=P Figure 42. ceamien oxen te mint Greate one tgs rca aren Figure 4 ta ache Coun me deen tons dg hypotte wt tetcte le ls oer ae ave he nowmecnserera eelgce en Su com hey corms he ooh oe Mean Vas and Stanaara Deviation {nthe hype can Piger 41, x manufacture ein! he Mites of 768 lite igh ul. The tr rat sows Ge mb of lls wha tne beach 20-5 irra Lieu apprcaimaie + Gasin derruon neers rarllons i Ge contrac oe HB ‘ub ch a ames icknes: and quay of wlacheneats, ae anda. The MOCK SHE ee Gans eration atest te dab. AMY Fin et fea Wi ary soe ‘Ligh Pa Uetines, ant te corresponding Gaussian curve. at chracead hy 1 Bs Meo ay ‘eters ee Rte inva a The Geek cpt sig, ens em: Byatt hens x, lnfiyee 41, temen wae wah sansa ovat called Oe variance. The sanan doviaineexprened a 3 econ (ou mean vale (= 0 7 called me ree a ton oF ae cont ornate CHAPTER staticmaterial for volumetric analysis should (amongst other characteristics) have 2s high a formula weight 23 posible, in order tn minimize these random weighing errors. when a solution of a given molarity is being made up. In some analyses ‘microbal- ances’ are used to weigh quantities of 2 few milligrams — but the errors involved are f e x i In volumetric steps nandam errors arise in the use of walumetric glassware. In fill- ing a 280ml standard flask to the mark, the error (ie. the distance between the meniscus and the mark) might be about £0.02 cm in 2 flask neck of diameter ca. ‘LS. cm. This comesponds te a velume error of only about 0.05 ml - only 0.02% af the: cerrat in reading 3 brett 0.1 mal divi sions is ex. 0,010.02 ml. Each titration involves two such resdings (the errors af which are mot simply additive — see Chapter 2). If the titration volume is ca. 25 ml, the percentage error ie again very small. The experimental conditions chould be arranged so that the volume af fitrant is aot too small (say aot less than 10 ml}, otherwise the errors will become appreciable. (This precaution is analogous 0. choosing 2 standard compound of high formula weight to minimize the weighing error.) Even though a volumetric analysis inwelves several steps, in each of which 3 Piece of volumettic glassware is used, if is apparent that the random errors should bbe small if the experiments are performed with care. In peactice a good volumetsic analysis should havea relative standard deviation (see Chapter 2} of act more than about 0.1%. Until recently such precision was not normally attainable in instru mental analysis methods, and it is still not common, ‘Volumetric procedures incorporate several imparant sources of systematic error. (Chief amongst these are the drainage-errors in the use of volumetric glassware, cali- bration errors in the glassware, and ‘indicator errory’. Pethaps the cammomest erat in routine volumetric analysis is to fail to allow enaugh time for a pipette to drain Properly, or a menisrus level in a burette to stabilize. Pipette deainage errors have 3 systematic as well as a random effect: the volume delivered is invariably less than it should be. The temperature at which an experiment is performed has two effects. Volumetric equipment is conventionally calibrated at 20°C, but the temperature inPRELIMINARY OPERATIONS OF ANALYSIS. 6 Fall ing: Just wot a container on the pan and touch the nezero butlon and the rae arg Jt a x conlaines display 17. Overload protection: Full-ange tring and ovecioad protection prevent damage to the balance ‘fecess weight & placed on the pas L644 Precantioas aad Procedures, With analytical balances the follwing guidlines should be vobuarved: |L Level the balance using the air bubble oat. 2% bw the mural warp period o eae the balance under power. Follow the required pesca ‘comsizatly under power. (3. Une any built-in calibeation mass und exicroprocessor-coairulled calibration cycle at Ube begin- ning of every workday. “Haale eating ote wih rey, Fngeinomplasorae on Baybee Fm an opr S. Always close the sliding doors om the halusce when weighing. zeroing. ot calibrating. 6 Acospl and second the displayed result ws soon as the balance indicates stability; cbsery the motice detector Fight in the display. Never atiempt to average the displayed numbers ‘mentally. 17. Chock the reiailty of each balance every day against certified weights (See. 1.6.7), = ‘cal othe performance ofthe laboratory. Halaaces should be Cleaned and calibrated al least twice ‘a your, more often if the werk Isad is unusually heavy. 1.85 The Weighing Station “The finer the readability of a balance, the more critical isthe choice of its proper location and eavi- ronmest. Cbserve these precautisas- |. Avoid air currents. Locate the station away from daces, windows, heat and airconditioning outlees. 12. Avoid having radiaat eat sources, such as direct sunlight, ovens, and haschoand heaters nearby. (3 Avoid areas with vibrations. Locale th sation away from eleratoes and rotaling machinery. Special ‘vibration-frse werk tables may be necded. To test, the displayed weight should noe change ifthe ‘operator shifis his oc her weight, leans on the table, o places a heavy olject next tothe baluace. 4. Choose un area free from sbecrmal miio-frequency and elecicenagnetic imerference. The bal- ‘ace should not be on the samme line circuit wilh equipment that generates such inteference, such a elecwic ares or sparks. ‘5. Maintain the humidity in the range from 15% to 85%. Dry air can cause weighing errors through celocrreataic charges on the weighing object and the balance wiadows. A room burnidifir might help. Humid air causes problems because of moisture absorption by camples and coniainer mar- (aces, A room dehumidifier would kelp. (6 Maictais an eves lempecature ofthe rooen and object weighed. Ef an object is warm relative to the balance, comectice cumeats case the pan te be buoyed up, sed the apparent mass is less thas the ‘nae mass. 7. Remember that matsials to be weighed take up water or eathon diovide from the air during the ‘weighing process in a clowad system, Weigh volatile mulerials in w cloned system, 9, Sit down when dsing precise weighing. The operator should be able us plant elbows on the work lable, thas allowing a steady hand in handling delicate samples