This action might not be possible to undo. Are you sure you want to continue?
Seventeenth Edition Fall 2011
California State University, Fullerton
Department of Chemistry and Biochemistry
TABLE OF CONTENTS
Grading Information Laboratory Grade Laboratory Reports Academic Honesty
1 2 3 4 5 8 9
Why Do Experiments? Safety in the Laboratory Waste Disposal The Laboratory Notebook Quantitative Observations Precision of Measurements Scientific Notation Relative and Absolute Precision Rounding Off Accuracy and Error Averaging Statistical Analysis: the Rule of Four Exploration A1: Is Volume Conserved? Objectives and Introduction Graph of Water Density Procedure Calculations Report Data Sheets
11 12 13 16 20 22 23
25 28 29 34 36 37
Exploration A2: Chemistry of Aluminum Objectives and Introduction Procedure: Formation of an Aluminum Compound Procedure: Displacement Reactions of Aluminum Procedure: Determining the Empirical Formula Calculations Report Data and Results Sheets Exploration A3: An Emission Spectroscope Objectives and Introduction Procedure: Construction of the Spectroscope Procedure: Measurements Calculations Report Exploration A4: Equivalent Mass of an Acid Objectives and Introduction Procedure Report Data and Results Sheet Exploration A5: Preparation and Analysis of a Compound Objectives and Introduction Procedure Analysis of the Compound Calculations Report Data and Results Sheets Appendix – Results Reporting Forms
41 47 49 52 58 61 62 65 70 74 76 76 77 80 83-84 85 86 88-89 90-93 93 95 96 99
2 A. Consult the syllabus of your lecture instructor for details. Total: 1. In addition. Accurate and reproducible results require that you take care and pay attention to detail while doing the experiment. Quality of Results: Your results for each experiment will be graded for accuracy and reproducibility. 2. The laboratory is worth 200 points. and that you develop and master the laboratory and technical skills required for each experiment.1 B. your laboratory manual contains specific instructions for preparing the report for each experiment at the end of the description of that experiment. Laboratory quizzes (25 points each): Laboratory reports and Quality of results: A.4 A. Care and good technique will yield good results scores.5 50 36 25 36 40 187 Laboratory Quizzes (50 points) A quiz testing your preparation and understanding of the laboratory experience will be administered at the beginning of the lab session Weeks 4 and 14. Laboratory Reports: See the next page for general information concerning laboratory report preparation. 2. 3. broken down as follows: 1.LABORATORY GRADE Your work in the laboratory will generate a point total that will be added to your lecture points to generate an overall point total for the course. 1 .
usually one week after the completion of the experiment. This will keep you from falling behind and will also help you to understand the experiment while it is still in progress. General Rules: ˚ Write clearly and concisely. addressing the points described in the instructions for the experiment. In addition. (3 points) 2. 2 . see each individual experiment for details (6 points). ˚ Do not repeat what is in the laboratory manual.m. Consult the laboratory schedule for exact due dates. turned in to your laboratory instructor at the end of each laboratory period (2 points). and a sample of each different type of calculation you made in obtaining the results from your data (5 points). readability and completeness. ˚ Follow the instructions for each report.) The carbon copies of your laboratory notebook pages. filled out neatly and completely. It is a good idea to plan ahead and write parts of your laboratory report before you have finished the experiment. on a specified day.) A data and calculations section containing the data from your experiment. 3. Grading: Reports are graded for organization. Contents: Each laboratory report should contain three parts: 1. Due Dates: Laboratory reports generally are due in the Department Office (MH-580) at 5:00 p. your instructor will have the following. clarity.) A written narrative. appropriately organized.LABORATORY REPORTS You are required to submit a laboratory report for each experiment. ˚ Avoid the use of "I" except when stating your opinion.) A copy of the Results Reporting Form for the experiment (see Appendix). which will be graded as part of your report: 4.
Some of the offenses that constitute academic dishonesty are: 1) Plagiarizing the laboratory manual or another person's writing. 7) Reporting an experiment that was not actually performed. “Academic dishonesty includes such things as cheating. 3 . inventing false information or citations. Depending on the incident. Reports that are group writing efforts or that have been copied from other reports will be given zero credit and may result in disciplinary action for plagiarism. the penalty will range from a loss of all possible points for that lab to failure of the entire 5-unit course with documentation of cheating on the students file. 2) Turning in someone else’s work. It usually involves an attempt by a student to show possession of a level of knowledge or skill which he or she does not possess. 3) Copying. p. 69 Penalties for academic dishonesty are severe.” 2011-2013 CSUF catalog. 8) Reporting work performed in a previous semester. You are encouraged to work together with classmates in doing calculations. as evidenced by the same mistake on different students' papers. analyzing data and arriving at correct interpretations. you must do the calculations and analysis on your own data and write your own report in your own words. 6) Adding to or changing material in one's laboratory notebook after duplicate pages have been submitted. Nevertheless. and helping someone else commit an act of academic dishonesty.ACADEMIC HONESTY Each laboratory report must be your own individual work. 5) Reporting laboratory work that is not on the duplicate notebook pages. be it a full report or just a few comments. 4) Presenting data in a report that are not on the duplicate notebook pages. plagiarism.
the scientist then uses it to deduce what should occur under other conditions (makes predictions). When the new experiments agree with the predictions. In either case. he or she then proposes a general conclusion regarding these results (frames a hypothesis). They are both the starting point of information gathering and the ultimate test of whether hypotheses are correct. First. 4 . When the experiments do not agree. whereas research explores the unknown. a scientist makes observations under controlled conditions (does an experiment). the scientist then makes more observations (tests the predictions). If the hypothesis is sufficiently general. In designing the explorations that constitute the laboratory portion of Chemistry 120A. and theories must agree with experimental observations. the hypothesis is incorrect and must be revised.WHY DO EXPERIMENTS? Our General Chemistry course includes a laboratory component because all of chemistry is based on observations. Chemistry provides particularly instructive examples of experiments in science because observations can be made in a chemistry laboratory under controlled conditions. The interplay between theory and observations can be described by a general method. In Chemistry 120A. but all chemical theory explains the observations that chemists have made. experiments occupy a central role in any science. we expect you to learn how chemists obtain the experimental information that underlies chemical theories. These explorations differ from chemical research in that the results that you will obtain are already known. Each of these involves experiments designed to generate data and results of the same sort that chemists obtain when they do research. You may get the idea from your textbook that chemistry is mostly theory. we had several goals. You can learn something about how chemists learn. You can learn some facts and laws of chemistry. When the scientist has enough results. and enough such support causes it to be accepted as a scientific law. You can learn much about chemistry as you carry out these explorations. the hypothesis is supported. a scientific method. 2. we ask you to complete five explorations. There is much theory in chemistry. To check the validity of the hypothesis. l. Still.
A chemistry laboratory is like a freeway -. you must pay attention and ask questions. Every good scientist is an active observer. risks are minimized and the laboratory made as safe as any other work place when everyone uses caution and common sense. For that purpose. in which all significant observations are written down. Form the habit of being an active. To become skilled at observations. every good experimenter keeps a laboratory notebook. particularly when the unknown is being explored. You can learn to work quantitatively. SAFETY IN THE LABORATORY Every good scientist takes appropriate safety precautions. You are expected to know them and obey them whenever you are working on an experiment. Why are we doing this particular procedure? What would be the effect of changing a condition? What might go wrong with the procedure? What is the meaning of the observations? Good laboratory workers are always thinking about what is going on. The following are general safety rules that must always be observed.3.it is safe for all. You can learn some important laboratory techniques. Form the habit of recording every observation that might be important. Form the habit of learning safety rules and living by them. questioning laboratory worker. 5 . Complete records must be kept of all procedures and observations. But just like a freeway. Every good scientist also is a careful record keeper. 4. There are basic safety rules for working in the laboratory that are analogous to traffic laws. Like any other human endeavor that is worth doing. An experiment is no better than the written records of what happened during that experiment. eventually died of cancer brought on by exposure to the radioactivity which they discovered and studied. it can be dangerous for all if anyone ignores the rules. 5. chemistry experiments involve a certain amount of risk. provided all understand and obey the rules. Nevertheless. for example. The Curies. You can learn to think like a scientist. asking questions and modifying their thinking as they go.
immediately inform your instructor. Mercury spills must be carefully cleaned up using a special air suction apparatus. Full goggles must be worn at all times in all chemistry laboratories and when picking up materials at the chemicals stockroom. and not taking anything for granted. A spill on a bench top may look like water but be strong acid. but they can be very dangerous if allowed to contact the wrong materials. -. If you must wear contact lenses. This is particularly true of strong acids and bases and human skin. observing what is going on. KEEP WORK AREAS CLEAN. ALWAYS BE CAREFUL. There is no excuse for not knowing as much as possible before beginning to work. 5. The more you know about the procedures and chemicals you are working with. 4. Read the exploration before coming to the laboratory. Note: this is not a local rule. Just as newborn 6 . the easier it is to avoid accidents. KNOW YOUR EXPERIMENT. Become familiar with a procedure. the worst enemy of safety is carelessness. We strongly recommend that you not wear contact lenses! They readily absorb chemical vapors that can lead to eye irritation and damage without you realizing it. 2. LAB COATS. Along with ignorance. 3. Chemicals become particularly dangerous when we are unaware of what they are. Chemicals used in the laboratory are safe as long as they are kept in their appropriate place.1. or chemical before you do experiments with it. Do not try to recover spilled mercury by yourself. there is a possibility of a mix-up. instrument. If you are unfortunate enough to break a thermometer.which can seriously injure the eyes. Any time you are working with more than one substance of similar appearance. LABEL ALL MATERIALS. but it is vulnerable to injury. etc. State law requires that eye protection must be worn wherever potentially harmful chemicals are stored. Accidents in a chemistry laboratory frequently involve flying materials -. The eye is a marvelous instrument. splintered glass. Always clean up any spilled material immediately. CLOSED SHOES. Care in the laboratory includes staying alert. WEAR SAFETY GOGGLES.splashing liquids. notify your laboratory instructor.
Be sure you know the location of the following. suffer from allergies. If they do happen. WEAR SENSIBLE CLOTHING. but many chemicals can cause adverse reactions for those who are especially sensitive. The chemicals used in General Chemistry are safe for general use. 10. BE AWARE OF SENSITIVITY TO CHEMICALS. long floppy sleeves and the like are invitations for accidents to happen. If you are careful. BEWARE OF FIRES. These are prohibited in the laboratory. If you have long hair. If you must wear fashionable and/or expensive clothing. tie it back on lab days. and how to use them: eye wash safety shower fire extinguisher first aid kit emergency telephones all exits If you get any chemical in your eyes. begin an eye rinse at the eyewash immediately. Eye damage can occur very quickly. or know of any special sensitivity. 6. though. immediately stop what you are doing and consult your instructor. DON'T EAT or DRINK. wear a protective lab coat or apron over it. 7. and (2) before using a flammable solvent to be certain no one has an open flame nearby. Hair very easily catches fire! 8. a quick response may be crucial to avoiding disaster. If you are pregnant. please notify your laboratory instructor or the laboratory coordinator before the beginning of laboratory work. KNOW WHERE SAFETY EQUIPMENT IS. If. High-heeled or open-toed shoes. samples in the laboratory should be uniquely identified. 7 . Too many chemicals are harmful when taken internally for it to be safe to eat or drink in the laboratory. accidents will be very rare. during a laboratory. 9. you experience unusual symptoms such as persistent itching or shortness of breath.babies are given name tags to prevent inadvertent confusion. Chemistry experiments frequently involve the use of open flames for heating. Always check around you (l) before lighting a Bunsen burner to be certain no one is using a volatile flammable solvent such as acetone.
and obnoxious materials in the fume hood. wet the glass with water or glycerol. 8 . Don’t put paper or chemicals in this container! ˚ Solid chemical waste container is for solid waste. ˚ Glass waste container is for glass waste. 5. To minimize waste disposal. Adding water to strong acid can liberate enough heat to boil the solution. Never return excess chemicals to their original container. toxic. Your laboratory procedure describes which container to use for each type of waste that you generate during an exploration. Never push glass into a stopper without protection. When diluting strong acids. Never taste or smell laboratory chemicals. 6. consult your laboratory instructor. Never pipet liquids by mouth suction.In addition to these general rules. Handle volatile. always add the acid to water. 2. causing splattering or "spitting" of hot acid solution in random directions. Discard excess chemicals in the appropriate waste container. 3. Place each kind of waste only in its proper container. follow the procedure and do not take more than is needed. 4. 7. WASTE DISPOSAL There are separate containers for different types of waste. wrap the glass with a towel. l. Never perform unauthorized or unsupervised experiments. Don’t put solids or aqueous solutions in this container! ˚ Aqueous waste container is for aqueous solutions that contain toxic materials. 8. Don’t put glass or liquids in this container! ˚ Non-Halogenated Liquid waste container is for organic liquids such as ethanol and acetone. some specific precautions apply when working in the general chemistry laboratory. Instead. and hold the glass near the stopper. When in doubt. use a rubber pipet bulb. When inserting glass into a stopper. Put nothing in drying ovens unless specifically instructed to.
enter the exploration number and the date. turn in the duplicate copies of your data pages to your laboratory instructor. For example. These notebooks have pages in alternating colors. Type of Notebook: You are required to make duplicate copies of all your notebook pages. Description. The originals should be on the white pages. so your laboratory notebook must produce a duplicate page for each original page. have your instructor date and initial your data pages for that day. becaise it is where you record all observations that you make while doing explorations. your first entry may be described "Preparation of Solution. we expect you to keep a complete notebook. so that it always shows all of the data that have been entered in it. The description should briefly identify the procedure. A good laboratory notebook is organized in a way that makes it easy for you to locate and identify an observation that you made at an earlier date. On the first page of each exploration. Before leaving for the day. Your laboratory notebook is the only place where the observations that you make in the laboratory should be recorded. In the General Chemistry laboratory. This table should have four columns: Date. Exploration number. 9 . Table of Contents: Reserve the first four pages of your notebook for a table of contents. and Page number. duplicates on the yellow or blue pages. Do not record data or observations on stray pieces of paper or in the laboratory manual." Update your table of contents after each laboratory period. Data Pages: At the top of each data page. Instructor Verification: At the end of each laboratory period. be sure to begin with the title of the exploration.THE LABORATORY NOTEBOOK Your laboratory notebook is the most important document in the laboratory. following the rules that are given below.
but an unrecorded observation is lost forever. Be sure to use carbon paper to make a duplicate copy of your data or have a notebook with paper that automatically produces a carbon copy. An observation that turns out not to be important can always be ignored. enter the calculation in your laboratory notebook." Be sure to identify these as opinions by using words like "I think". When you void data." When in doubt.): identify the data fully. include units. etc. Comments and speculations: anything that you think of which may help you in interpreting the data and results can be included as a comment. draw a line through the mistake and write the correct information above or next to the mistake. If a small mistake is made. masses. "It appears"." "Balance #5 had to be re-zeroed before making this weighing. If an entire page needs correcting.Types of Data: You should include the following: Numerical data (temperatures. Special Instructions: Write only on the numbered side of the pages. For example: "When the 2 solutions were mixed. etc." 10 . Write only in ink (ball point pen). Never erase errors. Here are two examples: "The balance was miscalibrated. record an observation. volumes. write an explanation of why it is invalid. Preliminary calculations: when the procedure calls for you to do a calculation before proceeding." "I used the wrong reagent in preparing my solution." Observations: record anything that you notice that might turn out to be important. but I think there were water droplets on the flask walls. a white precipitate formed. "Maybe". draw a large X across the entire page and write VOID in large letters. For example: "This calibration doesn't agree with the first one. and give the correct number of significant figures. For example: "Mass of empty flask and stopper: 27.4586 g.
and a precision. 1. You might look at it and estimate. Precision is the degree of certainty with which a numerical value is known: "about 20 miles" is a much less precise statement than "21. always include all three of these parts. As an example of how this rule works.8 meters. consider measuring the length of a table. This means you are stating that the table is greater than 1. but less than 3. Now you are asserting that the table is longer than l. Consider." The length has been expressed as a one-digit number. "This is a 2-meter table. "This table is more than 1.PRECISION OF MEASUREMENTS Chemistry is a quantitative science. Numerical value is self-evident. unless told otherwise. Most of the time. Of these three parts. Units are what allow us to scale a numerical value appropriately (20 miles is quite different from 20 centimeters).5 miles. Unless otherwise stated. "6") 11 . meaning that you know the table to be longer than 1.827 meters.826 meters.7 but shorter than 1.825 but shorter than 1." After a crude measurement. for example. A measurement with a better measuring device might give you a result of 1. it is understood that the measurement is precise to within one unit in the last significant figure. precision requires further discussion. A very careful measurement with a good tape measure might yield the result. that this result contains three certain figures and one doubtful (the last. a length that is reported as 1. Chemical observations must be expressed as quantitatively as possible. you might be able to state the length more precisely as 1.84 meters long. appropriate units. this statement means.9 meters.83 meters. a chemist wants to know not only what is happening but also to what extent (how much).0 meters long. There are four significant figures and we assume. When recording data in your laboratory notebook and when reporting results in your laboratory reports. Quantitative measurements have three equally important parts: a numerical value. The number of digits in a numerical result is called the number of significant figures. Scientifically speaking.826 meters." Quantitative scientists have established a basic rule for stating the precision of numerical values: the number of digits recorded for the numerical value expresses the precision of the measurement.0.82 meters long but less than 1.
it is hard to tell. SCIENTIFIC NOTATION Scientists commonly work with very large and small quantities. Very sensitive instruments yield measurements of high precision. to express these numbers. can be written as 3.84 x 108 meters.827 meters). Expressing the value in a different unit such as centimeters. How many significant figures does each of these distances contain? As the numbers are written. The diameter of an atom.84 x 10 x 10 x 10 x 10 x 10 x 10 x 10 x 10. an atomic diameter of 0.000 kilometers in the course of a month. Our moon's orbit is not perfectly circular.000 meters.4 ÷ 10 ÷ 10 ÷ 10 ÷ 10 ÷ 12 . is 0. The precision of a measurement depends on the quality of the measuring device used to obtain the measurement. and the average distance of the moon from the Earth is 384. A scientific example of this kind of fluctuation is the distance between the Earth and its moon.figure. This specific measurement is understood to be 1. In our example of the table. for instance. 8 times"): 3.001 meters (i. 182. That looks cumbersome. to lie between 1. Similarly. To eliminate the ambiguity created by zeros needed to locate the decimal point.000. so this distance fluctuates with time.825 meters and 1. because all the extra zeros are needed to locate the decimal points. does not change the number of significant figures (still four). The precision of a measurement can also depend on variations in its value. scientists commonly use a special format. scientific notation. The moon's distance from earth. depending on whether it was measured at a protrusion or an indentation.00000000014 meters.6 cm. and to shorten the writing of small and large numbers. in which case its length would vary by a few centimeters. They have nothing to do with the precision of the number.e. Scientific notation is based on the fact that any number can be expressed as a number between 1 and 10 multiplied or divided by ten an appropriate number of times. 384.000. the table top might be scalloped or fluted. but we can abbreviate the 8 " x 10" 's as 108 (meaning "multiply by 10.000 meters. The analytic balance is the most sensitive instrument that you will use in General Chemistry. varying by about 48.00000000014 meters can be written as 1. but less sensitive instruments yield results of lower precision.826 ± 0.
001 so the computed answer is rounded to a single digit.000. As an illustration. To illustrate these concepts. either relative or absolute precision can be used. The number 3. If a measurement of the thickness gives 0.001 meters. The relative precision is 0.841 x 108 meters.84 x 108 meters means "not less than 3. Notice that while absolute precision has the same units as the measured quantity. or 5 x 10-4.320 meters (3. Each of these ways of looking at precision is important.how big is the uncertainty relative to the value itself).20 x 10-1 m). The precision of a number that is written in scientific notation is unambiguous.10 ÷ 10 ÷ 10 ÷ 10 ÷ 10 ÷ 10." RELATIVE AND ABSOLUTE PRECISION The degree of precision in a given experimental value can be viewed in two different ways: as the absolute precision (how big or small is the uncertainty in the value?) or as the relative precision (what is the fractional uncertainty in the value -.475 x 10-4.826. or 0." Extra zeros now mean extra precision: 3. There are several different ways of expressing relative precision: we can state it as 1/1826. nor more than 3.001/1.015 meters (1.85 x 108 meters. consider the volume and perimeter of the table top whose length we measured earlier. while its relative precision is 1/320. or 0.05% (percent is relative precision x 100). If the table has been measured to be 1. not 5. 5 x 10-4.839 x 108. 0 times": 1 x 100 =1). relative precision is a ratio of two values having the same units and is therefore dimensionless. the absolute precision of the measurement is ±0. nor more than 3. The absolute precision of this width measurement is ± 0. the form of the combination determines which type of precision is more useful. we return to our example of the table length. Suppose we find its width to be 0.5 x 10-2 m).840 x 108 meters means "not less than 3. the 13 . 10 times"). abbreviated as l. but when measurements are combined to compute a result. Note that you only have single digit precision in 0. When you are reporting a measurement. 100 has a specific meaning: "multiply by 10.4 x 10-10 (meaning "divide by 10.001 meters. (Although it is not needed for scientific notation.826 meters long.003 (3 x 10-3). or 5 parts per 10. or 5 x 10-4.83 x 108.
826) + 2(0.7 x10-2): 0.321 meters. Now combine these measurements to determine the perimeter P and the volume V of the table top.76 x 10-3 ± 0.76 x 10-3 meters.067 = ± 0.7 x 10-2). values? The precision of computed results can be found from the precision of individual measurements by considering the largest possible change in each individual measurement. Notice that this is the sum of the absolute precisions of the individual values: 0. Notice that the relative precision for the volume is the sum of the relative precisions of length (5 x 10-4).absolute precision is 0. volume is V = L x W x T = 1. errors will cancel -.003 + 0.826 x 0.015 = 8.292 meters.319 x 0. in the same direction. consider the table's perimeter. How precisely do we know each of these computed. or as small as 1.827) + 2(0. The volume is 8. or as small as 2(1. Applying the same logic to the volume computation.38 x 10-3 cubic meters.001 meters.76 x 10-3 = ± 0.320 x 0. Perimeter is P = L + L + W + W = 2(1.825) + 2(0.004 meters. the length might be as large as 1. but the width is a bit smaller -but we are interested in how precisely we know the perimeter.827 meters.014 = 8. but this procedure is tedious.827 x 0.62 x 10-3/8.001 = ± 0. or there is a relative imprecision of 0. For multiplication and division. The absolute precision in the perimeter is ± 0.321 x 0. 14 . or as small as 1. we find that it might be as large as 1. According to the precision of the length measurement.071.067 (or 6. For addition and subtraction.319) = 4.the length may be a bit larger than measured.001 + 0. the relative precision of the result is the sum of the relative precisions of the individual values.288 meters.296 meters.071 The precision of a composite result can always be determined by the type of analysis described above. First.15 x 10-3 cubic meters. In the worst case. Some of the time. width (3 x10-3) and thickness (6.320) = 4.321) = 4. Fortunately the outcome is always the same. both measurements are off by the maximum amount. so we will assume the worst case.62 x 10-3 cubic meters. The width might be 0.004.319 meters. or derived. Then the perimeter could be as large as 2(1. or 0.825 meters.0005 + 0.016 = 9.001 + 0. and the relative precision is 1/15 or 0. the absolute precision of the result is the sum of the absolute precisions of the individual values.001 + 0.825 x 0.
Another example will illustrate the application of these rules for precision. A student, asked to determine the density of a non-volatile unknown liquid, filled a 25-mL graduate cylinder until it contained 25.0 mL of liquid. The full cylinder weighed 47.5764 g. Using an eye-dropper, the student carefully removed liquid until the cylinder contained 20.0 mL of liquid, whereupon it weighed 43.0464 g. Consider the various quantities involved in this example. Table I-1 summarizes the measurements, computations, and precisions. The absolute precision of each measured quantity is found directly from the measurement, and the relative precision is the absolute precision divided by the measured value. The precision of each computed quantity is determined by adding the appropriate precisions (absolute or relative) of quantities used in the calculation. The computed precision values in bold face are the ones that we find directly from the measured data, while the other computed precision values are obtained from the bold face values and the value of the quantity.
TABLE I-1: MEASURED AND DERIVED QUANTITIES AND PRECISIONS
QUANTITY initial Cyl. Vol initial Cyl. mass final Cyl. Vol final Cyl. mass MEASURED QUANTITIES VALUE ABS. PRECISION 25.0 mL 0.1 mL 47.5764 g 0.0001 g 20.0 mL 0.1 mL 43.0464 g 0.0001 g REL. PRECISION 1/250 1/475,000 1/200 1/430,000
QUANTITY vol. transferred mass transferred liquid density VALUE 5.0 mL 4.5300 g 0.9060 g/mL
QUANTITIES ABS. PRECISION 0.2 mL 0.0002 g 0.04 g/mL REL. PRECISION 2/50 = 1/25 1/20,000 1/25 = 0.04
Specifically, the volume transferred is obtained by subtracting two volumes, so its absolute precision is the sum of absolute precisions of the volumes. The mass transferred is obtained by subtracting two masses, so its absolute precision is the sum of absolute precisions of the two masses. The relative precision for each of these measurements is then obtained from the values of their absolute precision. The density is obtained by dividing mass by volume, so its relative precision is the sum of relative precisions of transferred mass and transferred volume. The sum of 1/25 and 1/20000 is 1/24.9687, which rounds to 1/25 or 0.04. After we find the relative precision of the density, we use it to compute the absolute precision. The absolute precision of the density is (1/25) x (0.9060 g/mL) = ± 0.04 g/mL. The direct calculation of the maximum and minimum density values again shows the validity of using the shortcut method to find the precision of the calculated result.
In the above example, the density might be as large as 0.944 g/mL or as small as 0.871 g/mL. It is incorrect to write it as 0.9060 g/mL, which implies that it is known to 0.0001 g/mL. In such cases, the result is rounded off -- non-significant figures are eliminated. Because the uncertainty in the density is in the second decimal place, this result is rounded off to two decimals: 0.91 g/mL. We have still overstated the precision, because 0.91 g/mL implies a precision of 0.01, while the actual precision is 0.04.
Rounding off one more place and giving the density as 0.9 g/mL would imply an uncertainty of 0.1, which is larger than the actual uncertainty. The convention is to round off until dropping one more digit would result in an uncertainty larger than the actual uncertainty. When the digit following the last significant digit is 5 or greater, the remaining digit is increased by one unit: 0.9060 becomes 0.91. If the digit following the last significant digit is less than 5, the remaining digit remains unchanged: 0.9045 rounded to 2 significant figures is 0.90.
Shortcuts to Precision
Chemists want to spend minimum time determining precision. Every time a chemist makes a measurement, precision and significant figures are a concern, but chemists are more interested in what experiments reveal than they are in significant figures. The first question, then, is "How important is precision for this particular experiment?" An analytical chemist, for example, might be interested in determining the level of a particular carcinogen in a sample of ground water. If the carcinogen is present at only about 1 part per billion, the precision of the measurement must be very carefully stated. On the other hand, a synthetic chemist whose goal is to synthesize new compounds is primarily interested in putting the substance in a bottle. The quantitative yield is important (the higher the yield, the less expensive the product will be), but precise values for this yield are not. When quantitative values are being reported, but their exact values are less important than the qualitative results, the detailed treatment of precision is not needed. Instead, we can use a simple system to determine the appropriate number of significant figures: 1. To determine the number of significant figures in an individual measurement, read the number from left to right, counting all the digits starting with the first one that is non-zero. 300. 3 sig. figs.
3 sig. Calculators do not necessarily give results with the correct number of significant figures. 1.020 3 sig. 5 sig.0) has a relative precision of 1/30.00 and 5. 2 sig. The divisor (3.00 on your calculator). 2 decimal places 1 decimal place 3 decimal places 1 decimal place Sum: 3. (But don't spend a lot of time worrying about it: either way of reporting is legitimate! What is not legitimate is to report this result as 1. Even when a calculator is programmed to report a particular 18 . figs.19665.1. if its importance is in its qualitative significance.0 2 = 1. 2 sig. 2. When adding or subtracting. They automatically drop trailing zeroes even when they are significant (try multiplying or adding 3. figs. so the result could be stated more precisely than this: the result. The number of significant figures is not relevant: 0. figs.00 0.490 13.2.20 (1 part in 120) rather than to 1. figs.365 significant figures: 4 x 2. figs. When multiplying or dividing.2 (1 part in 12).20 would be the more appropriate number to report. could be rounded to 1.) 4.12 1. The number of decimal places is not relevant: 1. figs.6 11.00 on your calculator) and they may carry extra decimal places even when they are not significant (try dividing 5. report 1. the number of significant figures in the answer should be the same as that of the quantity with the fewest significant figures:.2 2 sig. 1.00 by 3. the number of decimal places in the answer should be equal to the number of decimal places in the number with the fewest places. If the importance of the result is its quantitative value.19665.2 2 The above example is one where the simplified procedure gives a different result than the more elaborate one.63 3 / 3.
number of digits. Never believe the number of significant figures on your calculator! 19 . that number of digits may not be the correct number of significant figures.
the buret has a line for every 0. called the meniscus. The graduated cylinder in the figure has a larger diameter than the buret. and we can estimate with an absolute precision of 0. A reading always is more precise than the scale markings.9 mL.34 mL. As examples. A liquid in any cylindrical container has a curved surface. as the figure shows. and the beaker contains 37 ± 2 mL The absolute precision of our measurement depends on the diameter and markings on the container.01 mL. In the figure. the gradiated cylinder contains 30. is the position that we read. so the absolute precision is 0. Figure I1: Examples of volume measurements. and its markings are every 1 mL.0 mL.1 or less than 29. The lowest point on the curved surface. but we can estimate that it is not more than 30. 37 mL.0 mL. We can never read that position exactly but must always estimate it as closely as possible. consider the three volume measurements illustrated in Figure I-1. The buret reading is 33.” This indicates that 20 . The buret reading in Figure I1 is 33.Precision in Volume Measurements Volume measurements illustrate both absolute and relative precision.1 mL and we record a volume of 30.34 mL. because we can estimate the distance of the meniscus from the nearest mark. This graduated cylinder is filled to the 30 mL line. We can estimate the volume of liquid in the 50 mL beaker to the nearest 1 mL.1 mL. but notice that the beaker is marked “±5%.
0 or 0. the uncertainty may be larger than ±1 in the last digit to the right.0 mL. The relative precision of a 30.8255 g for the mass of the same beaker. because the "true" mass may have any value between these two measurements. as the amount of liquid in the cylinder changes. two balances may read 35. For example. Mass measurements using an analytic balance are more precise than volume measurements using burets. The absolute precision of a volume measurement in the graduated cylinder shown in the figure is ±0. Precision in Mass Measurements The most precise mass measuring device in the introductory chemistry laboratories is the electronic analytic balance. whether the volume is 30. In this case. the relative precision would be 0. ACCURACY AND ERROR Our discussion so far has concentrated on the precision of numerical results. To be sure of the precision of a digital readout.0001 g using an analytic balance. If the graduated cylinder were filled.the lines marked on the beaker are only reliable by this amount.8252 g and 35.0003 g.1/100.0001 gram (0. a relative precision of 3 x 10-4.003. which is the uncertainty in the numerical value. This balance reads mass digitally with an absolute precision of 0. on the other hand. when a digitally reporting instrument displays a particular number of digits. we conclude that the precision of the balances is ± 0.0 mL or 100. preferably using different instruments. the accuracy of a result is even more important because the accuracy indicates how close the result is to the actual or true value.0 mL volume is 0. we should report this volume as 37 ±2 mL.1/30. This is a relative precision of 3 x 10-6 .0 or 0001. Because 5% of 37 mL is 2 mL. we must measure the same object several times.1 mg). however.01 mL using a buret. The relative precision changes. 100 times more precise than the volume measurement.1 mL. 21 . Although precision is very important in quantitative scientific work. You can measure the volume of 35 mL of water to ± 0. but you can measure the mass of the same amount of water (about 35 g) to ± 0. However.
It's not easy. On closer inspection. Gauge 2 was on the downwind side of the house and therefore had been protected from the rain.78 mm. and Gauge 3. RE = (M − T ) T Think about how scientists can be sure of the true value of any quantity. Although it is almost always necessary to measure with great precision in order to achieve accuracy. A supposedly dry sample that contains some water will have an erroneously high mass. Gauge 1. Like precision. In chemistry experiments. bought 3 precise rain gauges.78 mm. You should always be alert to the possibility of such errors and do your best to avoid or minimize them. because every experimental measurement is subject to error. they cannot all be accurate. will have an erroneously low mass. Gauge 2.01 mm.45 mm. registered 7. outside his bedroom. some of which has been accidentally lost. An everyday example will illustrate this point.Absolute error (E) is defined to be the difference between the measured (M) and the true (T) values. A pressure reading thought to be of only one gas may actually be the total pressure of more than one gas. He installed two on different sides of his house and one on a fence post beside his fields. on the fence post in the open. E=M-T Absolute error can be either positive or negative. concerned about whether his crops were receiving enough rainfall.65 mm. registered 17. mistakes in what is measured can cause precise measurements to be in error. outside his kitchen. precise measurements may not be accurate. the farmer found that Gauge l was just at the edge of his roof and had been collecting a significant amount of roof runoff. he read each gauge. on the fence post. each capable of registering rainfall to 0. registered 55. Relative error (RE) is the ratio of the absolute error to the correct value. 22 . Only Gauge 3. A sample. error can be expressed either as absolute or relative. After the next rainfall. Although each of these readings was precise to 0.01 mm. was both precise and accurate: the true rainfall was 17. and the usual way of discovering errors is by comparison with a "better" or "truer" value. A farmer. particularly if what is actually measured differs for some reason from what it is intended to measure.
e. which you will be asked to calculate in several of the reports for Chemistry 120A: RAD = ∑ Drel N The average deviation and relative average deviation are good measures of precision. always positive) of the difference between the value and the average. In such replications of experiments. we obtain the relative deviation.the Greek capital letter sigma . The farmer has bought a fourth rain gauge (being skeptical of all of them) and has installed one at each corner of his field.A| This is the absolute deviation. The average value (A) is the sum of all individual values divided by the number of values (N): A= ∑M N (The symbol ∑ .AVERAGING One way to avoid accidental mistakes in measurement is to repeat an experiment several times and then report the average of several measurements as the most reliable result. If we divide an absolute deviation by the measured value. because they reflect the uncertainty in a whole set of measurements. Drel: Drel = D M We can average a set of deviations to obtain an average deviation (Dav): Dav = ∑D N The average of the relative deviations is the Relative Average Deviation. We return to our (now wiser) farmer friend for an example of these concepts.means "add up all the individual values of"). RAD. 23 . D = |M . he checks all four gauges. After the next storm. The deviation (D) of each individual value is the absolute value (i. in addition to precision and error we can also define the average or mean value and the deviation of individual values from this average value.
54 242.10 Relative Deviation 103(|M-A|)/A Parts per 1000 (ppt) 1.04 0.32 60. exclude the result (Remember the farmer's first placement of his rain gauges. and 60. Table I-2 summarizes the measurements and their deviations from the average. one result deviates greatly from the other results. each relative deviation is rounded off to 2 significant figures. however. Table I-2 Deviations in Measured Rainfall Gauge Units: 1 2 3 4 Sum Average Reading mm 60.58 Absolute Deviation |M-A| mm 0.52.10 0. Then the deviation 24 .0 1. STATISTICAL ANALYSIS: THE RULE OF FOUR Sometimes.10 mm.finding readings of 60. 60.78.54 mm. a statistical test can be applied to find out whether the result should be retained or rejected.6 1. the cause of a large deviation is not known.6 The average absolute deviation is 0. The average (mean) value is calculated without including the value which deviates the most.52 60. If the large deviation is due to known experimental error.6 3.20 0.78 60. In such a case.06 0.3 0. and the average deviation is computed for the set without this value.40 0. and the average relative deviation is 0.48 60.01 mm out of about 0.7 6. in a set of measurements. The easiest test is the "Rule of Four".6 ppt (parts per thousand).1 mm).0016 or 1.) Many times. Because the absolute deviations are only precise to about 1 part in 10 (0.16%. the set must include at least four values.48. 60. For the Rule of Four to be valid. or 0.
is more than four times that. and the deviation of the Gauge 3 reading.07 0. its exclusion is statistically valid.02 mm.02 0. This gives the results shown in Table I-3: Table I-3 Adjusted Rainfall Deviations Gauge Units 1 2 4 Sum Average 3 Reading mm 60. if its deviation is less than four times the average deviation. and the mean value and average deviations must be obtained for the entire set.51 ± 0. 0. Conversely.52 60.48 60.27 The average deviation of the three remaining values is only 0. we are justified in rejecting the Gauge 3 reading and reporting the rainfall as 60.78 Absolute Deviation mm 0.02 mm.54 181. that from Gauge 3.51 60.01 0. if it is greater than four times the average deviation. 25 . the result must be included in the set as a valid measurement. we temporarily exclude the reading with the highest deviation.54 60.03 0.of the excluded value is evaluated.27 mm. Applying the Rule of Four to the data in Table I-2. On statistical grounds.03 0.
We can theorize all we like. Is volume conserved? This question must be answered by experiments. Bathroom scales measure mass. for more details about measurements and density. you already know something about how to measure them. but all the concepts described in a textbook are based on observations and experiments done by generations of chemists. Some of these laws involve conservation.6. We say that mass is conserved. INTRODUCTION Consult your textbook. To explore volume conservation. you need to measure masses and volumes with higher accuracy than everyday measuring devices allow. you will learn how to make quantitative measurements of both mass and volume. Chemistry textbooks describe theories that predict behavior. This is an example of a conservation law. mass is conserved. Usually. In this exploration. How about volume? Your objective in this exploration is to determine whether volume is conserved. when two liquids are mixed together. Because mass and volume are everyday properties. and measuring cups measure volume. however. but no theory will tell us what actually exists in nature. Sections 1. you will learn to 26 . To determine this. In other words. You will explore whether volume is also conserved.EXPLORATION A1 IS VOLUME CONSERVED? OBJECTIVES Science is built on sets of general laws. You probably already know one of the fundamental laws of nature having to do with mass: mass is neither created nor destroyed in physical or chemical processes. Energy is conserved. is the new volume always equal to the sum of the volumes of the individual samples? In order to study any property like mass or volume. we must have techniques for making quantitative measurements.5 and 1.
0001 g (0. Analytic balances are more versatile than volumetric glassware. which contain known volumes of liquid. it contains a known volume of liquid. Whereas a bathroom scale measures mass only to the nearest half-pound. and volumetric pipets. provided that temperature does not change. while volumetric glassware measures volumes accurately. For volumes other than the fixed volume.1 mg). Volumetric glassware and measuring cups both work by measuring height. it is more convenient to measure mass and find a way to convert to volume. In the case of volumetric glassware. given by the equation. a quality analytic balance can measure to 0. they allow the measurement of volumes with high precision and accuracy. we always fill to some prescribed mark. provided we know the proportionality. can accurately and precisely measure just one fixed volume. we fill "to the brim" or to a mark etched on the cup. so force measurements can be converted to masses. because the analytic balance measures masses over a continuous range with high precision and accuracy.use precision scientific tools for measuring mass and volume. Force is directly proportional to mass (f = ma). by measuring the amount of gravitational force that a mass exerts. so it will be convenient to measure masses in grams and volumes in milliliters. In the case of measuring cups. Bathroom scales and analytic balances both work by weighing . Each has been carefully manufactured so that when full. 1 pound = 454 g and 1 mg = 0. Nonetheless. An analytic balance measures masses with high accuracy.that is. This ratio is defined to be the density d. You will use two types of such glassware: volumetric flasks. Experiments have shown that the ratio of mass to volume of any pure liquid or solid is a constant. which deliver known volumes of liquid. 27 . Using the conversions.001 g (10-3 g). Each volumetric flask and volumetric pipet. m d= Equation A1-1 V Density commonly is expressed in units of g/mL or g/cm3 (1 mL = 1 cm3). we can see that an analytic balance is over 2 million times more precise than a bathroom scale. Each of these is very simple: it is nothing more than a piece of glassware with a line scribed on it. in contrast. Density provides a connection between mass and volume.
Water is the most convenient liquid to use for such measurements. you are taring the scale). If you weigh a container filled with a liquid of known density. When this is done. you can weigh a sample of known volume. mobject = m2 . To apply Equation A1-2.Equation A1-1 links three quantities. then calculate density using Equation A1-1. Taring sets m1 = 0. It is inexpensive. To determine density. 28 . When you weigh an object. as Figure A1-1 (next page) shows. you compare the gravitational force on the balance pan plus the object to the force on the balance pan alone. however. you can use mass measurements and Equation A1-2 to determine the volume of any particular container. we must measure the temperature as well as the mass. non-toxic. you can use a rearranged version of Equation A1-1 to calculate the volume: V= m d Equation A1-2 Accurate mass determinations actually involve two mass measurements. you compare the mass of a container filled with liquid to the mass of the empty container. and its density has been very accurately measured. because the density of water varies slightly with temperature. This is called taring the balance. To obtain the mass of a liquid sample. If the density of a liquid is accurately known.0 = m2 Equation A1-2 provides a way of determining volume to high precision. If you know any two of these three quantities.m1 = m2 . you can calculate the third.m1 Many analytic balances permit the mass reading to be pre-set to read zero for the comparison mass. giving mobject = m2 . the second mass reading gives the mass of the object directly (When you zero a bathroom scale before stepping on it.
Part E: Quantitatively determine whether liquid volumes are conserved.999 Density (g/mL) 0.996 0.995 5 10 15 20 Temperature (˚C) 25 30 35 Figure A1-1: Density of water as a function of temperature SEQUENCE OF EXPERIMENTS Part A: Estimate whether liquid volumes are conserved.997 0. Part D: Determine precisely the density of an Unknown liquid. 29 .1 0.998 0. Part B: Calibrate a 10-mL Volumetric Flask to determine its precise volume. Part C: Calibrate a 5-mL Transfer Pipet to determine the precise volume it delivers.
add another 5. Invert them in a 250mL beaker containing a paper towel and allow them to drain. and then discard the acetone in the acetone waste bottle. Once you have clean glassware. Dry the inside by inserting a Pasteur pipet attached to the house vacuum and drawing air through until the glassware is dry. Again using your wash bottle.0 mL of deionized water to your 10-mL graduated cylinder.0 mL of deionized water to your 10-mL graduated cylinder. because none of the liquids contaminates glassware. and then read and record the total volume. stir thoroughly with your metal spatula. add 5. 30 . clean it by washing with soap and water.) Using your wash bottle. Do not blow air through the glassware. Discard the water in the graduated cylinder. Pour this liquid into the clean test tube. 3. then rinsing thoroughly with tap water. add 5. Dry the outside of the glassware with a paper towel. and then pour it into the clean test tube. Pour the water from the test tube back into your 10-mL graduated cylinder.0 mL of deionized water to your 10-mL graduated cylinder. you need not clean it again during this exploration. 2.) Clean your 10-mL graduated cylinder and one test tube. add 2-3 mL of acetone to the clean glassware.) Again. because compressed air contains oil droplets that will contaminate the glassware! Part A: Preliminary Study of Volume Conservation 1. Drying: When the procedure calls for dry glassware.PROCEDURE Precaution: no open flames are permitted during this experiment! Cleaning: The first time you use a piece of glassware. Rinse your metal spatula with deionized water. and finally rinsing with about 5 mL of deionized water from your wash bottle. swirl to wet all surfaces.
) Does it appear to you that volume is conserved when the same liquids are mixed? When different liquids are mixed? Part B: Volumetric Flask Calibration The quantitative determination of whether volume changes when two different liquids are mixed requires the calibration of a volumetric flask (Part B) and a pipet (Part C).) Clean and dry a 10-mL volumetric flask and stopper. Rinse your 10-mL graduated cylinder with about 3 mL of acetone. 1.4. and then read and record the total volume.) Now add 5. swirl to wet all the surfaces. 2. After drying. then discard the liquid in the acetone waste bottle. 5. and give your reasoning. Let it stand so that its temperature will equilibrate with that of the lab.) Place about 11 mL of deionized water in your clean 10-mL graduated cylinder. 31 . stir the liquid mixture thoroughly with your metal spatula.) Answer the same questions when two different liquids (water and acetone) are mixed. Discard this liquid in the waste bottle marked "acetone waste. 3.) Obtain an acetone wash bottle. Record this mass. A.) Zero an electronic analytic balance.) When you mixed two volumes of the same liquid (water) was the resulting volume close to or equal to the sum of the two volumes? B. handle them only with a paper towel or Kimwipe. D. Add the water from the test tube to the acetone in the graduated cylinder. and then weigh the stoppered flask to the nearest 0. Note: Comments should appear on both the original and the carbon copy of your notebook pages.1 mg)." Answer the following questions as comments in your notebook.0001 g (0.0 mL of acetone to your 10-mL graduated cylinder. Do not handle the flask any more than is necessary. because oil from your hands can change the mass of the flask.) Is the sum of the two volumes within the range of uncertainty with which you can read volume using the 10 mL graduated cylinder? C.
fill the flask with deionized water until the bottom of the meniscus is exactly even with the mark. 32 . Fill a 250-mL beaker with about 200 mL of deionized water.1 mg. and invert it on a paper towel to allow it to drain.) Stopper the flask and reweigh to the nearest 0. 6. Rinse with acetone and draw a vacuum through it using a Pasteur pipet.) Repeat steps 1-6 four more times to obtain five sets of data.) Clean a 50-mL Erlenmeyer flask. Adjust the water level with the Pasteur pipet. temperature of the water to the nearest 0.) Return the sample to the graduated cylinder. Part C: Pipet Calibration Note: The upper limit of electronic balances is 105 g.) Using a Pasteur pipet and rubber bulb. 1. using the same balance as for the weighing in step 2. Note: It is essential that you dry your volumetric flask for each trial. being careful that no water droplets adhere to the walls of the flask above the mark Figure A1-2: Proper location of liquid level when a volumetric container has been correctly filled to the mark. wipe the outside dry. DO NOT BLOW HOUSE AIR INTO THE FLASK.5. (See Figure A1-2). Measure and record the 7.5 oC. Handle the flask with a paper towel or Kimwipe to prevent fingerprints. 5.
If drops still adhere. Measure and record the temperature of the water in the 250-mL beaker. otherwise your data will be neither accurate nor precise. The water should drain without leaving drops on the pipet walls. It will include an unknown liquid for Experiment A1. using the same balance for this and subsequent weighings. Using your 5-mL transfer pipet. 3. Carry out steps 1-6 of procedure B using your unknown liquid instead of deionized water. add another 5 mL of deionized water to the Erlenmeyer flask and then weigh it. recording the water temperature and weighing after each addition. deionized water (3 times).) You can deliver very precisely the same volume each time if you master pipetting. acetone (once).1 mg.) Dry your 10-mL graduated cylinder. Use this liquid in the following procedure and in Part E. Part D: Density of an Unknown Liquid 1. seal it with your fingers at both ends.) Clean your 5-mL pipet. and shake. but reproducibly delivering the same volume requires practice. let it drain by gravity (do not shake or blow out the liquid). Repeat with three additional samples of deionized water. Use your fingertip to control the pipet as you drain it to the mark while holding it vertical. After a minute.) Obtain from the solutions stockroom (SLC-242) a yellow box containing your unknowns for the semester. and deionized water (3 times).) Weigh your clean 50-mL Erlenmeyer flask to the nearest 0. Consult your instructor to determine how to clean your pipet with NOCHROMIX. drain the pipet (do not blow). Return the liquid to the graduated cylinder after each 33 . Use a pipet bulb to draw water from the 250mL beaker into the pipet until the level is above the pipet mark.) Measure and record the temperature of the water in the 250-mL beaker. This is the first calibration of the pipet. Once the pipet is at the mark. Repeat the process. Using the same pipet. 4. Fill it about 1/2 full with soapy water.2. Then rinse the pipet with tap water (3 times).1 mg. Weigh it again to the nearest 0. 2. so the flask should contain 25 mL of deionized water. transfer a 5 mL sample of deionized water to this flask. This gives a total of five additions. 5.
Then reweigh the flask and record the mass. 5. allow it to stand for 2-3 minutes and then observe the liquid level in the flask.) Repeat step 3 until the liquid level remains at the line after mixing and standing. add a 5 mL sample of deionized water to the volumetric flask. repeat again to obtain a third set of data. The liquids used in this procedure are organic materials that are injurious to the biosphere. Fill your 50-mL beaker about half full of deionized water. repeat the procedure once more. Do not pour them down the sink! Part E: Additivity of Volumes 1. invert it several times to mix thoroughly. Using a Pasteur pipet and rubber bulb.) Discard the liquid in your volumetric flask and any liquid remaining in the 10mL graduated cylinder in the Organic Liquid Waste container. 2. From the mass differences and the calibrated volume of your 10-mL volumetric flask. to four significant figures.) Transfer about 11 mL of your unknown liquid into your 10-mL graduated cylinder.) Stopper the flask. Repeat Part E to obtain a second set of data. 3. Repeat the procedure three times. 34 . Using a Pasteur pipet and rubber bulb. Using your 5-mL transfer pipet.1 mg.) Clean and dry your 10-mL graduated cylinder and 10-mL volumetric flask. 3. 4.) Discard this liquid mixture in the waste bottle labeled "Non-Halogenated Liquid Waste". add additional unknown liquid until the liquid level is again at the line. calculate the density of the unknown liquid. If the results from the two sets of data do not agree. Stopper and weigh to the nearest 0. add the unknown liquid to the volumetric flask until the meniscus coincides with the line. It is essential to dry your volumetric flask at the start of each trial.trial. If your three results do not agree to within 1%.
CALCULATIONS Calculations for Part B: as follows: Compute the mass of water in the flask for each trial mwater = mfull flask . Dev. Absolute Deviation = Vflask .. and you can read the density of water to 0. Read the density from the graph to the correct number of significant figures. You measured 5 the mass of water with an accuracy of 0. Use this average value in all calculations that call for the volume of your volumetric flask. 23-24) to discard any volume that is not statistically valid.mempty flask Use the water temperature and Figure A1-1 to find the density of water at this temperature... calculate the average deviation and relative average deviation (RAD). so each calculated volume should be reported with a precision of 1 part in 104..trial 2 + . average = (Vtrial 1 + Vtrial 2 + . Dev. ) Number of trials Relative Average Deviation = (Rel. These deviations are a measure of the uncertainty of the volume determinations.. ) Number of trials Use the rule of four (pp. Calculate the average volume of your experimental values.. Use the mass of the water and its density to compute the volume of the flask. Vflask.1 mg out of 10 g (1 part in 10 ). average Relative Deviation = Absolute Deviation Average Volume Also. Average Deviation = (Deviationtrial 1 + Deviationtrial 2 + ...trial 1 + Rel.. Vflask = mwater dwater Record this result with the correct number of significant figures. ) Number of trials Determine and report the absolute deviation and relative deviation of each measurement.Vflask..0001 g/mL (1 part in 104). Calculate the average volume from the statistically valid data... 35 .
the average deviation.. mwater = mflask. Use this statistically valid average value in all calculations that call for the volume of your 5-mL transfer pipet. You will have five separate values.. the absolute and relative deviations of the individual results.mflask. Calculate the average volume of your pipet using all statistically valid data. prior to adding 5 mL Use the water temperature and Figure A1-1 to find the density of the water at this temperature. The volume of water is equal to the calibrated 36 . with 5 mL added . compute the mass of water delivered by the pipet.. Compute the average volume delivered and the deviation of each individual value from this average. and the RAD. Read the graph to the correct number of significant figures and record the density reading in your notebook. Calculations for Procedure D: Compute the density of your liquid from the mass data and the average flask volume from calculation B: mliquid = mfull flask . 34). Vpipet. Vtrial 1 + Vtrial 2 + . Calculations for Procedure E: The calculation of volume change on mixing uses the results of earlier calculations. For each addition of water in part C. average = Number of trials ( ) Also determine and report the absolute deviation and the relative deviation of each measurement as well as the relative average deviation (see p. average Calculate and report the average of your determinations.. Use the rule of four (pp. Take the average of your experimental values. Use the mass and density to calculate the volume delivered by the pipet: Vpipet = mwater dwater Calculate the pipet volume to the correct number of significant figures.Calculations for Procedure C: Calculate the pipet volume for each trial. 23-24) to discard any statistically invalid measurements.mempty flask dliquid = mliquid Vflask.
change ∆Vmix is the volume of the flask minus the initial volume: ∆Vmix = Vflask. convert your result to percent change: % change = 100% ΔVmix Vflask. 4 points. 6 points. (Could your experiments be in error? By how much?) DATA AND CALCULATIONS: Construct and print out an Excel spreadsheet organized according to the data sheets that appear on the following pages.Vinitial After computing ∆Vmix. state your conclusions concerning the conservation of volume. REPORT RESULTS REPORTING FORM: Attach a completed copy of the form in the Appendix. which you calculated in part D: m − mE1 Vliquid = E4 dliquid The initial volume is the sum of these two volumes: The final volume is the volume of your volumetric flask. QUALITY OF RESULTS: There are 20 results points in this experiment: calibration of the volumetric flask. the volume Report ∆Vmix and the percentage change with the correct number of significant figures. and state how reliable you think your conclusion is. The volume of your unknown liquid is found from the mass difference between step E1 and E4 and the density of your liquid. and volume change on mixing. calibration of the pipet. describe the evidence that leads you to these conclusions. average . WRITTEN NARRATIVE: In no more than one typewritten page. 37 . 6 points. 4 points. average Vinitial = Vpipet + Vliquid Thus.volume of your transfer pipet. density of the unknown liquid.
EXPLORATION A1 – IS VOLUME CONSERVED? DATA AND RESULTS SHEETS PART B – CALIBRATION OF THE VOLUMETRIC FLASK Trial mass (flask empty) mass (flask & water) mass (water) ____ ____ 1 ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ 2 ____ ____ ____ ____ ____ ____ 3 ____ ____ 4 ____ ____ ____ ____ ____ ____ 5 ____ ____ ____ ____ ____ ____ water temperature (oC) water density (from graph) ____ flask volume average flask volume absolute deviation average absolute deviation relative deviation ____ relative average deviation (RAD) average flask volume from statistically valid data 38 .
PART C – CALIBRATION OF THE PIPET Trial mass (before addition) mass (after addition) mass (water added) water temperature (oC) 1 ____ ____ ____ ____ 2 ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ 3 ____ ____ ____ ____ ____ ____ 4 ____ ____ ____ ____ ____ ____ 5 ____ ____ ____ ____ ____ ____ water density (from graph) ____ pipet volume average pipet volume absolute deviation ____ average absolute deviation ____ relative deviation ____ ____ ____ ____ ____ ____ ____ relative average deviation (RAD) average pipet volume from statistically valid data 39 .
PART D – DENSITY OF AN UNKNOWN LIQUID Trial 1 2 ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ ____ 3 ____ ____ ____ 4 ____ ____ ____ 5 ____ ____ ____ mass (flask empty) ____ mass (flask + unknown) mass (unknown liquid) average flask volume from part B density of unknown liquid ____ average density of unknown liquid absolute deviation average absolute deviation relative deviation ____ relative average deviation (RAD) average density of unknown liquid from statistically valid data 40 .
from B) ∆Vmix average ∆Vmix percent change average percent change _____ _____ 41 .PART E – DETERMINING IF VOLUME IS CONSERVED Trial mass (flask + 5 mL water) _____ _____ 1 ______ ______ ______ _____ ______ _____ _____ _____ ______ ______ ______ ______ ______ ______ ______ ______ ______ ______ 2 ______ ______ ______ 3 mass (flask + water + unknown liquid) mass (unknown liquid) _____ average density of unknown liquid (from D) volume of unknown liquid average pipet volume (from C) initial volume (water + unknown liquid) final volume (average V of flask.
by preparing a precisely known volume of solution containing a precisely weighed amount of a compound of known purity. such as a change in the color of an indicator. Instead. The objectives are to learn how to make accurate quantitative chemical measurements and carry out acid-base analysis with an accuracy of better than 0. the end point is also the stoichiometric point. hydroxide ions (OH-) react with acidic hydrogen atoms. The end point of a titration is the point when there is an abrupt change in some property of the reaction system. for more details about acid-base reactions and the technique of titration.5%. In the titration of an acid by a strong base.6. In a good titration. When this is not convenient. A buret is used to deliver and measure the standard solution. we measure mass (m) and volume (V).EXPLORATION A4 EQUIVALENT MASS OF AN ACID OBJECTIVES The mole is the currency of chemistry. You will standardize a solution and use that solution to analyze an unknown substance. In this exploration. A standard solution may be prepared directly. One important way to do this uses chemical reactions that proceed quantitatively. At the stoichiometric point. Section 4. The point of a titration at which exactly enough titrant has been added is the stoichiometric point. n hydroxide ion = n acidic hydrogen We do not measure amounts of moles (n) directly. In titration. The molar mass (MM) and concentration (M) provide connections between these measured quantitites and the amount in moles: 42 . you will make use of acid-base neutralization and its quantitative measurement by means of titration. INTRODUCTION Refer to your textbook. the amount of a substance in a sample is determined by measuring the volume of a solution of known concentration (the standard solution) required to react completely with the substance. the moles n of hydroxide added exactly equals the moles n of acidic hydrogen atoms initially present. and chemists often have to analyze substances using mole calculations. standardization can be done by titrating a precisely weighed amount of a compound of known purity with the solution that is to be standardized.
Suppose that titration of a known mass (macid) of an acidic substance with a solution of strong base of known concentration (Mbase) requires volume Vbase to reach the stoichiometric point. one mole of sulfuric acid. The equivalent mass of an acid is related to the molar mass through the number of acidic hydrogen atoms that the acid contains: EM = MM # of acidic H Here are two examples illustrating the concept of equivalent mass.(aq) + 2 H2O (l) Each oxalic acid molecule contains two acidic hydrogen atoms. without knowing how many acidic hydrogen atoms an unknown substance contains. We define a new quantity. so the equality at the stoichiometric point is: n hydroxide ion = n acidic hydrogen Mbase Vbase = macid EM acid Equation A4-1 Rearranging gives an expression for the equivalent mass in terms of measured quantities: 43 . Whereas one mole of HCl will consume one mole of hydroxide ions. so one mole of this acid reacts with one mole of hydroxide ion.(aq) → CH3CO2. The equivalent mass of CH3CO2H is numerically the same as its molar mass: EM = 60 g / mol MM = = 60 g/eq # of acidic H 1 eq/ mol 2) reaction of oxalic acid with hydroxide ions: H2C2O4(aq) + 2 OH. so one mole of oxalic acid reacts with two moles of hydroxide ions.(aq) + H2O (l) Each acetic acid molecule contains one acidic hydrogen atom. The number of moles of acidic hydrogen atoms is the mass of acid divided by the equivalent mass. 1) reaction of acetic acid with hydroxide ions: CH3CO2H (aq) + OH.(aq) → C2O42. will consume two moles of hydroxide ions.n= m MM and n= MV One mole of a substance may generate one or more moles of hydronium ions or hydroxide ions. The units of equivalent mass are g/eq. to be the mass in grams that reacts with one mole of strong base. H2SO4. the equivalent mass (EM) of an acid. the equivalent mass is one-half the molar mass: EM = 90 g / mol MM = = 45 g/eq # of acidic H 2 eq / mol The usefulness of equivalent mass is that we can calculate it from the results of a titration. In this case.
) At the beginning of the laboratory period. Your primary standard is potassium hydrogenphthalate (KHC8H4O4). discontinue heating. dry weighing bottle. After standardizing your NaOH solution. Dispose of them in the sink with a tap water rinse. you will use acid-base titrations to determine the equivalent mass of an unknown acid. 204. the mass of the acid. and the molarity of the titrant will all be known. After titration. Preliminary Procedures: 1.EM acid = macid Mbase Vbase Equation A4-2 In this exploration. While the water cools. As soon as it boils vigorously. the volume of the titrant (NaOH). and it reacts completely and cleanly with OH-: HC8H4O4-(aq)+ OH-(aq) → H2O(l) + C8H4O42-(aq) The equivalent mass of KHC8H4O4 is therefore numerically the same as its molar mass. The hydrogenphthalate anion has only one acidic hydrogen atom.) Check the color of the solid drying agent in your desiccator. titrating it against a known mass of an acid that is a primary standard.) Clean and dry a weighing bottle.23 g/mol. fill your 500-mL plastic storage bottle with deionized water. PROCEDURE Solution disposal: The solutions used in this exploration are not toxic. take the desiccator to the solutions stock room and exchange the drying agent for a fresh supply. carry out steps 2-7. You will first standardize a solution of NaOH to determine its molarity. A primary standard is a pure compound that can be weighed accurately and then titrated.) You should have vials of unknown acid and potassium hydrogenphthalate in your box of unknowns. you will use it to titrate a known mass of unknown but pure acid. I. and allow the water to cool until the beaker can be handled without discomfort. 3. put the uncovered bottle 44 . Transfer this water to your largest beaker and heat until the water boils. cover loosely with Al foil. This salt dissolves in water to yield potassium ion (K+) and the hydrogenphthalate ion (HC8H4O4-). so you can calculate the equivalent mass of the unknown acid. 4. If it appears pink. Transfer the KHC8H4O4 into the clean. The primary standard reacts completely and in only one way with the titrating reagent. 2. It should be blue.
) Mount your buret in a buret clamp. Then open the stopcock slowly and allow ten drops to fall from the buret. consult your instructor for the appropriate cleaning procedure. Step 7. Tare the balance and weighing paper. then record that mass. 6. so the titrations against KHP will allow you to calculate exact NaOH concentration in the stock solution instead of approximate values. Add approximately 5 mL (graduated cylinder accuracy) of the NaOH stock solution. calculate the size of one drop for your buret. 8. Mix this solution thoroughly by inverting the storage bottle and shaking many times (approximately thirty) so that the solution is perfectly homogeneous. Thorough mixing is essential for good results. and dry it in the oven at 110 oC for at least an hour. Weighing and Titration Procedures: Weighing: Each solid sample must be weighed on weighing paper to the nearest 0. Transfer the solid quantitatively to a clean 45 . so it is in fully vertical position. Record your unknown number in your lab notebook. Once the exact value of the NaOH concentration in stock solution is known. cover loosely with Al foil. Close the stopcock. (MM = 204. If droplets adhere on the walls. and the density of this solution is about 1. fill it about halfway with deionized water.) Store the vial of unknown acid. 9. 7. Once it is cool. The approximations calculated for the NaOH stock solution concentration.23 g/mol) that will be neutralized by 20 mL of this NaOH solution.1 mg. pour about half the water into your 500-mL storage bottle. cap the weighing bottle and keep it in your desiccator with its cap on except when actually weighing (this prevents absorption of water by the potassium hydrogenphthalate). The stock solution is about 50% by mass NaOH (MM = 40 g/mol).) When the beaker of boiled water from step 1 is cool enough to handle without discomfort. capped. Read and record the buret reading.5 g/mL. The KHP mass that you weigh out. and the molar mass of KHP. II.) Calculate the approximate molarity of the NaOH solution that you are going to prepare.) Remove your weighing bottle containing potassium hydrogenphthalate from the oven and let it cool (lid still off) in your closed desiccator. then the NaOH stock solution will be used to titrate your unknown acid to allow calculations of its equivalent mass. in your desiccator. 5. When your buret is clean. What is the correct number of significant figures for these results? Show your calculations to your laboratory instructor and verify that they are correct before proceeding further. are known precisely. NOTE: DO NOT DRY YOUR UNKNOWN. KHC8H4O4. Also calculate the mass of potassium hydrogenphthalate. Check the buret for cleanliness by filling with deionized water and allowing it to drain. then add the remaining water and cap the bottle. You will dilute 5 mL of this solution to about 500 mL. read and record the new buret reading.and its stopper (do not stopper the weighing bottle) inside a 250-mL beaker labelled with your name and section number. This is your standard base solution. add solid KHC8H4O4 until you have the appropriate mass calculated in Part 1. From the volume difference. give the estimated amount of KHP that you will use in the first titrations. Keep it capped except when you are transferring it to your buret (this prevents absorption of carbon dioxide from the atmosphere).
For subsequent titrations. reweigh.1500 g. you must have at least three "good" titrations that agree within 5 ppt! Solid disposal: Any unused solid can be disposed of by washing down the sink with tap water. calculate the molarity of your NaOH solution. rinse your buret with a few mL of standard base. Use these three to compute the molarity of your standard base and label your storage bottle accordingly. Allow about 1 mL to drain out. calculate the mass that will require 22 mL of titrant. After the endpoint is reached. Make sure no bubbles appear in the tip. Continue doing standardizations until you have 3 results that agree within 5 ppt. The first sample mass should be within 10% of your calculated amount for 20 mL of base. Transfer no more than 25 mL of solution at a time.135-0. use a mass within 10% of 0. Touch the tip to the side of the titration flask to transfer the partial drop. The mass of solid in the Erlenmeyer flask is the difference between these two recorded masses. in order to conserve your solution.5%). Caution: Dark pink means you overtitrated! When you get near the endpoint (pink color disappears slowly). consult your instructor before proceeding with the third titration. consult your instructor if you see bubbles. always transfer standard NaOH solution from your storage bottle to a clean. based on your calculated molarity from your initial titration. Titration: To avoid spillage.01 mL. After each titration. 46 . dry 50-mL beaker and use this to fill and refill your buret. Do this transfer immediately before filling.125-mL Erlenmeyer flask. (You can use simple proportions to get this result!). Titrate each sample to the first. Standardization: Titrate at least four KHC8H4O4 samples. you can add a partial drop by opening the stopcock just long enough for a droplet to form on the buret tip. Before beginning titrations. Add to the Erlenmeyer flask about 30 mL of deionized water and 2-4 drops of phenolphthalein indicator. For the first titration. If the results of the first two titrations disagree by more than 5 ppt (parts per thousand: 5 ppt is 0. Then fill it so the volume of titrant is more than 25 mL.15 g (0. then return the weighing paper to the balance.165) (Do not waste time by attempting to have a mass of exactly 0. record the buret reading to the nearest 0.01 mL. If you believe that one additional drop will exceed the endpoint. Subsequent samples should have a mass that you expect to require 22-24 mL of base. you have not yet reached the true endpoint. Read and record this volume to the nearest 0. At the end of the titration. rinse the sides of the flask using a squeeze bottle filled with deionized water (to be sure that none of the sample was splashed on the sides). and swirl the flask to mix the partial drop with the solution. To get full points for results. add base dropwise with swirling. and record the new mass. pale pink color that persists upon thorough mixing. as base solution that stands in contact with air becomes contaminated with carbon dioxide. Equivalent Mass: Titrate at least four samples of unknown acid.) From the result of this "pilot" titration. If the color disappears. use a sample mass within 10% of this value.
the three that give you the highest point total will be graded. show only the calculations for the first trial. Organize the sample calculations in a clear. If you report more than three values.) Provide a clear and organized set of sample calculations. DATA AND CALCULATIONS: This consists of three parts: 1. 2. For example. Use the data for your first trial to estimate the error limits.0001 g and the buret can be read to a precision of ± 0. your reported average value will be graded on a 0-5 basis. Determine these error limits by assuming you can weigh to a precision of ± 0. QUALITY OF RESULTS (20 points): Your three best values for the equivalent mass of your unknown will be graded on a 0-5 basis. Part of your grade will depend on your organization and clarity. coherent and well-labeled fashion. 47 .) Report the error limits on your value for the standard base molarity.01 mL.REPORT RESULTS REPORTING FORM: Attach a completed copy of the form in the Appendix. but do not show all calculations. if you carried out four trials of one type. In addition. 3.) Complete an Excel spreadsheet that is constructed according to the layout on the following page. See the Quantitative Observations section at the start of this manual. you may wish to consult reference sources such as the Handbook of Chemistry and Physics). describe how each part of the procedure in this exploration is important for obtaining accurate results. WRITTEN NARRATIVE: In no more than one typewritten page. Provide a sample calculation for each unique type of calculation. Comment on whether or not the equivalent mass that you obtained for your acid is a reasonable one (The unknowns are organic acids.
EXPLORATION A4: EQUIVALENT MASS OF AN ACID DATA AND RESULTS SHEET A. Analysis of the Unknown Acid Unknown Number Trial Mass of Unknown Titration Volume of NaOH Moles of acidic H atoms I _________ _________ _________ _________ II ________ ________ ________ ________ ________ _________ ________ ________ ________ ________ _________ III IV _________________ ________ _________ _________________ _________________ Equivalent Mass of Unknown_________ Average Equivalent Mass Absolute Deviation Average Absolute Deviation Relative Average Deviation (ppt) 48 . Standardization Trial Mass of KHC8H4O4 Titration Volume of NaOH Molarity of NaOH Solution Average Molarity Absolute Deviation Average Absolute Deviation Relative Average Deviation (ppt) _________ ________ ________ I ________ _________ _________ II ________ ________ ________ ________ ________ ________ _________ III IV _________________ ________ _________ ________ _________ B.
You will determine its chemical composition (empirical formula) by a combination of mass determinations. and analysis (determination of an empirical formula). and deductive reasoning. oxalate and waters of hydration. Oxalate is quantitatively oxidized by potassium permanganate (KMnO4). you can determine the water content by difference. Then you can determine the moles of potassium per gram of compound using the requirement that the compound be electrically neutral. volumetric procedures. You will prepare a green compound containing potassium.6. and 4. Experiments will let you compute grams and moles of iron and oxalate per gram of the compound.EXPLORATION A5 PREPARATION AND ANALYSIS OF A COMPOUND OBJECTIVES Chemists make new substances and then have to analyze them. purify it. and determine what it is. and redox reactions. for more details about formula determination. 4. and then analyze it. synthesis. isolate it. Five moles of oxalate react with two moles of permanganate.7. according to this net reaction: 16 H3O+(aq) + 2 MnO4.(aq) + 5 C2O42-(aq) → 2 Mn2+(aq) + 10 CO2(g) + 24 H2O(l) 49 .5. INTRODUCTION Consult your textbook. Sections 3. Your objectives are to make a substance. You have already carried out explorations involving simple synthesis and analysis. You will analyze for oxalate by doing redox titrations. iron. purification. and potassium per gram of compound. oxalate. Once you know the grams of iron. Now you will combine these two basic chemical procedures. Then you can find mole ratios and convert these ratios into an empirical formula. the way a research chemist might. purify it by crystallization. This exploration combines synthesis.
Light reduces all the iron in your green compound to Fe2+ ions. which is also its number of moles of iron.ions. Fe3+. A5-2 g of compound = 1− g of compound g of compound g of compound 50 . you can calculate the number of moles of solid. This analysis is similar to the one that you carried out on the aluminum compound in Exploration A2. The remaining C2O42. utilizing a unique light-driven redox reaction. Knowing moles of oxalate per gram. 2 Fe3+(aq) + 3 C2O42-(aq) + 4 H2O(l) → 2 FeC2O4. and some oxalate is oxidized to carbon dioxide. you can also calculate grams of potassium per gram of the green compound. From the mass of the solid. A5-1 Knowing moles of potassium per gram.First you will standardize a KMnO4 solution by titrating known samples of Na2C2O4 with permanganate solution. Knowing moles of iron per gram. You will deduce the amount of water in the green compound by difference. so: 3+ 2.2 H2O solid. This green compound contains K+. a canary-yellow insoluble solid. and C2O42. You will deduce the moles of potassium per gram of the green compound from the requirement that the compound be electrically neutral. Then you will titrate samples of your compound with the standard permanganate solution in order to determine the moles of oxalate per gram of the green compound. you can also calculate grams of iron per gram of the green compound. The sum of the grams per gram values must equal one.2 H2O. so the requirement for electrical neutrality is: mol C O2 − mol K+ 2 4 −3 =2 g of compound g of compound mol Fe3+ g of compound light Eq. you can also calculate grams of oxalate per gram of the green compound. Knowing the moles of iron and the mass of the original compound that was decomposed. + g of H O g of Fe g of C O g of K 2 2 4 − − Eq.2 H2O (s) + 2 CO2(g) You will collect and weigh the yellow FeC2O4.combines with Fe2+ to form FeC2O4. you can calculate the moles of iron per gram of the green compound. You will analyze for iron gravimetrically.
you can determine the empirical formula from the mole ratios.) Measure 4. 51 . and then transfer your sodium oxalate (in your unknowns box) into this bottle. and mix thoroughly with your glass stirring rod. place it (uncapped) in a 250mL beaker labeled with your name and section number. transfer the uncapped weighing bottle to your desiccator for storage. add it to the Erlenmeyer flask. Rinse the weighing bottle with deionized water. 2.5 M FeCl3 solution.Once the moles of each component per gram of compound is known. discard the potassium hydrogenphthalate in your weighing bottle. 3. Heat this mixture over a Bunsen burner.0 mL (graduated cylinder) of 2. You will use the dried sodium oxalate in Part II C. rounding as needed. Before the end of the period.0 g of K2C2O4•H2O on any convenient balance. Transfer the solid into a clean 125mL Erlenmeyer flask and add 12 mL (graduated cylinder) of deionized water. and dry it in the oven at 110oC for at least one hour. Remove it from the oven. and dry it in the oven for 10 minutes.) Place the flask in an ice bath and allow it to stand until the solution forms a large quantity of green crystals. allow it to cool.) Weigh 6. until the solid dissolves completely (the solution should not boil). PROCEDURE At the beginning of the first lab period. PART I: PREPARATION OF THE COMPOUND A. stirring occasionally with your glass stirring rod. Place the uncapped weighing bottle back in your 250-mL beaker labeled with your name and section number. Formation of the compound: 1.
and continue suction for at least 10 minutes to partially dry the solid. dry. and rinse twice with small quantities (several mL each) of acetone. turn on the suction to your filtration apparatus. Add 12 mL of deionized water to the flask. clean. 3. Then place the flask in an ice bath. stir it thoroughly.) Assemble your suction filtration apparatus. 4. 2.) Pour off the liquid above the green crystals. and pour the mixture onto the Büchner funnel. resume suction. and place the test tube in the ice bath to cool.) While you are waiting. and store in your locker when not in use. 52 . Purification of the compound 1. 6. After all the liquid has passed through. removing as much liquid as you can without losing any of the solid. stir the solid around and blot with an additional piece of filter paper. spread the solid out. Record the mass.B.) At the beginning of the next laboratory period. and heat the flask over a Bunsen burner until the solid redissolves.) When the cold flask contains a large amount of green crystals. rinse the solid with the cold water from the test tube. wrap the sample bottle in aluminum foil to protect the compound from light. and cover with a second piece of filter paper. Record the mass. Label the vial with your name and section number. transfer the Büchner funnel to the rinsing setup in a hood. 8.) Turn off the suction. Wet the filter paper with deionized water and turn on the suction briefly to draw the water through. Blot with the filter paper. Store the compound between the two pieces of paper in your locker until the next laboratory period. 7. and weigh your larger screw-capped vial.) Add 2-3 mL of deionized water to a test tube. transfer the solid to the screw-capped vial and weigh vial plus solid. Then return the Büchner funnel to your suction apparatus.) Transfer the solid to a large piece of filter paper on a watch glass. 5. and if the filter paper becomes visibly wet.
Continue the exposure to sunlight during the second laboratory period. so the irradiation will have to be done during two laboratory periods. Then leave it to stand until the next laboratory period. The filter paper should extend above the bottom of the funnel and around its entire circumference. Analysis of the compound for iron Note: while Step 2 is being carried out. a yellow precipitate is present. As the reaction proceeds. this is carbon dioxide being released in the reaction. 53 .PART II: ANALYSIS OF THE COMPOUND A. Label the test tube with your name and section number. Form the filter paper into a cup fitting snugly inside your Büchner funnel (recall exploration A2). stir the mixture thoroughly with your stirring rod. 4. The reaction will take several hours to go to completion.1 mg) a 7 cm piece of filter paper. gas bubbles will form.) Check your test tube about once every hour. proceed with Parts B and C. Assemble the funnel containing the filter paper in your filter flask and wet the filter paper with deionized water using your wash bottle. The reaction should be completed during this period. and LEAVE THE STIRRING ROD IN THE TEST TUBE. BE CAREFUL NOT TO TEAR THE FILTER PAPER DURING THIS OPERATION. Quantitatively transfer the weighed compound to a test tube and add 20 mL (graduated cylinder) of 10% (by volume) acetic acid. Stir the mixture with a glass stirring rod (no policeman).) Place the test tube in a test tube rack exposed to direct or diffuse sunlight (your instructor will tell you the proper location). BECAUSE CO2 GAS IS EVOLVED DURING THE REACTION. stirring it gently to insure that the solution is well mixed.) Weigh about 1. 1.1 mg) of your compound on weighing paper. The reaction is complete when the solution is nearly colorless. weighed to 0. At the end of the first period.1 grams (± 10%. and there is no green solid remaining.) Accurately weigh (0. 2. DO NOT STOPPER THE TEST TUBE. Turn on the suction to the filter flask and GENTLY press the filter paper down with your fingers until it contacts the funnel bottom completely. 3.
DO NOT USE ACETONE AT THE BENCH BECAUSE OTHERS MAY BE USING BUNSEN BURNERS. Repeat this process only once if all the precipitate has not yet been transferred. 54 . using the stirring rod to transfer as much of the precipitate as possible. The procedure for both types of titration is the same. as described in steps 1-3 below. cover with a watch glass. Finally. Do not use soap and water or acetone for cleaning. NOTE THAT THIS IS A DIFFERENT TEMPERATURE THAN BEFORE. stir thoroughly with your stirring rod. In the fume hood set up for acetone rinse by suction filtration. Then discontinue suction. and place the beaker in the drying oven at 60 ˚C for 1 hour. AND DO NOT LEAVE THE BEAKER IN THE OVEN OVERNIGHT. add about 4-5 mL of acetone to the test tube. Titrations using potassium permanganate Note: Your first titration should be a blank. Add several mL of deionized water to the test tube. Preparation of standard potassium permanganate solution Clean your 500-mL plastic storage bottle by rinsing it three times with small quantities of deionized water. Store the covered beaker in your locker until the next laboratory period. B. 6. Then weigh the filter paper and precipitate. Do an additional standardization after completing the titrations of your compound. Cap the bottle and mix thoroughly by inverting and shaking the bottle about thirty times.5. Then do three standardizations and three titrations of your compound. stir the solution and precipitate in the test tube thoroughly. remove the filter paper.) Continue suction on the filter flask for 10-15 minutes. place it in a beaker labeled with your name. Then pour it onto the filter paper.) Using your stirring rod. Repeated rinses will cause large errors in the determination since iron(II) oxalate is slightly soluble in water. C. rinse the entire filter paper with acetone from a wash bottle. being careful to transfer the last of the precipitate in the process. These leave a residue that will react with permanganate! Prepare 500 mL of potassium permanganate solution by transferring 35 mL (graduated cylinder accuracy) of stock permanganate solution into the 500mL storage bottle and filling with deionized water to within 1 inch of the top of the bottle. and rinse the precipitate on the filter paper with this solution. mix thoroughly and pour over the filter paper.
so you must perform a blank titration. Rinse your buret twice with 5 mL portions of your standard permanganate solution and then fill it to within 1 mL of the top. use a mass that requires between 22 and 24 mL of titrant.Blank: (Do only once). Drain about 0. weighed to the 0. and read and record the initial buret volume to the nearest 0.5%). For subsequent titrations. For your first standardization titration. but weighed to 0.1 mg). Subtract this volume from the volume of permanganate solution required to titrate each sample solution.) Set up your buret clamp on a ring stand. and 1 ml of concentrated H3PO4 .(oxalate) ions at the stoichiometric point (see net ionic equation on first page of Exploration A5) when calculating molarity of the permanganate solution. Titration: For your first titration on your compound. Standardization: Follow the titration procedures used for Analysis (see below) for both the standardization of the permanganate solution against sodium oxalate and the titration analysis of your compound.1 mg) of the dried sodium oxalate. For subsequent titrations. dry beaker and then pour this solution into your buret. use a proportional mass of dried sodium oxalate that requires between 22 and 24 mL of titrant. See the Data and Results sheet to guide you on the molarity calculation for the permanganate solution. weigh approximately 0.This titration should take no more than a few drops to reach the endpoint.15 gram (within 10%.(permanganate) ions for every 5 C2O42. Remember that there are 2 MnO4. The filling procedure for KMnO4 is the same as that used for standard base. make sure there are no bubbles in the buret tip. Transfer about 25 mL of solution to a clean. Follow the titration procedure on a solution that contains 50 mL deionized water. Remember to heat the contents of the flask to 80oC before titration with permanganate solution. Repeat standardization titrations until your molarities of permanganate solution agree within 5 ppt (0.15 gram (within 10%. Deionized water and the dilute sulfuric acid used to prepare the sample solution for titration may contain some impurities that react with permanganate ion.01 mL. 1. weigh a sample of your compound of about 0. Record this small volume. 5 mL of 6M H2SO4. 55 .5 mL out.
) Calculate the molarity of your standard potassium permanganate solution from the titration results for sodium oxalate.) Heat the solution to 80 ˚C. CALCULATIONS 1. and H3PO4 acts as a catalyst that speeds up the redox reaction. MnO2 may form instead of Mn2+. 3.) Weigh the sample to be titrated. d. swirling the flask as you add. The H2SO4 provides an excess of hydronium ions. Transfer the flask to the titration setup and begin adding KMnO4 solution. When permanganate reacts in a region that is low in acid concentration. a. and 1 mL (graduated cylinder) of concentrated H3PO4. f. 2.) Determine g/g and moles/g of water using Equation A5-2.) Determine moles/g and g/g of iron from the iron oxalate precipitate. e. do not multiply through to clear fractions. The pink color is due to a slight excess of permanganate ion. Titrate the solution with permanganate until you first see a permanent pink color in the mixed solution that lasts after thorough mixing.2. c. be sure that permanganate is added directly into the solution with good mixing.) Report the subscripts for potassium and oxalate to two decimals and the number of hydrated water molecules to one decimal. Calculate the molar mass based on these rounded values. even if the values are not close to integers. giving erroneous results. 5 mL (graduated cylinder) of 6 M H2SO4.) Determine moles/g and g/g of oxalate from the permanganate titrations. and transfer the solid to a clean 250-mL Erlenmeyer flask. During the titration. g. which is present in the system after all of the oxalate ions have been oxidized to CO2. The acid concentration may fall too low if the solution is not well mixed or if the permanganate is added down the side of the titration flask.) Round each value to the nearest integer. Add 50 mL (graduated cylinder) of deionized water.) Divide through by moles/g of iron to convert your results to one iron atom per formula unit (Do this even if it gives less than 1 for any of the other amounts).) Calculate the empirical formula of your compound as described in the introduction.) Determine moles/g and g/g of potassium using Equation A5-1. b. 56 .
assuming that iron is the limiting reactant and that each mole of iron should yield one mole of product. 57 . Calculate your percent yield of the compound. steps 6 and 8.4.) Calculate the mass of your purified product from the masses recorded in Part I. Convert to moles using the moles of iron per gram of compound that you determined in Step 2b.B.
18 points for the empirical formula. 3 points for the molarity of KMnO4. Include balanced chemical reactions. Provide a clear and organized set of sample calculations. you need show only the calculations for the first trial. coherent and well-labeled fashion. but do not show all calculations. WRITTEN NARRATIVE: In no more than one typewritten page.REPORT RESULTS REPORTING FORM: Attach a completed copy of the form in the Appendix. Comment on whether or not the empirical formula that you obtained for your compound is a reasonable one (you may wish to consult reference sources such as the Handbook of Chemistry and Physics). 58 . if you carried out four trials of one type. Include a sample calculation for each unique type of calculation. Organize the sample calculations in a clear. For example. DATA AND CALCULATIONS: Construct an Excel spreadsheet organized according to the layout on the following pages. QUALITY OF RESULTS: Your results are worth 24 points: 3 points for the yield of product. Part of your grade will depend on your organization and clarity. describe what happens to iron and oxalate in each step of the exploration in which a chemical change occurs.
) Sample Mass 2.) Mass of Sample Vial Plus Product 2. 1.) Moles of FeC2O4•2 H2O Precipitate (A4/MM) 6.) Mass of the Empty Sample Vial 3.) Mass of FeC2O4•2 H2O Precipitate (A3 – A2) 5.) Mass of Filter Paper 4.PREPARATION AND ANALYSIS OF AN IRON COMPOUND DATA AND RESULTS SHEETS I: Preparation and Yield of the Compound 1.) Moles of Iron Per Gram of Compound (A5/A1) 7.) Mass of iron/ g compound (A6 x MM Fe) Analysis of the Compound for Iron _______________ _______________ _______________ _______________ _______________ _______________ _______________ 59 .EXPLORATION A5 .) Mass of Filter Paper Plus Precipitate 3.) Mass of Product _________ _________ _________ II: Analysis of the Compound A.
) Moles of oxalate (B2/MM Na2C2O4) _________ 2 4.) Mass of Na2C2O4 (g) 1 _________ ________ ________ ________ ________ ________ _________ _________ ________ _________ _________ _________ 2 _________ _________ _________ _________ ________ 3 3. Standardization of KMnO4 1.) Moles C2O42-/g compound (C3/C1) 1 _________ _________ _________ _________ _________ _________ 2 _________ _________ _________ _________ 3 _________ _________ _________ _________ 60 .) Moles of C2O42. Titrimetric Analysis of the Compound for Oxalate Trial 1.) Blank volume: _____________ Trial 2.) Net Volume of MnO4.) Molarity of KMnO4 (B4x1000)/B5 7.B.) Net Volume of MnO4.) Moles of permanganate ( ) X (B3) _________ 5 5.(mL) (Subtract B1) 3.(5/2)(B7 x C2/1000) 4.) Mass of Sample 2.) Average Molarity of KMnO4 Absolute Deviation Average Absolute Deviation Relative Average Deviation (ppt) C.(mL) (Subtract B1) € 6.
A5-1) 2.) Mass oxalate/g compound (moles/gram x MM C2O4):_________ D Determination of Empirical Formula _______________ _______________ _______________ _______________ 1.) Moles of Potassium Per Gram Compound (Eq.) Mass potassium/g compound (moles/gram x MM K) 3.) Average Value (moles oxalate/g compound): Absolute Deviation Average Absolute Deviation Relative Average Deviation (ppt) _________ _________ _________ _________ _________ _________ 6.) Mass of water per gram of compound (Eq.) Moles of Water Per Gram Compound (D3/ MM H2O) Unrounded Empirical Formula of Compound: K____ Fe (C2O4)_____ • ___ H2O (report to 2 decimal places) Rounded Empirical Formula of the Compound: K___ Fe (C2O4)___ • _____ H2O (integral values) 5.5. A5-2) 4.3 x A6) % Yield of Product ___________ ___________ 61 .) Molar mass of compound calculated from the rounded formula: _________ E Determination of Yield Moles of FeCl3 used ___________ Moles of iron in product (I.
Appendix: Results Reporting Forms 62 .
and staple it to the front of your laboratory report. Density of Unknown Liquid ( Part D) Liquid Unknown Number: ________ Average Density: ______ D. FIRST NAME__________________ LAST NAME_______________________ SECTION NUMBER________ LAB INSTRUCTOR_____________________ A. Volume change on mixing (Part E) Average ∆Vmix (mL): _______ Average Percent Change ______% 63 .EXPLORATION A-1 Instructions: Copy this sheet. Volume of the 5-mL Pipet (Part C) Trial pipet volume 1 ____ 2 ____ ____ ____ ____ ____ 3 ____ 4 ____ ____ 5 average pipet volume (three significant figures) absolute deviation ____ ____ C.CHEMISTRY 120A RESULTS REPORTING FORM . fill it out completely. Do NOT place this sheet as part of your Data and Calculations section. Volume of the 10-mL Volumetric Flask (Part B) Trial flask volume 1 ____ 2 ____ 3 ____ ____ ____ ____ ____ 4 5 ____ ____ average flask volume (five significant figures) absolute deviation ____ ____ B.
CHEMISTRY 120A RESULTS REPORTING FORM . Do NOT place this sheet as part of your Data and Calculations section.) Empirical Formula (report unrounded values to two places): Based on 1 mole of Al3+ moles K+: _________ moles H2O: moles SO42-: _________ _________ Based on 2 moles of SO42moles K+: _________ moles H2O: moles Al3+: _________ _________ 64 .) Molar Mass of Aluminum (three significant figures) acidic trial: molar mass aluminum basic trial: molar mass aluminum 3. FIRST NAME__________________ LAST NAME_______________________ SECTION NUMBER________ 1. 2.) Yield of Product: mass purified compound ____________ percent yield ____________ LAB INSTRUCTOR_____________________ Calculate the percent yield using the molar mass of your empirical formula. and staple it to the front of your laboratory report.) Moles of Components per Gram of Compound moles of aluminum per gram compound moles of sulfate per gram compound moles of potassium per gram compound moles of water per gram compound ____________ ____________ ____________ ____________ ____________ ____________ 4. fill it out completely.EXPLORATION A-2 Instructions: Copy this sheet.
Do NOT place this sheet as part of your Data and Calculations section. Wavelengths of Hg lines λ (nm) blue ________ green __________ yellow ________ II. fill it out completely.CHEMISTRY 120A RESULTS REPORTING FORM . and staple it to the front of your laboratory report. Rare gas emission lines (List each color and wavelength) Neon Argon Krypton Xenon __________ __________ __________ __________ __________ __________ __________ __________ __________ __________ __________ __________ __________ __________ __________ __________ __________ __________ __________ __________ 65 . FIRST NAME__________________ LAST NAME_______________________ SECTION NUMBER________ LAB INSTRUCTOR_____________________ I. Fluorescent lights (List all that you observed) color: wavelength: _______ _______ _______ _______ _______ _______ _______ _______ _______ _______ III.EXPLORATION A-3 Instructions: Copy this sheet.
EXPLORATION A-4 Instructions: Copy this sheet. Do NOT place this sheet as part of your Data and Calculations section. FIRST NAME__________________ LAST NAME_______________________ SECTION NUMBER________ LAB INSTRUCTOR_____________________ A. and staple it to the front of your laboratory report. Equivalent Mass of Unknown Acid (report four best values) Unknown Number Trial Equivalent Mass Average Equivalent Mass Absolute Deviation Average Deviation _______ 1 _______ 2 ______ 3 ______ 4 ______ _______ _______ ______ ______ ______ _______ ______ Relative Average Deviation (parts per thousand) 66 . fill it out completely. Molarity Determination for NaOH (report four best values) Trial Molarity of NaOH Average Molarity Absolute Deviation Average Deviation 1 _______ 2 ______ 3 ______ 4 ______ _______ _______ ______ ______ ______ _______ ______ Relative Average Deviation (parts per thousand) B.CHEMISTRY 120A RESULTS REPORTING FORM .
CHEMISTRY 120A RESULTS REPORTING FORM . FIRST NAME__________________ LAST NAME_______________________ SECTION NUMBER________ 1.EXPLORATION A-5 Instructions: Copy this sheet.) Empirical formula (based on Fe3+-= 1) Report unrounded values to two places K+ _______ C2O42-________ H2O________ ____________ ____________ ____________ ____________ RAD (ppt): ______ LAB INSTRUCTOR_____________________ Molar mass based on rounded empirical formula ___________ 67 .) 2.) Yield of Product Mass of Purified Compound ____________ Percent Yield ____________ (Use your value for moles of iron per gram of sample to calculate the percent yield. fill it out completely.) Moles of components per gram of compound Moles of iron per gram compound Moles of oxalate per gram compound Moles of water per gram compound Moles of potassium per gram compound 4.) Molarity of KMnO4 Average Molarity _________ 3. Do NOT place this sheet as part of your Data and Calculations section. and staple it to the front of your laboratory report.
This action might not be possible to undo. Are you sure you want to continue?
We've moved you to where you read on your other device.
Get the full title to continue reading from where you left off, or restart the preview.