the bottom of the meniscus coincides with the calibration line on the pipette. Note: Press directly on the letter A, S, or E when opening valves. Applying pressure away from the center of these valves will damage them. Draw the water from the beaker up into the pipette. When the water has been sucked up, read and record the volume of water in the pipette. 3. You will now dispense this water into a graduated cylinder, Figure 6. Press on valve "E" to expel liquid into your graduated cylinder. Carefully remove the pipette (see warning in step 2.) and touch the tip of the pipette to the inside of the receiving flask to drain the last bit of solution. Figure 6 Read and record the volume of water in the graduated cylinder. 4. Carefully pour the contents of the graduated cylinder into a 50ml beaker. a. Read and record the volume of water in the beaker. b. Compare and contrast the volume measurements made using the four devices. c. Identify one advantage and one disadvantage of using a buret to measure liquids. 6 d. Identify one advantage and one disadvantage of using a graduated cylinder to measure liquids. e. Hypothesize a reason why a beaker is NEVER used to measure liquids. 5. Empty the water from your 50ml beaker into the sink. 6. Carefully measure 25.0ml of distilled water, using your graduated cylinder. 7. Slowly pour the distilled water into the beaker containing the nickel sulfate from part 1. Stir gently with the glass stirring rod to until all of the solid has dissolved. 8. Record two observations that you made while the reaction was taking place: 9. Hypothesize as to what has happened to the solid crystals. Explain your reasoning. 10.If you are not continuing on to Part 3, cove the beaker with parafilm and lock securely in your lab equipment drawer. PART 3: FILTRATION Safety Take the necessary safety precautions before beginning each part of this experiment. Always wear safety goggles, apron and closed-toe shoes when in the laboratory. Get into the ‘good habit’ of always putting on this standard safety equipment as soon as you enter the lab. It is important that you and your partner observe all safety precautions while conducting experiments. Read all safety precautions while conducting experiments. 7 Apparatus Ring stand Stirring rod Iron Ring Evaporating dish Funnel Matches Iron Ring Filter Paper Ceramic-centered Wire gauze Materials Sodium Hydroxide, NaOH, 1M Hydrochloric Acid, HCl, 1M Nickel sulfate compound from Part 2 Figure 7 Procedures 1. Sometimes liquids contain particle of insoluble solids, present either as impurities or as precipitate formed by the interaction of the chemicals used in an experiment. If the particles are insoluble and denser that water, they soon sink to the bottom. Most of the clear, supernatant (swimming above) liquid may be poured off without disturbing the precipitate. Such a method of separation is known as decantation. The soluble salts are in the supernatant liquid which has been decanted into the beaker. 2. Fine particle, or particles that settle slowly, are often separated from a liquid by filtration. Support a funnel on a small ring on the ring stand as shown on Figure 7. If the ring is too large place a clay triangle on top of the ring to support the funnel Use a beaker to collect the filtrate. Adjust the funnel so that the stem of the funnel just touches the inside wall of the beaker. This will speed up the filtration process by decreasing the dropping, hence increases the continuous flow through capillary action due to the intermolecular force, hydrogen bonding. Figure 8 3. Fold a circular piece of filter paper along its diameter, and then fold it again to form a quadrant. See Figure 8. Separate the folds of the filter, with three thicknesses on one side and one on the other; then place it into the funnel. The funnel should be wet before the paper is added. Use your plastic wash bottle to do this. Then wet the filter paper with a little water and press the edges firmly against the sides of the funnel so no air can get between the funnel and the filter paper while the liquid is being filtered. 8 4. EXCEPTION: A filter should not be wet with water when the liquid to be filtered does not mix with water. WHY? ______________________________ _ 5. Using your graduated cylinder, measure 25.0ml of hydrochloric acid, HCl. 6. Place your beaker containing the nickel sulfate compound, from Part 2, under your personal hood.(This is the white box on the wall next to your lab station. Each lab group has its own personal fume hood). Carefully pour the hydrochloric acid into this beaker. Stir gently. 7. Record one observation from this reaction. 8. The contents of your beaker contains nickel (II) chloride and water. Rinse your graduated cylinder with distilled water. Then use it to measure 25.0ml of sodium hydroxide, NaOH. 9. Pour the sodium hydroxide into the beaker containing the nickel (II) Chloride. Stir gently and record one observation. 10.Measure an additional 25.0ml of sodium hydroxide, NaOH, into your graduated cylinder, and slowly add to your beaker. Gently stir and record one observation. 11.The solid that forms from the mixing of two solutions is called a precipitate. 12. To separate the precipitate from the solution, pour the beaker contents into the filtering system you set up in Part 3 steps 1-3. a) The filter paper should not extend above the edge of the funnel. It is better to use a filter disc that leaves about 1cm of the funnel exposed. b) Do not over fill the filter. It must never overflow. The liquid must never go above the paper line. Figure 7 9 c) Try to establish a water column in the stem of the funnel thus excluding air bubbles, look at step # 2, and then add the liquid just fast enough to keep the level about 1cm from the top of the filter paper. d) When a liquid is poured from a beaker or other container, it may adhere to the glass and run down the outside wall. This may be avoided by holding a glass stirring rod against the lip of the beaker, as shown in Figure 7. The liquid will run down the rod and drop off into the funnel without running down the side of the beaker. e) To remove the remaining precipitate from the beaker. Hold the beaker with its spout down towards the funnel and squirt your wash bottle up into the beaker, behind the precipitate, to wash out the solid product. This is a useful skill. The precipitate is retained on the filter paper. What PROPERTY of the precipitate enables it to be separated from the water by filtration? What does the filtrate contain? 13. If you are not completing Part 4 today, cover the beaker contents, filtrate, with parafilm and store in your lab equipment drawer. 14.If you are not completing Part 4 today, carefully place the filter paper, along with the precipitate, into a different beaker. Cover the beaker with parafilm and store in your lab equipment drawer. 15.At the end of this part of the experiment, all equipment you store in the lab drawer should be completely cool, clean, dry, and arranged in an orderly fashion for the next lab experiment. 10 PART 4 THE BURNER Apparatus Heat Resistant Mat Crucible tongs Burner Matches Evaporating dish Materials Copper wire, 18 gauge Procedures 1. The Bunsen or Tirrell burner is commonly used as a source of heat in the laboratory. Although the details of construction vary among burners, each has a gas inlet located in the base, a vertical tube or barrel in which the gas is mixed with air, and adjustable opening or ports in the base of the barrel. These ports admit air to the gas stream. The burner may have an adjustable needle valve to regulate the flow of gas. In some models the gas flow is regulated simply by the flow of gas. The burner is always turned off at the gas valve on the supply line, never at the needle valve. Look at Figure 9 as you examine your Bunsen burner and locate these parts. Figure 9 CAUTION Before you light the burner, check to see that you and your partner have taken the following safety precautions against fires: Wear safety goggles, and aprons. Confine long hair and loose clothing: Tie long hair back at the back of the head away from the front of the face, roll up long sleeves on shirts, blouses and sweaters away from the wrists. You should also know the locations of fire extinguishers, fire blanket, safety showers, and sand buckets and how to use them in case of a fire. 2. In lighting the burner, partially close the ports at the base of the barrel, light the match. Hold the lit match just below the top of the barrel. Turn the gas full on and slowly raise the lit match toward the top of the barrel. The gas flow may be regulated by adjusting the gas valve until the flame has the desired height. If a very low flame is needed, remember that the ports should be partially closed when the gas pressure is reduced. Otherwise, the flame may burn inside the base of the barrel. When improperly burning in 11 this way, the barrel will get very hot, and the flame will produce a poisonous gas, carbon monoxide. CAUTION Carbon monoxide is a poisonous gas. If the flame is burning inside the base of the barrel, immediately turn off the gas at the gas valve. Do not touch the barrel of the burner, for it is extremely hot! Allow the barrel of the burner to cool off and then proceed as follows: Begin again, but first decrease the amount of air admitted to the burner by partly closing the ports. Turns the gas full on and then relight the burner. Control the height of the flame by adjusting the gas valve. By taking these steps, you should acquire a flame that is burning safely and is easily regulated throughout the experiment. 3. Once you have a flame that is burning safely and steadily, you can experiment by completely closing the holes (ports) at the base of the burner. Describe what the flame looks like when the ports are completely closed. 4. Using the crucible tongs, carefully hold an evaporating dish in the tip of the flame (underside to the flame) for about 3 – 5 minutes. Place the dish on the ceramic pad, allow the dish to cool, and then examine the underside. Describe the results and suggest a possible explanation for this observation. Such a flame is seldom used in the laboratory. For laboratory work, you should adjust the burner so that the flame will be free of yellow color, nonluminous, and also free from the ‘roaring’ sound caused by admitted too much air. 5. Regulate the flow of gas to give a flame extending roughly 8cm above the barrel. Now adjust the supply of air until you have a quiet, steady flame with a sharply defined, light blue inner cone. This adjustment gives the highest temperature possible with your burner. Using the crucible tongs, inset a 10cm piece of copper wire into the flame just above the barrel. Lift the wire slowly up through the flame. Where is the hottest portion of the flame located? 12 6. Hold the wire in this part of the flame for a few seconds. Observe both the flame and the wire. Describe the results of each. 7. Shut off the gas burner. Now think about what you have just observed in procedures 4-6. Why is the nonluminous flame preferred over a yellow luminous flame in the laboratory? 8. Now that you have mastered the Bunsen burner, you will be using it to evaporate the filtrate from Part 3. 9. Set up the evaporating equipment as shown in Figure 9. Do NOT place the Bunsen burner under the wire gauze and do NOT light the Bunsen burner yet. Do NOT place the evaporating dish onto the wire gauze at this time. 10.Using your graduated cylinder, measure 15.0ml of your filtrate and pour into your evaporating dish. 11. Place the Bunsen burner NEXT to the evaporation set up, NOT underneath it. Light the burner and adjust the burner until you have a blue cone that is about 1 ½” tall. Contact your instructor if you have difficulty doing this. 12.When evaporating, the tip of the blue cone should just touch the surface of the wire gauze. Because the flame is NOT under the wire gauze, you can adjust the height of the iron ring and gauze without getting burnt. Figure 9 13.Once the adjustment is complete, carefully place the evaporating dish and filtrate onto the wire gauze. 14. NOW you may move the Bunsen burner into position under the wire gauze by grabbing at the base and sliding it into position. 15.Soluble products can be recovered from the filtrate by pouring the filtrate into an evaporating dish and evaporating it nearly to dryness. 16.Pay close attention as the filtrate begins to boil. Continue heating until most of the liquid portion has been removed. 17.Turn off the burner BEFORE all the liquid has been removed. The evaporation set up is extremely hot. Do NOT attempt to move any equipment while it is hot. 13 18.Record two observations from the evaporation process. 19.Provide a possible explanation for what you observed 20.What PROPERTY of salt prevents it from being separated from the water by filtration? 21.When the evaporating dish has completely cooled, discard the contents of the evaporating dish into the sink along with the unevaporated filtrate in your beaker. 22.At the end of this part of the experiment, all equipment you store in the lab drawer should be completely cool, clean, dry, and arranged in an orderly fashion for the next lab experiment. 23.Check to see that the valve on the gas jet is completely turned off. Wash your hand thoroughly before leaving the lab. PART 5 Dissolving a Precipitate Apparatus Beaker Graduated Cylinder Stirring Rod Materials Nickel precipitate from Part 3 Ammonia, NH3 6M Procedures 1. This procedure MUST be done under your personal fume hood. This is the white box on the wall next to your lab station. Each lab group has its own personal fume hood. 2. Place your 250ml beaker containing the filter paper and precipitate under your personal fume hood. 14 3. Using your graduated cylinder, carefully measure 50.0ml of NH3, ammonia. 4. Slowly pour the ammonia directly into the beaker containing the filter paper and precipitate. 5. Gently move the filter paper around with a glass stirring rod, to ensure that all the precipitate has dissolved. 6. Using your forceps, hold the filter paper above the solution and rinse gently with distilled water to wash all ions back into the solution. 7. Dispose of the filter paper in the garbage can. 8. Record two observations from this part 9. Provide a possible explanation for what you observed 10. Discard of the contents of your beaker as directed by your instructor. PART 6 Making a Solution Apparatus Beaker Graduated Cylinder Volumetric Flask Stirring Rod Scale Weigh Paper Materials Nickel Nitrate Hexahydrate, Ni(NO3)2*6H2O Ethylenediame (10ml/100ml Solution) Hydrochloric Acid, HCl, 6M Procedures 1. Using the proper procedure, mass out 4.75 grams of nickel chloride hexahydrate. (Note: Hexahydrate means that water molecules are bonded to the nickel chloride). 15 2. Carefully add the nickel compound to a clean, dry 100ml volumetric flask. 3. Add distilled water to HALF-FILL the volumetric flask and swirl the contents until the solid has been completely dissolved. 4. Once the solid is dissolved, slowly add distilled water to the volumetric flask, until the bottom of the meniscus is at the etched line on the neck of the flask. This indicated that you have exactly 100ml of solution. 5. Due to hydrogen bonding, it is difficult to thoroughly mix the solution in the volumetric flask. Pour your solution into your 250ml beaker and stir gently with your stirring rod. 6. Using your graduated cylinder, measure 5ml of the solution into four separate test tubes. 7. Test tube #1 is your control. 8. Rinse your graduated cylinder. 9. Measure 5 drops of the Ethylenediamine and pour it into test tube #2. 10.Measure 15 drops of Ethylenediamine and pour it into test tube #3. 11.Measure 30 drops of Ethylenediamine and pour it into test tube #4. 12.Record your observations 13.Provide an explanation for your observations. 14.To test tubes #2, 3, and #4, add the hydrochloric acid, HCl, dropwise to each until you observe a change back to the original color. 15.Note how many drop of HCl were required for each test tube. Test Tube #1 None Test Tube #2 16 Test Tube #3 Test tube #4 16.Provide a possible explanation for your observations. 17.Dispose of the product as directed by your teacher. At the end of this part of the experiment, all equipment you store in the lab drawer should be completely cool, clean, dry, and arranged in an orderly fashion for the next lab experiment. QUESTIONS Answer the following questions using complete sentences. Remember, all answers should be your own words. 1. As soon as you enter the lab, what standard safety equipment should you put on immediately? 2. Before doing an experiment, what should you read? 3. Before you light a burner, what safety precautions should always be followed? TRUE or FALSE Read the following statements and indicate whether they are true or false. Place your answer in the space next to the statement. 1. Never work alone in the laboratory. 2. Never lay the stopper of a reagent bottle on the lab table. 3. At the end of an experiment, save all excess chemical and pour them back into their stock bottles. 4. The quickest and safest way to heat a material is a test tube is by concentrating the flame on the bottom of the test tube. 17 5. Use care in selecting glassware for high temperature heating. Glassware should be Pyrex or a similar heat-treated type. 6. Safety goggles protect your eyes from particle and chemical injuries. I do not need to make my teacher aware of the fact that I wear contact lenses. 7. Never use the wastepaper basket for disposal of chemicals unless told to do so by your teacher. 8. First aid kits may be used by anyone to give emergency treatment after an accident. CHEMICAL APPARATUS Identify each piece of apparatus. Place your answers in the ell with the picture in it. 18