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# Intro Analyt Chem CHM 3120

FIU

GPA 3.76

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This 10 page Class Notes was uploaded by Celestine Raynor V on Monday October 12, 2015. The Class Notes belongs to CHM 3120 at Florida International University taught by Jose Almirall in Fall. Since its upload, it has received 4 views. For similar materials see /class/221826/chm-3120-florida-international-university in Chemistry at Florida International University.

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Date Created: 10/12/15

Welcome to CHM 3120 Introduction I To Analytical Chemistry The required textbook for this course is Quantitative Chemical Analysis Seventh Edition by Dan Harris Instructor Jos Almirall PhD Office CP 316 Labs CP194 CP153 OE109 x u v Email almirafiuedu Office Hours TuesThurs 2 3 pm The Almirall Research Group 2007 Tel 305 3483917 or by appointment Lecture 2 Overview LIBS Plasma Evolution Basic Tools Good Laboratory Practice GLP I I I I gt LabwareEquipment 10ns 500ns 1u810us 100us time Me hods Intensit Experimental Error Types of Error Significant Figures Propoga ion of Error in Analysis Early stages dominated by broadband continuum 010ps Rapid expansion and cooling Neutral and ionic dominated emission Theresuits arebackfromthelab Experimental Setup John Whispegnant Nd YAG Fundamental 1064nm 220mJ max energy 067Hz Rep Rate 266 and 532nm lasers New Wave Tempest 4th harmonic 266nm 27mJ max energy per pulse 067Hz Rep Rate Andor iCCD Camera Mechelle 200900nm Q V yin v c Chapter 3 Opener Quantitative Chemical Analysis Seventh Edition 2007 W HFreeman and Company GLP Laboratory Safety 1 Hazard Labeling Good Laboratory Practice GLP m embodies a set of principles that provides a iigi i39 39 eateg framework within which laboratory studies are 0203 Ombuwb39equotqwmghpmnmf planned performed monitored recorded reported iozo fRN39NGiF39ammab39equotq df39aShp 39quottlt and archivedGLP helps assure regulatory W 4F39ammabegas reXtreme39y ammab39equotqu39d authorities that the data submitted are true 1 Ei ii 39liii usemap Instability reflection of the results obtained during the study niamiy39siiiixviydb iharmfuquotf m and can therefore by relied upon when KJOYXQEnN ftai i i t x 39 iiif 39 om Mayreactf 4 DANGER May be atal on short heated or mixed with water exposure Specialize protective 1 2 WARNING Unstable or may react if mixed with water 3 DANGER Maybe exp osive if shocked heated confined or equipment required Specific Hazard w fVOidPS 0f water D TZEdAVKlngR tEplosive material 5 Rad39at39on N at room temperature ACID Acid ALK Alkali COR Corrosive OXY Oxid zer GLP Laboratory Safety GLP Laboratory Safety 1 Hazard Labeling 1 Hazard Labeling 2 Material Safety Data Sheet MSDS Physical Data Toxicity Health Effects First Aid Reactivity Storage Disposal Protective Equipment Spill Handling W FLAMMEELIOUID IRRITANT SON 6 GLP Laboratory Safety GLP Laboratory Safety Hazard Labeling Material Safety Data Sheet MSDS Protective Wear Fume Hoods Hazard Labeling Material Safety Data Sheet MSDS Protec ive Wear Proper Clothing no sandals shorts etc Safety GlassesGoggles Lab Coats flame and spillresistant Gloves PON PPON GLP Laboratory Safety Hazard Labeling Material Safety Data Sheet MSDS Protec ive Wear Fume Hoods Waste Disposal Spills and Accidents CDFNThPONT STATION KEEP AREA CLEAR GLP Laboratory Safety Hazard Labeling Material Safety Data Sheet MSDS Protective Wear Fume Hoods Waste Disposal Spills and Accidents Label Containers NQthPONT GLP Laboratory Safety Hazard Labeling Material Safety Data Sheet MSDS Protec ive Wear Fume Hoods Waste Disposal Spills and Accidents Label Containers Other NQWerON NOTICE N0 FOOD OB DRINK IN THIS AREA GLP Laboratory Notebooks A laboratory notebook should state what you did and what you observed and should be understandable to a stranger The measure of scientific truth is the ability to reproduce an experiment Never erase information crossout with a single line to make corrections WI W 10 a Basic Elements Purpose Materials Method Results Conclusions Measuring Mass Gravimetric Analysis Analytical Balance Shielding doors 5 prevent drafts l 393 Typically sensitive to 001 to 01 mg Use weighing weighing paper NOTE Brush clean after use l l l l I r gt v u39 r K l h I P l gt39 I I L I 39 i I t 6 1 l r 1 y 4 i 3 gt r a affili AA 7 gt r A L quot 5 Tare zero the balance Null detector Error signal vessel eg pan J Balance pan Y Coil of C electromagnet r Control lcit39N S Quit correct39on Servomotor current uantitative Chemical Analysis Seventh Edition co 2007 W H Freeman and Company Balince beam Optical scale Balance point V iiiiilimtmi Fulcrum knife edge Counterweight Removable weights Balance pan FigureZ Quantitative ChemimiAnaIysis Seventh Edition a 2007 w HFreeman and Company Table 2l Tolerances for laboratory balance weights Denomination Tolerance mg Denomination Tolerance mg Grams Class 1 Class 2 Milligrams Class ll Class 2 500 12 25 500 0010 0025 200 050 10 200 0010 0025 100 025 050 100 0010 0025 50 012 025 50 0010 0014 20 0074 010 20 0010 0014 10 0050 0074 10 0010 0014 5 0034 0054 5 0010 0014 2 0034 0054 2 0010 0014 1 0034 0054 1 0010 0014 a Tolerances are defined in ASTM American Society for Testing and Materials Standard E 617 Classes 1 and 2 are the most accurate Larger tolerances exist for Classes 3 6 which are not given in this table Table 21 Quantitative ChemicalAnalysis Seventh Edition 0 2007 w HFreeman and Company Measuring Mass Gravimetric Analysis Filtration and Gravimetric Analysis Gooch Crucible other Liquor Adapter Glass Rubber 6 H gt gt Vacuum Filtrate gt Trap Measuring Mass Gravimetric Analysis Filtration and Gravimetric Analysis Ashess Filter Paper Weighing By Difference Weightanalyte Weightfinal Weight initial Where Weightimtial is the weight of the vessel eg crucible filter paper etc and Weight nal is the weight of the vessel eg crucible filter paper etc containing the analyte Moisture and Gravimetric Analysis Hygroscopic rapidly absorb moisture water MethodsTools for HVCIroscopic Substances 1 Drying Ovens 2 Vacuum Dessicators 3 Dessicants 4 Repeated Weighing by Difference Preventing Weighing Errors Measuring Volume Volumetric Analysis Burets 963 mL 1453 mL 1 WaterAbsorption 2 Contact with VesselSample 3 Effects of TemperatureDrafts 4 Vibrations 5 Level 6 Spills 7 Calibration A 9 10 Level of meniscus 11 Quantitative ChemicaIAnaIysis evemh Edition 2007 w HFreeman and Company Table 22 Tolerances of Class A burets Buret Smallest volume graduation Tolerance ml ml ml 5 001 001 10 005 or 002 002 25 01 1003 50 01 1005 100 02 101 0 Quanmmive ChemicaIAnaIysis evemh Edition 2007 w HFreeman and Company Measuring Volume Volumetric Analysis Digital Burets l b 1 Delivery knob Digital Ii counter Reagent ca dge De very tube Fig ure 26b uanli drive hemiml Analysis Seventh Edition 2007 w HFreeman and Company Experimental Error Precision reproducibility of a result measurementquot Accuracy how close a measured value is to the true valuequot Accurate Precise Accurate NOT Precise NOT Accurate and Precise Experimental Error Significant Figures minimum number of digits needed to write a given value in scientific notation without loss of accuracyquot expressed in powers of 10 Examples 4 1234 X 10395 Igt Four 4 significant figures 4 h 000001234 4 5 6 123 4 a 1234 X 105 12340 X 105 123400 X 105 Experimental Error The Rules for Zerosquot Zeros are significant when they occur in the middle of a number Example 12034 X 105 Zeros are significant when they occur at the end of a number on the righthand side of a decimal point 5 Example 1 234QX 105 NOTE Assumes that zero is accurate estimate Experimental Error Significant Figures The last significant digit in a measured quantity always has associated uncertainty KNOWN eg 963 mL Interpolation Estimation of readings to the nearest tenth of distance between scale readings l 7 Final Reading 4 15 mL initial Reading 863 mL Experimental Error Significant Figures Some numbers are exact with an infinite number of unwritten significant digitsquot Example 5 people 50 people 500 people 5000 people Experimental Error Arithmetic and Significant Figures 1 AdditionSubtraction Express numbers with the same exponent Significant figures are limited to the least certain number 1234 X 10395 1 234 X 10395 678 X 10399 0000 78 X 10395 1234 78 X 10395 Significant Answer 1235 X 10395 Signi cant Figures Number 0 all certain d 39 its lus the first uncertain d 39 it 20 L or 2000 mL best expressed as 20 X 103 mL 2 sig gs sig gs 2 sig gs Significant Figures Rules for 39 39 39 the number of 80 fias 1 Disregard all initial zeros 2 Disregard all nal terminal zeros unless they follow a decimal point 3 All remaining digits including zeros between non zero digits are signi cant Tip Express data in scientilic notation to avoid conlusion in determining whether terminal zeros are signi cant Significant Figures Numerical Computation Convent ns When adding and subtracting express the numbers to the same power often 34 2432 X 106 2432 X 10B 00 0 6512X104 006512X10E 731 1227X105 012 7X10E 107 237 2X10E Answer 107 Answer 2374 X1W For Multiplication oi DlVlSlOn iouno tne answer to contain tne same 4 of sig gs as tne onginai number Witn tne smallest of sig gs 1 Arithmetic and Signi cant Figures AdditionSubtraction The number of signi cant gures in the answer may exceed or be less than that in he original data lfthe numbers being added do not have the same number of signi cant gures we are limited by the leastcertain one 5345 4 sig gs 726 x10M 6728 4 sig gs 669 x10M 12073 5 sig gs 057 x10M Rules for Roundingquot lfa number is less than halfWay lt 5 then round DOWN e g i 234 ruundstu i 23 Witn 3 signi cantuigits lfa number is more han hal vayquot gt 5 then round Q a g i 2345s ruunds to i 2346 Witn 5 signi cant digits lfa number is exactly hal vayquot 5 then round to the nearest EVEN number a g i 2345 ruundstu i 234 Witn 4 signi cantuigits i 2355 ruundstu i 236 Witn 4 signi cantuigits Additi onlSubtracti on Experimental Error Arithmetic and Signi cant Figures Express numbers with the same exponent Signi cant gures are limited to the least certain number 1234 x 10395 1234 x 105 678 x 10399 0000678 x 105 1234678 x 10395 123x10395 Lie Experimental Error Signi cant Fidures and Roundind OfF Rounding should only be done on nal answers not intermediate results to avoid accumulating roundoff 2416 mL 963 mL 14 53 mL 145 mL 242 mMm mL ill 1 ll l lll ill 1 ll Experimental Error Arithmetic and Signi cant Figures 1 AdditionSubtraction 2 MultiplicationDivision Signi cant gures are limited to the least certain number Multiply Example 1234 x 105Add exp nents x 678 x 10399 836652 x 103914 837 Experimental Error Arithmetic and Signi cant Figures 1 AdditionSubtraction 2 MultiplicationDivision Signi cant gures are limited to the least certain number Example Measure blood glucose level for three people and calculate average level 45 mM 678 mM 910 mM Exact number hasv 3 infinite significant figures 933333 67 68 Experimental Error Arithmetic and Signi cant Figures 1 AdditionSubtraction 2 MultiplicationDivision A Logarithms and Antilogarithms log n a logarithm ofn is a a is comprised of characteristic and mantissa eg a 1234 THE K mantissa characteristic n 10a n is the antilogarithm of a Experimental Error Arithmetic and Signi cant Figures 1 AdditionSubtraction 2 MultiplicationDivision 3 Logarithms and Antilogari hms Number of digits in the mantissa of the log of a number should equal the number of signi cant gures in that number Number of signi cant gures in the antilog should equal the number of digits in the mantissa Experimental Error Arithmetic and Signi cant Figures 1 AdditionSubtraction 2 MultiplicationDivision 3 Logarithms and Antilogarithms 4 digits Example log x 10395 49086848 4 significant 49087 Experimental Error Arithmetic and Sidnificant Fiqures 1 AdditionSubtraction 2 MultiplicationDivision 3 Logarithms and Antilogari hms 3 signi cant E 39 ti 1 23 171395731 xamp e an l 09 W 3 digits 171 Experimental Error Propoqation of Uncertainty from Random Error We can usually estimate or measure the random error associated with a measurement more next week Experimental Error Absolute Uncertainty i 00001 g s quot 2415 mL Experimental Error Absolute Uncertainty Relative Uncertainty compares the size of the absolute uncertainty with the size of its associated measurement Relative Uncertainty absolute uncertainty Wota M Units magnitude of the measurement Relative Uncertainty absolute uncertainty x 100 magnitude of the measurement Experimental Error Propoqation of Uncertainty from Random Error 1 AdditionSubtraction efinal 4 Zen2 Where efinal is the final calculated error and Zen2 is sum 2 of the squared errors en2 Experimental Error Propoqation of Uncertainty from Random Error 1 AdditionSubtraction efinal 94 Zen2 e 123 1001 e J e2e2e2 456 10027 63 1 2 3 789 003 I 0012 0022 0032 1368 e nak 00001 00004 00009 e4 1368 i 0 03 00014 3 0037 1O Experimental Error Pro a atian anncertain fram Random Error 1 AdditionSubtraction Percent Relative Uncertainty Relative Uncertainty 0037 00027 1368 0 0027 x100 027 Percent Relative U rt 39 t nce am y 03 Experimental Error Prapagatian anncertainty 39am Random Error 1 AdditionSubtraction 2 MultiplicationDivision quotnew Imam Where emai is the nal calculated percent error and Ze2quot is sum afthe squared percent error enz Experimental Error Pro a atian anncertain fram Random Error 1 AdditionSubtraction 2 M It39 I39 t39 D 39 39 u 1p Ica Ian Ivrsian quotAle39ma eaJ Zen2 e12 922 WX 4 My MEX 123 1015 e 001123x100 081 y mam EV in EX X456 00 e2 002456x100044 W a E mm E 561 e ewk 0302 144 v j X e r 561109 3 fggs 019 v7 lnx 4 e E 5e1eo05 082 Vex a 2w EX V Experimental Error Prapagatian anncertainty 39am Random Error 1 AdditionSubtraction MultiplicationDivision 3 Expanents and Logarithms Experimental Error Prapagatian anncertainty 39am Systematic Errar Example 1 Uncertainty in Molecular Mass Uncertainty in molecular mass oro2 Systematic Error Atamic Mass afOxygen 159994 1 Nule Dnieienee due to number uineuiions in atums isotope vaiiaiion We simply ADD systematic error 2 o o 00003 00003 00006 Experimental Error Prapagatian anncertainty fram Systematic Errar Example 1 Uncertainty in Molecular Mass Uncertainty in molecular mass of CZH Systematic Errar C2 C C 2 x 00008 00016 H4 HHHH 4 x 000007 000028 c2 H4 000102 0000202 39 R for andam Er 00016 errur in c and H independent NOT 000032 000032

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