Lab Notebook Composition and Separation Chemistry is the study of the composition and properties of matter and the changes it undergoes. When two or more substances that do not react chemically are blended, the result is a mixture in which each of the component substances retains its identity and its fundamental properties. The separation of the components of mixtures is a process frequently encountered in chemistry. Physical processes are often used so as to retain the fundamental properties of the components in the mixture. Physical techniques used to separate mixtures rely on differences in the properties of the components in the mixture. These physical separation techniques include filtration, distillation, sublimation, and extraction. You will apply these techniques in this experiment to separate a sample containing a homogeneous mixture of ammonium chloride (NH4Cl), sodium chloride (NaCl), and sand (silicon dioxide, SiO2) into their individual components. Sublimation is the direct passage of a substance from the solid to the gas state. You will remove ammonium chloride from the mixture of solids by subliming it, since it is the only component in the mixture capable of subliming under normal experimental conditions in the chemistry laboratory. As the ammonium chloride compound sublimes it will chemically react to release ammonia gas and gaseous hydrochloric acid which are both harmful to breathe so this first part of the procedure must be done in the chemical fume hood in the lab. Extraction is a separation technique that involves transformation of a substance in the mixture from one phase to another. Since sodium chloride is soluble in water you will extract the sodium chloride out of the remaining solid sample by adding water to the solid sample. Once the sodium chloride dissolves in the water the sand will remain in the solid phase to create a solid-liquid heterogeneous mixture. Filtration is a separation process for a solid-liquid mixture by passing the mixture through a barrier, usually filter paper, with fine pores. The larger particles of sand will be trapped by the filter paper allowing the liquid phase solution containing the water and dissolved sodium and chloride ions to pass through. Distillation is a process used to separate the components of a homogeneous solid-liquid mixture (a solution containing dissolved solids). The liquid component vaporizes as is reaches its boiling point, leaving a residue of the solid component in the bottom of the container. The sodium chloride can be recovered from the sodium chloride homogeneous solution by evaporation of the water. Measurement Chemistry is an experimental science studying matter and the changes it undergoes. Measurements are fundamental in experimental science to determine whether change has occurred and, if it has, how much change has occurred. In this experiment you will become familiar with measuring mass and volume. Scientific measurements must be as precise as possible. This means that every measurement will include one uncertain or estimated digit. When making measurements we normally estimate between the smallest scale divisions on the instrument being used. Then only the uncertain digit should vary if the measurement is repeated using the same instrument, even if it is repeated by someone else. The accuracy of a measurement or calculated quantity refers to its agreement with some known value. For example in this experiment you will be trying to determine the percent composition of each component in the mixture. Once the experiment is completed and turned in your instructor will tell you the known composition and with this
2 information you could then determine the accuracy of your lab work. Because every measurement made in the laboratory is really an approximation, it is important that the numbers you record reflect the precision of the device you are using to make the measurement. The assumption is made in this course that an uncertainty of at least one unit exists in the last digit. The uncertainty of the measurement should be given with the actual measurement, for example: Analytical Balance Mass example: 5.0988 +/- 0.0001 g 25 mL Graduated Cylinder Volume example: 10.5 +/- 0.1 mL Each instrument has an inherent amount of uncertainty in its measurement. Even the most precise measuring device cannot give the actual value because to do so would require an infinitely precise instrument. A measure of the precision of an instrument is given by its uncertainty. If you are unsure of the uncertainty of an instrument a good rule of thumb is to assume the uncertainty of a measuring device is 20% of the least count. Recall that the least count is the smallest subdivision given on the measuring device. Significant Figures When a measured value is determined to the highest precision of the measuring instrument, the digits in the measurement are classed significant digits or significant figures. When reading data measured by other scientists it is important to be able to determine the precision of any measured value so a set of rules was established. The following rules will help you determine the number of significant figures in any measurement. 1. All nonzero digits are significant. (3.467 cm = 4 significant figures) 2. Zeros between nonzero digits are significant. (2.07 mL = 3 significant figures) 3. Zeros beyond the decimal point at the end of a number are significant. (6.00 mL= 3 significant figures) 4. Zeros preceding the first nonzero digit in a number are not significant. (0.0341 g = 3 significant figures) 5. Zeros at the end of a number are significant if the number contains a decimal point. 0.0300 g (three significant figures) 3.0 cm (two significant figures) A problem arises when a number ends with zeros but contains no decimal point. In such cases, it is normally assumed the zeros are not significant. Scientific (exponential) notation can be used to clearly indicate whether the zeros at the end of a number are significant. For example, a mass of 11,500 g can be written in scientific notation showing three, four, or five significant figures depending on how the measurement is obtained: 1.15 x 10 4 g (three significant figures) 1.150 x 10 4 g (four significant figures) 1.1500 x 10 4 g (five significant figures) Significant Figures in Calculations When carrying measured quantities through calculations, the least certain measurement limits the certainty of the calculated quantity and thereby determines the number of significant figures in the final answer. To keep track of significant figures in calculations, we will make frequent use of two rules, one for addition and subtraction and another for multiplication and division.
3 Addition and subtraction the result of a calculation has the same number of decimal places as the measurement with the fewest decimal places (the least precise measurement). When the result of the calculation implies more precision than could be possible, due to the measurements taken on the centigram and decigram balances, it must be rounded off. For example: Add the mass measurements taken from three different balances, each having a different degree of precision. Centigram balance 20.42 g Two decimal places
Analytical balance 1.3220 g Four decimal places Most precise measurement Decigram balance + 83.1 g One decimal place Least precise measurement Final calculated answer 104.8420 Implies more precision than could be possible so it must be rounded to the least precise measurement, the tenths place (0.0) Correct answer 104.8 g Four significant figures after rounding
Multiplication or division the result of a calculation contains the same number of significant figures as the measurement with the fewest significant figures. When the result contains more than the correct number of significant figures it must be rounded off. For example, if we have 5.098 g of sodium chloride and 30.5 mL of solution and we wanted to determine the density (mass/volume) of the salt solution in this experiment: (5.098 g) / (30.5 mL) = 0.167147541 is the answer on the calculator However, this answer describes a precision of 9 significant figures which is far beyond the precision of the original measurements. Although the mass of sodium chloride has four significant figures (5.098 g), the volume of the solution has only three significant figures (30.5 mL) so the density of the solution can only be recorded as 0.167 g/mL, with three significant figures. Note that for addition and subtraction, decimal places are counted; whereas for multiplication and division, significant figures are counted. Rounding of Numbers When rounding off numbers, look at the leftmost digit to be removed to determine whether you will round the number up or down. If the leftmost digit to be removed is less than 5, the preceding number is left unchanged. Rounding 6.248 to two significant figures gives 6.2 If the leftmost digit to be removed is 5 or greater, the preceding number is increased by 1. Rounding 5.735 to three significant figures gives 5.74 and rounding 3.376 to two significant figures gives 3.4.
4 Mass The directions in this experiment are written for use with an analytical balance. These milligram balances are extremely precise giving a mass measurement to the ten-thousandth place (0.0001 g). This is considered the precision (or an uncertainty of +/- 0.0001 g) of the balance. Even though this is a digital instrument, the balance is making an estimate at the ten-thousandths place. All measurements of mass taken on the analytical balance recorded in your data sheet should reflect this degree of precision. When using the analytical balance please be gentle with these sensitive instruments and use the following procedures: 1. Before placing your item to be massed on the balance check the display to make sure it is reading zero. If not press the tare bar once to zero out the balance. 2. Carefully open a side door and place the item on the pan and close the door. 3. Allow sufficient time for the mass to be measured. 4. Record the mass, remove the item and close the door. 5. Never place chemicals directly on the balance pan; first place the weighing boat or container on the balance pan, tare the balance and then mass the chemicals by placing them onto the weighing boat or into the container (beaker, for example) 6. Please be sure to clean up any materials you spill on or around the balance and close all the glass doors on the balance once you are done with you measurement. 7. Never make any adjustments to the balance. If it seems out of order tell your instructor. 8. Make sure items to be weighed on the balance are at room temperature, never put a hot object on the balance pan.
Volume The graduated cylinder is the device you will be using in lab to measure liquid volumes. Graduated cylinders are tall, cylindrical vessels with graduations scribed along the side of the cylinder. Since volumes are measured in these cylinders by measuring the height of liquid, it is crucial that the cylinder have a uniform diameter along its entire height, which is the case with the glass cylinders you are using in lab. Beakers and flasks are marked to indicate only approximate volumes and should not be used to measure volumes during experiments. When observing a volume in a graduated cylinder, read the point on the graduated scale that coincides with the bottom of the curved surface called the meniscus of the liquid. Most volumes measured in the graduated cylinder should be estimated and recorded to the nearest 0.1 mL but check with your instructor if you are not sure.
5 Brief Review of Metric Systems more information available in your textbook In science the metric system is used almost exclusively. The basic unit of length is the meter (m); of mass, the gram (g); of volume, the liter (L). The meter, the gram, and the liter are related to larger and smaller units by multiples of 10. Prefixes are used for the unit of measure expressing these multiples of 10. Prefix Abbreviation Value x basic unit Some Conversion Factors Kilo- k 1000 1 km = 1000 m Deci- d 0.1 1 m = 10 dm Centi- c 0.01 1 m = 100 cm Milli- m 0.001 1 m = 1000 mm How does 1 kilometer compare to the other units in the metric system? 1 km = 1000 meters = 10,000 dm = 100,000 cm = 1,000,000 mm Safety You must wear goggles and an apron whenever you are working in the lab. Before coming to lab class for this experiment you are required to go to the Flinn Scientific MSDS web page (http://www.flinnsci.com/search_MSDS.asp) and read the MSDS information required for your pre-lab assignment. Refer to the syllabus and additional materials for more details regarding the pre-lab. Disposal of Chemicals Place the sand remaining at the end of the experiment in the waste crock. Rinse the sodium chloride in the second evaporating dish down the sink. Objectives 1. Experiment with physical processes used to separate the components of mixtures. Be able to identify characteristics of physical processes as compared to chemical processes. 2. Use Bunsen Burner properly and safely. 3. Apply techniques of filtration, extraction, and sublimation for separating the components of mixtures. 4. Correctly measure and record the mass and volume in this experiment. Be sure to record measurements with the correct number of significant figures and the uncertainty of each measurement. 5. Determine the % Composition of your sample.
6 Procedure Part A. Percentage of ammonium chloride, NH4Cl In this step ammonium chloride is removed from the mixture by sublimation and its mass is found by difference. #1. Weigh a clean, dry evaporating dish and record the mass of the evaporating dish in Table I of the Report Sheet (B). #2. Check out an unknown sample from your instructor and record the number or letter of your unknown sample on the Report Sheet. #3. Add approximately 1.00 g of the sample into the evaporating dish and reweigh. Record the actual mass of your sample in the appropriate place in Table I of the Report Sheet (A). #3. Place the evaporating dish with the sample on wire gauze supported by a ring on a ring stand IN THE FUME HOOD as shown in the picture below:
The gas valve is the lower of the two knobs (blue label) located on the side of the hood and the gas outlet is the lower of the two outlets in the hood (color coded blue). Heat the evaporating dish containing the solid sample with a burner for about seven minutes. Remove the flame and gently stir the mixture with a stirring rod (being careful to wipe any solid on the lip of the evaporating dish as you finish stirring), then apply heat again for at least five minutes. #4. Let the evaporating dish cool. Use the metal crucible tongs to carefully remove the evaporating dish and place it on a clean, dry watch glass for transport to the balance area. Weigh the evaporating dish and remaining solid, recording the mass measurement Table I (C). I would suggest you take a couple of minutes to complete questions 1 and 2 at this point since they are asking about the sublimation portion of the experiment. Part B. Percentages of sodium chloride, NaCl, and of sand In this step the solid remaining from the previous step is mixed with water in order to dissolve the sodium chloride. The solution is filtered away from the sand and the mass of sodium chloride is found by evaporating the water from the solution. The sand remaining on the filter paper is dried and its mass determined. #1. Measure approximately 20 mL of deionized water using a 25 mL graduated cylinder and record the volume in Table II. Add this water to the solid in the evaporating dish and stir gently. Record the volume of water in Table II (D). #2. Obtain a second clean, dry evaporating dish and weigh it. Record the mass in Table II (E).
7 #3. Obtain a piece of filter paper and fold it as illustrated below, and weigh it. Record the filter paper mass in Table II (F) #4. Place the filter paper in a funnel supported by a clay triangle on a ring attached to a ring stand, and wet it gently to make the paper stick to the funnel. Place the second weighed evaporating dish under the funnel with the end of the stem of the funnel lightly touching the inside of the evaporating dish.
#5. Slowly pour the sand-water heterogeneous mixture into the funnel and filter paper. Add a small amount of distilled water from your wash bottle to rinse out any remaining solid (sand) from the original evaporating dish and pour it through the filter. (Add only enough water to remove any solids. Excess water will have to be evaporated.) #6. After the liquid has drained through the filter, carefully remove the paper from the funnel, open it out and place it on a watch glass. Place the glass and paper under a heating lamp to dry. Check the drying progress of the filter paper as it may burn if it becomes overheated. You need to weigh the dried paper to find the mass of the sand, which is in step 7 however, you can proceed to step 8 while the filter paper is drying. #7. Weigh the dried sand and filter paper and record this mass data in Table II (F). I would suggest you take a couple of minutes to complete questions 3 and 4 at this point since they are asking about the sand portion of the experiment. #8. Clamp a ring on the ring stand and adjust its height so that the hottest part of the Bunsen burner will reach the ring. Place wire gauze on the ring.
8 # 9. Fill 250-mL beaker about two-thirds full with deionized water (use the deionized water faucet at the instructors station) and set it on top of the wire gauze. Use the crucible tongs to carefully put the evaporating dish on the beaker. # 10. Light the Bunsen burner, adjust the burner to maximum flame height, and heat the water to a fast boil. At this point, the flame height may be lowered slightly. Add water to the beaker if necessary by using a wash- bottle. DO NOT let the beaker boil dry. #11. Evaporate the solution until only dry solid remains in the evaporating dish. #12. Turn off the Bunsen burner, and when the water in the bath has cooled down slightly, remove the evaporating dish from the bath with a tong and set it on the bench top to cool. Weigh the cooled dish plus solid and record it in Table II. I would suggest you take a couple of minutes to complete questions 5 and 6 at this point since they are asking about the sodium chloride portion of the experiment.
Data Section of you lab notebook should contain the following information: (1) Unknown Number (or Letter) __________________________________ (2) Data table below: Table I Sublimation Data of ammonium chloride, NH4Cl Item Measured Measurement (include uncertainty and unit) # sig figs (A) Mass of evaporating dish with sample before heating
(B) Mass of empty evaporating dish
Mass of sample (A B)
(C) Mass of evaporating dish with sample after heating
9 Table II Percentages of sodium chloride, NaCl, and of sand Item Measured Measurement (include uncertainty and unit) # sig figs (D) Volume of water used
(E) Mass of 2 nd evaporating dish
(F) Mass of filter paper
(G) Mass of dry filter paper with sand
(H) Mass of 2 nd evaporating dish with remaining solid
Questions For each of the following questions involving calculations you must show the mathematical set up required to answer the question in your lab notebook and have the correct number of significant figures in order to receive credit for your response. Question #1: Determine the mass loss due the sublimation of ammonium chloride (NH4Cl). This mass loss is the mass of ammonium chloride that was originally present in the mixture. Question #2: What is the percentage of ammonium chloride present in the original solid sample? Question #3: Determine the mass of the solid substance in the filter paper. This is the mass of sand (silicon dioxide, SiO2) that was originally present in the mixture. Question #4: What is the percentage of sand (silicon dioxide, SiO2) present in the original solid sample? Question #5: Determine the mass of the solid substance in the 2 nd evaporating dish. This is the mass of sodium chloride (NaCl) that was originally present in the mixture. Question #6: What is the percentage of sodium chloride (NaCl) present in the original solid sample?
10 Question #7: Complete the following table in you lab notebook:
Theoretically, what should be the total percentage?
Question #8: Percent error is a calculation done after an experiment that gives the experimenter an idea of how the accuracy of their work in lab. Use the following mathematical equation to determine the percent error for the total percentage of the substances you have separated in the experiment. Percent error = |experimental percent theoretical percent| / [theoretical percent] Question #9: Using your own words in a complete sentence give a definition and one common example of each of the four types of separation techniques used in this experiment. (a) sublimation (b) extraction (c) filtration (d) distillation Question #10: A 4.00 gram sample of a solution of sodium chloride in water was heated until all the water had evaporated. The sodium chloride that remained weighed 1.22 grams. Calculate the percentage of water in the original solution. Question #11: A laboratory technician wants to prepare 80.0 grams of a mixture containing 50.0 % sand, 30.0 % sodium chloride, and 20.0 % ammonium chloride by mass. Calculate the mass of each substance that the technician would need to mix. Question #12: What are the possible sources of experimental errors in this experiment? Question #13: During dental work or minor surgery, a local anesthetic, such as procaine or lidocaine, is used to deaden the pain in a small area of the body. Although both are about equally effective in numbing the pain, procaine is eight times more toxic than lidocaine. With which anesthetic is it more important to be precise and accurate in administering a dose? Use a sentence or two to explain your choice. Question #14: When cutting the legs of a table to make it lower, precision is usually far more important than accuracy. Use a sentence or two to explain your choice Question #15: Determine the density of the sodium chloride solution that was collected after the filtration was completed in part B. Assume the volume of the sodium chloride solution is the same as the volume of water used in the experiment. Conclusion Write a short paragraph summarizing your work in this experiment and describe what you have learned after completing this experiment. Please note: Your conclusion should always include a sentence or two reporting the actual results of your experiment - in this case, it should include the % composition of the unknown sample you analyzed in lab. Please be sure to include this information - do NOT leave your results out of your conclusion - you are guaranteed to lose at least 1-2 points (or more). Substance Percentage found Ammonium chloride, NH4Cl Sand, SiO2 Sodium chloride, NaCl Total