THE CALIBRATION OF VOLUMETRIC WARE, Reference: Soot D. As West, D.M. Fundamentals of Analytical Chemisty, 4th ed; Saunders: Philadelphia, 1982; pp. 717-728, Introduction and Background: In the previous experiment you used Minitab to explore certain relationships involving the tolerances of volumetric flasks. How are tolerances (or more generally, uncertainties) handled in the laboratory? In this experiment you are asked to employ appropriate techniques to calibrate a volumetric flask, a pipet, and a buret. General Approach. The most common way to calibrate volumetric ware is to accurately measure the mass of a Specific volume of liquid, Water isa convenient liquid for thie Purpose. A table giving the den- sity of H,0 as a function of its temperature is provided on poe 4 The coefficient of expansion of liquid water is about 0.023% Per degree near room temperature. This Value is large enough to cause only a minof variation in temperature to affect the precision of ordinary volumetric measurements, For example, a 50.00 mL sample of H,0 at 15° occupies 50.17 mL at 30°: AV = 50.00 mL. x 0,00023 x (30°- 15°) = 40.17 mL Ghainical Balances. ‘There axe five different types of analytical balances in Houghton 211, Each has its own capacity and accuracy (see p. 4). Over the course of the semester you should master all five. As Ageneral rule, however, you should use the same balance for all selaces weighings (ie. " ‘afler measurements), In this experiment itis especially important thet you be aware of ‘se the most accurate balance which has the necessary capacity for your purpose. Tes. There isa difference between the volume of water a pipet contains and what it delivers. (Why??) The pipets you will use are of the volumetric type; that is; a 25 cor pipet will deliver 25.0 mL of liquid iter tsed properly. (Fillo the meniscus; drain completely and ther Temove any droplet adhering to the tip, but do not shake or blow it out,) sre Burct technique is very important in analytical chemistry (and to your grade in this course!), Some general considerations: 1. Water does not bead on the inside wall of a Properly cleaned buret; rather, it flows in sheets, dime et Pouring a solution into your buret, wait for atleast 30 seconds before taking a reading to permit time for drainage. Before beginning a titration, check the stopcock for leakage and remove any air bubbles from the tip.3. Always read the meniscus to two decimals, 4, Remove a pendant drop by touching the drop (but not the buret tip) to the side of the receiving flask, 5. Your technique should be such that you can add a fraction of a drop at a time, 4. Perfect” buret should deliver $0.00 mL of liquid when drained from the 0.00 to the 50.00 mL calibra- tion mark, However, that isn’t necessarily good enough. Shouldn't it also deliv 25.00 mL when Grained from the 0.00 to the 25.00 mL mark, and 25.00 ml. when drained from the 25.00 to the 50.00 mL mark? Procedure: 4. Begin by cleaning a 400 mL beaker with soap and tap water. Rinse twice with tap water and then {ith @ few milliliters of deionized water. Fill with deionized water, and place a thermometer in the beaker. "*** Why are you doing this??. **+# & lise soap and tap water to clean your buret prior to use. The final rinsing should always be done with ‘Whatever liquid you intend to measure from it- in this ease, deionized water The volumetric flask and pipet can be assumed to be clean. (Keep them dry.) 3, As a warm-up" procedure, calibrate your volumetric flask; one tral will be adequate. This can be Accomplished by taking the cae (empty) mass, filling with water to the mark (aren't medicine droppers hhandy tools?) and then re-weighing it. How te Stme basic principle (mass/densty of water) can be applied in ealibrating a volumetric pipet How exactly will you do it? Whatever procedure you choose, be sure to utilize the meniscus. Carry out four trials - at least three must agree within experimental error. Bae, Souls in calibrating the buret are to measure the volume delivered by drainage of approximately the top half, the bottom half, and the entire buret. Perform at least two replicate measorceeney Report: ‘The report for this experiment is relatively simple; you need only do the following: 4. Asalways, submit the carbon copy of your notebook notations for this experiment. Fg ennclate the containment volume of your volumetric flask and the delivery volumes of your pipet find buret (0-25, 25-50, and 0-50 mL). Your answers must take the temperature into accouat re cee to have significance.TABLE 14-2 eee ee Oe ee The Density of Water (g/cm’) at 0.1°C Temperature Intervals TCO. 00" 01 02". oar 04 0 0.999840 847 853 860 866 872-878-883 BBD 894 1 899 904 909 913 917 922-926 930-933-937 2 940 943 946 949 952 954-956-959 960 962. 3 964 966 967 968 969 970 971 OT 972 972. 4 972 972 972 91 971 970 969 968 967 966, 5 964 962 960 958 956 954-951-949 946943, 6 940 937 933 930 926 922 918 914-910 906, iu 8 9 10 07 08 901 896 892-887-881 876-871-865. 860 RSH B48 842 836 829 823-816 809 803.796 788 781 774 766 758 750 742 734 «726-717-708 700 691 682 673 664 654 G45 635-625 GIS "1 60S 595 584 574 563-553. 542 S31 520 508 12 497 485 474 462 450438426414 401389 B 316 363. 350. 337-324. 31-298 284. 271-257 4 243-229 «215-201-186 «172,157 143.283 1 098 083 068 052-037021-«006 990" 974" 958" 16 0.998942 926 909 893 876 860 843 826 808 791 7 714 757 739° 721 704 686-668-650 «632613. 18 595 576 558 539 520 S01 482-463. 444425 19 405 385 366 346326 306-286 265-245-225 20 204 183 163 142 121 100-079-057 0361S 21 0.997993 971 949 928 906 883.861 «839816794 2 711 748 725 702 679 656 633 609 586563 2B 539 SIS 492 468 444 «420-396-371 347323 4 298 273 248 224 199 173 148 123 097 O72 25 046 020 995" 969" 943" 917" 801" S64" 838" BIZ 26 0.996785 758 732 705 678 651 «624 596-569 S42 2 S14 486 459 431 403375347319 291262. 28 234 205 177 148 119 09106203304 97H" 29 0.995945 916 886 857 827 797-768 « 738 708—«678 648 62 «595653 443 4 ‘Source: Landolt-Bornstein, 6th ed., Numerical Data and Functional Relationships in Physics, Chem istry, Geophysies and Technology, H. Borchers, K.-H. Heilwege, and K. Schifer, eds, vol. IV. pt. Springer-Verlag, New York, 1980, pp. 101-102. "The first three digits are the same asin the next entry ofthe 0.0 column.