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Pitfalls and Errors of HPLC in Pictures

 E-Book
Sofort lieferbar | Lieferzeit: Sofort lieferbar I
ISBN-13:
9783527659135
Veröffentl:
2013
Einband:
E-Book
Seiten:
224
Autor:
Veronika R. Meyer
eBook Typ:
PDF
eBook Format:
Reflowable E-Book
Kopierschutz:
Adobe DRM [Hard-DRM]
Sprache:
Englisch
Beschreibung:

The third edition of this popular problem-solving guide for this widely-used method includes eleven completely new examples and several updated ones, adding up to 100 contributions about pitfalls and errors in HPLC. Each example is presented on a double page with the text on the left-hand and a fi gure on the right-hand side, true to the motto 'a picture says more than a thousand words'. In addition, the author presents essential fundamentals as well as helpful strategies, such as equipment tests or quality assurance processes. New in this edition * Variability of the standard deviation * Infl uence of the acid type and concentration in the eluent * Water as an unintentional additive in the mobile phase * Inadequate purity of mobile phase water * Incomplete degassing * Inadequate stabilization of the extraction solvent * Tailing of phosphate compounds in the presence of steel * Different detection properties of diastereomers * Detector overload in ELSD * System suitability test * From repeatability to reproducibility A must-have resource for all users - showing how to use HPLC efficiently and obtain reliable results.
The third edition of this popular problem-solving guide for this widely-used method includes eleven completely new examples andseveral updated ones, adding up to 100 contributions about pitfalls and errors in HPLC. Each example is presented on a double page with thetext on the left-hand and a fi gure on the right-hand side, true to the motto 'a picture says more than a thousand words'. In addition, theauthor presents essential fundamentals as well as helpful strategies, such as equipment tests or quality assurance processes.New in this edition* Variability of the standard deviation* Infl uence of the acid type and concentration in the eluent* Water as an unintentional additive in the mobile phase* Inadequate purity of mobile phase water* Incomplete degassing* Inadequate stabilization of the extraction solvent* Tailing of phosphate compounds in the presence of steel* Different detection properties of diastereomers* Detector overload in ELSD* System suitability test* From repeatability to reproducibilityA must-have resource for all users - showing how to use HPLC efficiently and obtain reliable results.
PREFACEINTRODUCTIONPART I: FundamentalsChromatographyChromatographic Figures of MeritThe Resolution of Two PeaksReduced ParametersThe Van Deemter CurvePeak Capacity and Number of Possible PeaksStatistical Resolution Probability: SimulationStatistical Resolution Probability: ExamplePrecision and Accuracy of an Analytical ResultStandard DeviationVariability of the Standard DeviationUncertainty PropagationReproducibility in Trace AnalysisRuggednessCalibration CurvesThe HPLC InstrumentThe Detector Response CurveNoiseThe Playground Presented as an Ishikawa DiagramThe Possible and the ImpossiblePART II: Pitfalls and Sources of ErrorMixing of the Mobile PhaseMobile Phase pHAdjustment of Mobile Phase pHInfluence of the Acid Type and Concentration in the EluentWater as an Unintentional Additive in the Mobile PhaseInadequate Purity of Mobile Phase WaterInadequate Purity of a Mobile Phase SolventInadequate Purity of a Mobile Phase ReagentIncomplete DegassingSystem Peaks and Quantitative AnalysisSample Preparation with Solid Phase ExtractionInadequate Stabilization of the Extraction SolventPoor Choice of Sample Solvent: Peak DistortionPoor Choice of Sample Solvent: TailingSample Solvent and Calibration CurveImpurities in the SampleFormation of a By-Product in the Sample SolutionDecomposition by the Sample VialArtifact Peaks from the Vial SeptumFormation of an Associate in the Sample SolutionPrecision and Accuracy with Loop InjectionInjection TechniqueInjection of AirSample Adsorption in the LoopExtra-Column VolumesDwell VolumeElution at t0Classification of C18 Reversed PhasesDifferent Selectivity of C18 Reversed PhasesDifferent Batches of Stationary PhaseChemical Reaction within the ColumnTailing of Phosphate Compounds in the Presence of SteelRecovery and Peak Shape Problems with ProteinsDouble Peaks from Stable ConformersInfluence of Temperature on the SeparationThermal Non-Equilibrium within the ColumnInfluence of the Flow Rate on the SeparationInfluence of Run Time and Flow Rate on Gradient SeparationsUV Spectra and Quantitative AnalysisUV Detection WavelengthDifferent Detection Properties of DiastereomersFluorescence Quenching by AirDetector Overload in UVDetector Overload in ELSDInfluence of the Retention Factor on Peak HeightInfluence of the Flow Rate on Peak AreaLeaks in the HPLC InstrumentImpairment of Precision as a Result of NoiseDetermination of Peak Area and Height at High NoisePeak Height RatiosIncompletely Resolved PeaksArea Rules for Incompletely Resolved PeaksAreas of a 1 : 10 Peak PairHeights of a 1 : 10 Peak PairQuantitative Analysis of a Small PeakIncompletely Resolved Peaks with TailingIntegration Threshold and Number of Detected PeaksDetector Time Constant and Peak ShapeQuantitative Analysis in the 99% RangeCorrelation Coefficient of Calibration CurvesPART III: Useful StrategiesColumn TestsApparatus TestsWavelength Accuracy of the UV DetectorInternal StandardsA Linearity TestRules for Accurate Quantitative Peak Size DeterminationHigh-Low ChromatographyControl ChartsVerification of the Analytical Result by Use of a Second MethodDescription of RuggednessRules for Passing On an HPLC MethodQuality Assurance in the LaboratoryStandard Operating ProceduresMethod ValidationSome Elements of ValidationA Validation ExampleSystem Suitability TestFrom Repeatability to ReproducibilityMeasurement UncertaintyFormal Quality Assurance SystemsINDEX

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