Appendix on folding small, mediumand large sized fluted filter papers.5:15 Minutes

Suction Filtration: The Buchnerfunnel and flask, use of aspiratorsand vacuum systems, avoidance ofsolid precipitating out in flask bypre-cooling; drying the solid; Hirschfunnel, Buchner tube; shutdownprocedure. 7:02 Minutes

Recrystallization: Heating thesolvent, adding the compound, hotfiltration using a fluted filter paperand short stemmed glass funnel,obtaining, washing and drying thecrystals. Appendices on: solubilitytesting, promoting recrystallization,handling oils and treating discoloredsamples with activated charcoal.11:30 Minutes

Sublimation: Sublimation atatmospheric pressure; reducedpressure technique for less volatilesubstances; subliming largerquantities. 3:42 Minutes

charging the flask, choosing heatsource, controlling temperature,safety hints; shutdown procedure.3:09 Minutes

Basic Laboratory TechniquesAssembling Apparatus: Laboratoryglassware; greasing joints andusing PTFE sleeves; condenserswith fixed and detachableside-arms; supporting glasswarewith clamps, bosses and stands;distillation and refluxing; safetyprocedures for overnight working.7:30 Minutes

Using Stirrers: Types of stirrers:magnetic, mechanical, paddle;attaching a stirrer rod to motor;sealing of glands for controlledatmospheres, setting up a stirrerwith motor, flask and oil cup seal.6:57 Minutes

Heating Samples: The Bunsen andmicro burner, steam baths, stirrerhotplates, oil baths, and heatingmantles; safety aspects. 10:17 Minutes

Using a Rotary Evaporator: Initialset up, mounting the sample flask,evaporation of solvent from sample,the use of a water bath, obtainingthe product; shutdown procedure,disposal of unwanted solvent. 4:19 Minutes

Distillation Techniques

Distillation at AtmosphericPressure: Distillation below 200°C,safe disposal of uncondensedvapors; water-cooled condenser;using a thermometer; oil bath;distillation and collection ofdistillate; shutdown anddismantling. 7:14 Minutes

Distillation at Reduced Pressure:Two-necked Claisen head, water-cooled condenser, capillary bleed,use of oxygen-free nitrogen-filled

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Practical Laboratory

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balloon, multi-flask receiver-adaptor,water pump, solid carbondioxide/acetone trap, oil bath forheating; distillation and collection offractions. Appendix on testingcapillary bleed. 7:58 Minutes

Fractional Distillation: Design offractionating columns;demonstration of procedure frominitial set up of apparatus toobtaining the fractions, columncleaning, shutting down. 5:11 Minutes

Steam Distillation: Use of atwo-necked flask, splash head,dropping funnel and double-surfacecondenser; problems arising fromlow melting point solids; steamgenerator system; shutdownprocedure. 4:34 Minutes

Semi-Microdistillation: Examinationof pear-shaped flask for star cracks;use of the micro-burner, glass wool;distillation under reduced pressure;shutdown procedure. 1:49 Minutes

Purification Techniques

Gravity Filtration: Funnel and filterpaper selection; cold filtrationprocedure; hot filtration on a steambath; simple quantitative filtration.

Program PLS-101

• Multiple-choice quizzes• Open-ended questions

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Program PLS-102 Refluxing: Setting up apparatus,

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Practical Laboratory SkillsThe Practical Laboratory Skills series of e-Learning modules has been carefully and

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intelligently designed for use as a training and teaching tool in industrial, academic,environmental, government, and medical laboratories.

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Extraction TechniquesSolvent Extraction: Use ofseparating funnel, extractions withorganic layer lighter and heavierthan water; drying. Appendix onemulsions. 8:44 Minutes

Soxhlet Extraction: Apparatusset-up, siphon discharge action,loading sample, filling the flask,heating; shut down procedure.5:05 Minutes

Continuous Flow Extraction:Choosing the solvent; extractionsusing solvent less or more densethan sample solvent;post-extraction. 7:12 Minutes.

Drying Samples: Removal of waterfrom thermally stable solids bysuction or oven heating and fromthermally unstable compounds witha desiccator; use of desiccatorcabinets, choosing desiccants, safeuse of a vacuum desiccator;removal of water from liquids usingdrying agents, removal of dryingagent; drying gases usingmolecular sieve and a drying tower,safe use of anhydrous calciumchloride. 8:35 Minutes

IR, UV/Vis & NMRSpectroscopyInfrared Spectroscopy of Solids:Sampling techniques, including:storage and handling of potassiumbromide, using a mortar and pestle,disc pressing, transferring sampledisc to sample holder; Nujol mulltechnique including: alkali halideplates, estimating quantities, mullpreparation and application,cleaning and care of plates. 9:42 Minutes

weighing solids and liquids;calibrated pipettes; manualvariable-volume dispensing pipette;graduated pipette; syringes;handling air and moisture-sensitivecompounds including: inserting aneedle, using a balloon filled withinert gas, and inserting syringe intoa stock liquid container. 6:45 Minutes

Heating Samples: Sand bath,hotplate, measuring temperature,exploitation of temperature gradientto effect gentle or vigorous heating.1:27 Minutes

Gravity Filtration: Pasteur pipetteusing cotton wool, shorteningpipette tip, filtering, using extrasolvent to rinse pipette so as toensure maximum recovery ofsample. 1:25 Minutes

Suction Filtration: Assembling aHirsch funnel, choosing a vacuumsource, adding suspended solids tofunnel, filtering and washing solidwith filtrate, drying sample undervacuum. 2:42 Minutes

Extraction and Partition: Pasteurpipette; mixing solvent layers;removing bottom or top layers;extracting immiscible organic solidfrom aqueous solution; removinginorganic impurities; drying extractswith anhydrous magnesium sulfate;removing drying agent; isolatingproduct by boiling off solvent. 6:56 Minutes

Distillation at AtmosphericPressure: Hickman still, heating ona sand bath, transferring liquid toflask, making secure joints,condensate collection, shut down.2:54 Minutes

Distillation of Higher Boiling Liquids:Assembling apparatus, choosingsource of vacuum, insulating flask,collecting distillate. 2:00 Minutes

Chromatographic TechniquesThin Layer Chromatography (TLC):Chromatography plate, choice ofeluting solvent; marking the plate,using a capillary tube to spot theplate, using a filter paper to saturateatmosphere, the separation,removal of plate, drying; detectingspots using the naked eye, UV light,

staining; interpreting results;monitoring reactions; calculating Rfvalues. 6:42 Minutes

Column Chromatography: Use ofTLC to pre-select solvent system;selection and preparation ofcolumns, adding solvent/silica gelslurry, recycling solvent, eliminationof air bubbles, using compressed airto force fresh solvent throughadding sample; collection of eluent,analysis of fractions by TLC,combination of fractions andconcentration. 6:36 Minutes

Ion Exchange Chromatography:Preparation of resin; preparation ofcolumn; addition of resin; drainingoff excess water; regeneration,addition of sample, eluting andtesting/titrating eluent. 8:15 Minutes

Gas Chromatography: Packed andcapillary columns, ovens, mobilephase/carrier gas, setting injector-port and oven temperatures,dissolving sample, sample injection,gaseous samples; detection,retention times; identification ofunknown compounds. 7:43 Minutes

Volumetric TechniquesUsing Balances: Weighing in thelaboratory: general purposebalance, analytical balance,containment vessels, location ofbalances, leveling a balance;weighing solids and liquid reagents,use of tongs, tweezers and gloves,quantitative transfer, weighing bydifference, absolute weightsmethod, gravimetric analysis andashing. 9:10 Minutes

Using a Pipette: Volumetric andmeasuring pipettes, pi-pump, rubberbulbs, safety precautions; rinsingand filling, calibration, aliquottransfer, valve leaks. 9:16 Minutes

Using a Burette: Capacity,stopcocks, leaks, rinsing; filling;removal of air, burette technique.4:32 Minutes

Making up Solutions: Choosing avolumetric flask; storing standardstock solutions; example based oncopper salt: drying and cooling,weighing, dissolution, mixing,diluting stock solutions. 7:04 Minutes

Infrared Spectroscopy of Liquids:Handling alkali halide plates, addingliquid between plates, mountingplates in plate holder; obtaininginfrared spectra of dilute solutionsincluding: the choice ofspectroscopic grade solvent, fillingcells with solution, mounting cells inspectrophotometer, cleaning anddrying cells. 4:26 Minutes

Infrared Spectroscopy of Gases:Filling a gas cell by the purgingmethod using carbon monoxide;loading gas cell into spectrometer,obtaining a rotation-vibrationspectrum, and flushing gas cell withnitrogen gas to clean it. Appendixon use of vacuum line to fill cells.5:16 Minutes

Ultraviolet and VisibleSpectroscopy: UV/Visibleabsorption spectra; selecting asolvent, making up samples, cuvettecare, adding sample and referenceto cuvettes, locating cuvettes in adouble beam spectrometer; tips ifbands are too strong or too weak.Appendix on spectral interpretation.4:54 Minutes

Proton NMR Spectroscopy:Materials and methods, deuteratedsolvents, NMR tubes; selecting asolvent, using non-deuteratedsolvent for solubility testing,cleaning tube, making up a sample,in situ filtration of sample solution,inserting tube into spinner, types ofinstrument; obtaining a spectrum;NMR spectra for other nuclei.5:38 Minutes

Microscale LaboratoryTechniquesAssembling Apparatus: Microscaleapparatus: reaction containers,magnetic stirring, setting up a reflux,use of Teflon tape to join glassware,assembling; protection againstmoisture including: anhydrouscalcium chloride tubes, siliconrubber septum caps, hypodermicneedles. Appendix on usingapparatus with screw-cappedcouplings. 4:17 Minutes

Weighing and Material Transfer:Use of four-decimal-place balance,procedures for transferring and

Program PLS-104

Program PLS-105

Program PLS-106

Program PLS-107

Program PLS-108

19 innovative educational programs

Inorganic Analysis MethodsGravimetric Analysis: Dryingsintered glass crucibles, quantitativetransfers of liquid or solid samples toreaction vessels, addition ofreagents, testing for completeprecipitation, digestion, transferring,filtering, drying and weighing. 11:02 Minutes

Electrogravimetric Analysis forMetals: Weighing electrode and salt,dissolution, acidification, setting upstirrer, mounting and connectingelectrodes, applying voltage toelectrogravimetric cell, testing forcomplete deposition, washing,drying and weighing electrode,procedure for mixed metal solutions.8:30 Minutes

Kjeldahl Determination of Nitrogen:Weighing salt to four decimalplaces, transfer to digestion flask,adding acid and indicator toreceiving flask, adding alkali todigestion flask, heating, titration,Kjeldahl digestion using heat andconcentrated acid to break downcompounds. 10:01 Minutes

Measuring & ControllingTemperaturesMeasuring and ControllingTemperature: Mercury, Beckmanand pentane thermometers,accuracy and limitations, immersiondepths, use in Quickfit apparatus,repairing a broken bead; electricaltemperature measurement:thermocouple and meter, bimetallicjunctions, thermistor, non-contactthermometers; controllingtemperatures, constant-temperaturebaths. 7:54 Minutes

Determination of MeltingTemperature: Purity, identity;grinding samples, transferring to amelting temperature tube, using analuminum block apparatus; mixedmelting temperature determinationusing two different substances.Appendices on sealing, Hot StageMicroscope. 8:12 Minutes

Determination of BoilingTemperature: Making a finecapillary tube, breaking andsealing, loading into meltingtemperature apparatus, recordingboiling temperature. 2:42 Minutes

Determining a Liquid/Liquid PhaseDiagram: Using phenol/watersystem: preparing knowncomposition mixtures, placingtubes, heating water jacket,recording temperature; plotting aphase diagram. 3:44 Minutes

Determining a Solid/Solid PhaseDiagram: Usingacetamide/p-nitrophenol system:preparing known compositionmixtures, heating each tube untilmelting the solids, cooling,recording temperature; plotting aphase diagram. 2:46 Minutes

Microscale ChromatographyThin Layer Chromatography:Choosing plate and eluting solvent;marking plate, spotting, saturatingatmosphere with solvent,separation, removal, drying;detecting spots by the naked eye,UV light, staining; interpretingresults; monitoring reactions,measuring Rf values. 6:42 Minutes

Column Chromatography:Comparison of microscale withconventional chromatography;preparing column and reagentsincluding: shortening pipette,inserting plug, clamping and filling,adding solvent, removing airbubbles and cracks; sampleloading; eluting fractions;identification of the separatedcomponents via TLC; recovery ofproducts. 9:56 Minutes.

Gas Chromatography: Columns,oven, mobile phase/carrier gas;setting injector-port and oventemperatures, dissolving sample,

injecting onto column, detection ofeluents; retention times;identification of unknowncompounds. 4:32 Minutes

Preparation of a Grignard Reagent:Assembling apparatus andpreparation: sealing condenser,fitting it with hypodermic needle anddrying tube; adding reactants,refluxing, injection; purification ofproducts: reaction with acid,separation and extraction ofaqueous and ether layers, drying,filtering, evaporation. 8:17 Minutes

Microscale Purification &CharacterizationRecrystallization: Solvent test usingheated samples, filtration, reducingsolvent volume, cooling andcrystallization, filtration of productusing a Hirsch funnel, washing anddrying crystals. 8:46 Minutes

Recrystallization Using a CraigTube: Dissolving sample, filtration,collecting filtrate and washings in aCraig tube, reducing solvent volume,capping, cooling, centrifugation,recovery, washing and dryingcrystals; dealing with very finelydivided crystals.5:12 Minutes

Determination of BoilingTemperature: Heating a meltingtemperature tube to form a very finecapillary, breaking and sealing,placing capillary tube and liquid,loading assembly, recording boilingtemperature. 2:42 Minutes

Determination of MeltingTemperature: Grinding a sample,transfer to melting point tube, usingan aluminum block melting pointapparatus; mixed meltingtemperature determination.Appendix on using a Hot StageMicroscope. 5:44 Minutes

Infrared Spectroscopy of Solids:Sampling techniques; potassiumbromide disc; storage and handling,using pestle and mortar to mix, discpressing, mounting in the infraredspectrometer, cleaning die bydissolving, oven-drying; Nujol mulls:alkali halide plates, estimatingquantities, preparation, application,cleaning. 5:00 Minutes

Infrared Spectroscopy of Liquids:Handling alkali halide plates,adding liquid between plates,mounting in a plate holder;obtaining a spectrum; reducingthickness of liquid film; cleaningand care. 1:58 Minutes

Volumetric Analysis Methods

Doing a Titration: Preparingburette; titration flask; pipettingreagents; preliminary and accuratetitration, half-drop technique; usingan automatic titrator. 5:09 Minutes

Some Common End Points: Usingindicators in titrations; endpointdemonstrations: methyl red, methylorange, screened methyl orange,phenolphthalein, bromothymol blue,bromocresol green, eriochromeblack T, murexide, fluorescein,potassium chromate, ammoniumiron (III) sulfate, starch,self-indicating immiscible solvents,sodium diphenylamine sulfonate,ferroin, self-indicating potassiumpermanganate. 6:19 Minutes

Potentiometric Titrations: pHtitrations: comparison of indicatorand instrumental methods, pHmeter, calibration, accuratetitration, examples, multipleendpoints; redox and silver halidetitrations; preparing systems, takingreadings, caring for electrodes,plotting results. 17:32 Minutes

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Program PLS-112

Program PLS-111

Program PLS-110

Program PLS-109

Program PLS-113

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refractometers; measuring refractiveindices for solids. 8:20 Minutes

Measuring Rates of RadioactiveDecay: Radioactive processes;description of equipment to measuredecay rates; measuring sample;interpreting data, obtaining half-life,shut-down procedure. 6:43 Minutes

Gas Phase Electronic Spectra:Description of simple and constantdeviation spectrometers; calibration;measuring emission and absorptionspectra. 6:10 Minutes

Flame Photometry, AA & TGAMeasurementsUsing a Flame Photometer: Start-upprocedure; selecting filter;instrument setup; calibration;sample measurement; shut-down;partially dissolved samples; handlingdata. 10:15 Minutes

Using an Atomic AbsorptionSpectrometer: Start-up procedure;lamp selection; choosing analysiswavelength; calibrating instrument;measuring sample; handling data;shut-down procedure. 7:12 Minutes

Thermogravimetric Analysis:Thermal processes; instrumentdescription; preparing crucibles;start-up procedure; doing a trial run;characteristic features of TGAtraces; inspecting residues; doing anaccurate run; using derivative plots;shut-down procedure. 11:01 Minutes

ThermochemicalMeasurements

Using a Bomb Calorimeter:Thermochemical measurements;calibration; preparation; firing thebomb; plotting results; correctionfactors; sampling techniques forsolid and liquid sample 13:15 Minutes

Using a Dewar Calorimeter:Description, preparing for a run;obtaining readings; interpreting data;dealing with corrections. 5:20 Minutes

Determination of Enthalpy ofNeutralisation: Use of Dewarcalorimetry for measuring enthalpies;preparation; taking calibrationreadings; determining corrections fordilution effects; obtaining results forsamples; interpreting data. 9:20 Minutes

Solution Kinetics Techniques Oxidation of Iodide By HydrogenPeroxide: Background to iodineclock reaction; definingexperimental conditions; making upsolutions; carrying out experiment;plotting results; determining theimportance of other variables. 5:51 Minutes

Oxidation of Iodide By PotassiumPeroxydisulfate: Background tokinetic determinations; preparingequipment; making up reagents;carrying out kinetic runs; plottingresults; obtaining activationenergies; determining importance ofother variables. 5:40 Minutes

Iodination of Ketones: Background tohalogenation reactions; importanceof controlling temperature; preparingsolutions; setting up UV/visiblespectrometer; carrying outexperiment; plotting results;obtaining kinetic parameters. 8:45 Minutes

Measuring Solution PartitionCoefficients: Partitioning materialbetween solvents with differingpolarities; determining saturationconcentrations for iodine in water

and toluene; using titration andspectrophotometric methods.5:56 Minutes

Colorimetric Analysis: Preparingsolutions; calibration procedure;measuring unknown samples;plotting results; caring for solutioncells. 3:37 Minutes

Electrochemical Techniques Using Galvanic Cells: Componentsof galvanic cells; different types ofelectrodes; caring for electrodes;calibration of digital voltmeters;using salt bridges. 4:09 Minutes

Determination of StandardElectrode Potentials: Preparingsample and reference cell; using asalt bridge; using digital voltmeters;drift; measurements; caring forelectrodes; plotting results. 4:46 Minutes

Electrochemical Method forDetermining Solubility Products:Preparing sample and referencesolutions; setting up measuringsystem; taking readings; hints forobtaining good data; solubilityproducts. 2:34 Minutes

Using Electrochemical Cells toDetermine ThermodynamicParameters: Electrode potentials;assembling button cell,electrochemical circuitry; takingreadings; plotting results. 2:06 Minutes

Using Conductivity Cells:Components of cells; setting upequipment; measuring cell constantand conductivities of samplesolutions; caring for dippingelectrodes. 3:19 Minutes

Conductiometric Titrations:Preparing sample solutions; testing;setting up burette; takingmeasurements; caring forelectrode; plotting results. 6:05Minutes

Using an Automatic Titrator:Background to multiple samplingtechniques; setting up automatictitrator; titration; plotting results;manipulating data, derivative plots;shut-down procedure. 3:57 Minutes

Gas Phase Measurements Determination of the MolecularWeight of Gases: Introduction andsafety aspects; description of typicalvacuum line; starting up vacuumline; pumping out; checking forleaks; connecting sample trap;attaching molecular weight bulb;weighing empty and filled bulbs;recovering bulb sample; shut-downprocedure. 12:12 Minutes

Measuring the NO2/N2O4Equilibrium: Equilibrium processes;description of vacuum line;evacuation; finding null point of spiralgauge; taking measurements;shut-down procedure; plotting data.10:00 Minutes

Measuring The Saturated VaporPressure of a Liquid at VariousTemperatures: Isoteniscopefunctions; evacuating system; settingup; taking measurements;suck-back; collecting data;shut-down procedure; plotting data.6:15 Minutes

Using a Fortin Barometer:Description; making adjustments;taking readings; correcting fortemperature effects. 1:28 Minutes

Polarimetry, Refractometry &Radiochemistry

Using a Polarimeter: Setting upinstrument; assembling and fillingsample tubes; recording nullposition; obtaining angular readingfor sample solution; measuringtime-dependent phenomena. 8:25 Minutes

Determination of the RefractiveIndex: Abbé refractometer; set-up;calibration; measuring refractiveindex of a liquid sample; dark liquids;shut-down procedure; correlatingrefractive indices with structure andother physical data; other types of

Program PLS-115

Program PLS-118

Program PLS-114

Program PLS-117

Program PLS-119

Program PLS-116

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