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Validation of Titration Methods - bikeitech.com

METTLER TOLEDO TitratorsValidation of Titration MethodsApplication brochure 16 Det LimResConcConf LimConf LimCalibration LineVEQEVPage 2/28 METTLER TOLEDOV alidation of Titration MethodsEditorialDear Readerthis Application Brochure provided by METTLER TOLEDO shows you how tovalidate a Titration method. The recommendations and remarks have been put to-gether by Chris Walter, Application Chemist of the Market Support AnaChem. Healso measured all the results and evaluated Validation of a method brings indeed some work, but thoughtful planning andcareful preparation limit the efforts. And you win a reliable method which you dailyapply with got the preface by courtesy of a user in the pacific region, who is a long timeexpert in method making.

Page 8/28 METTLER TOLEDO Validation of Titration Methods There are two practical ways to check a titration method for linearity: A) The regression coefficient (R 2) of the linear regression described in graph 1 must be better than a given limit, depending on the demanded accuracy for the specific determi-

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Transcription of Validation of Titration Methods - bikeitech.com

1 METTLER TOLEDO TitratorsValidation of Titration MethodsApplication brochure 16 Det LimResConcConf LimConf LimCalibration LineVEQEVPage 2/28 METTLER TOLEDOV alidation of Titration MethodsEditorialDear Readerthis Application Brochure provided by METTLER TOLEDO shows you how tovalidate a Titration method. The recommendations and remarks have been put to-gether by Chris Walter, Application Chemist of the Market Support AnaChem. Healso measured all the results and evaluated Validation of a method brings indeed some work, but thoughtful planning andcareful preparation limit the efforts. And you win a reliable method which you dailyapply with got the preface by courtesy of a user in the pacific region, who is a long timeexpert in method making.

2 We wish you many successful titrationsG. ReutemannH. HuberManager Market SupportRegional Market ManagerNorth East AsiaValidation of Titration MethodsMETTLER TOLEDO Page 3/28 ContentsPreface ..41 Summary ..52 Principle of of Validation and Recommended Limits .. of Accuracy .. of Precision .. Errors and Linearity .. of Systematic Errors .. of Linearity .. of Robustness and Ruggedness .. of Determination Limit .. 94 Practical Hints .. and Precautions .. Control Parameters .. Evaluation Parameters .. 115 Possible Sources of 116 Recommendations for not Conforming to Specifications ..138 Examples .. of Sulphuric Acid .. Determination .. and Accuracy .. Errors, Linearity.

3 And Ruggedness .. Limit .. Remarks .. 219 Appendix 1 ..2210 Appendix 2 .. of Results .. versus Accuracy .. 2411 Glossary ..2512 Literature ..26 Page 4/28 METTLER TOLEDOV alidation of Titration MethodsPrefaceIn this increasingly competitive world of business, the challenge of delivering highest-qual-ity products to consumers is a must. Behind any quality product are robust analytical meth-ods that ensure accurate addition of ingredients needed to deliver what is method must be simple yet accurate. Serious consideration must be given to the possibil-ity of the method being automated. This strategy eliminates human errors, increases produc-tivity and reduces the time needed to release the product to consumers without compromisingmethod accuracy and reproducibility hence, product quality.

4 Of course along with all themethods simplification comes analysis cost-saving. In addition, the method must be environ-ment-friendly via reduction, if not elimination, of the conventional use of organic solvents,especially non-biodegradable and toxic chemical protocols/SOP's followed during method Validation work are generally universal,irrespective of country, industry, company or product category. The only thing that is differ-ent between them is the accuracy required, with the strictest limits applied to those productsprepared for human consumption, , food and this brochure, METTLER TOLEDO summarizes the general method development include accuracy, reproducibility, linearity, ruggedness and limit of determination.

5 Eachmethod must pass all these tests, just like the consumer products for which the method will of Titration MethodsMETTLER TOLEDO Page 5/281 SummaryThe goal of all measurements and determinations is to generate correct results. Correct re-sults are accurate compared to the true value and precise in their statistical deviation [1].A detailed method is applied to obtain correct results. This method describes all the differentsteps from the sampling to the result. Whether correct results can be obtained or not with acertain method has to be validated. Validation of a method comprises tests for accuracy,precision, linearity, systematic errors, robustness/ruggedness and detection limit/determina-tion limit.

6 So the Validation of a method proves, whether or not the instruments used for thispurpose fulfill the specific the context of Validation a variety of expressions is used. Please refer to the glossary(chapter 11) for a short definition of the expressions used in this of ValidationAccuracy, Precision, Linearity, Systematic Errors, Robustness/Ruggedness and Determina-tion limit are checked, considering the complete analytical procedure from taking the sampleto result calculation and documentation. Use of a standard substance (Primary standard) allows the assessment of accuracy. Statistical evaluation of multiple sample series shows precision/reproducibility. Varying the analyte concentration indicates the linearity and systematic errors.

7 If the results show no deviations due to different analysts, time or day of analysis, instru-ments and electrodes, temperature or matrix effects, the method can be considered asrobust/rugged. The smallest amount of substance giving a detectable potential change with a quantifiabletitrant consumption is the detection limit. The smallest amount of sample that can be ti-trated with a good precision is the determination limit. So for the Validation only thedetermination limit is needed, since it includes the detection following application serves as a guideline, showing how a Titration method can be vali-dated. As an example, the method for the determination of sulphuric acid was limits for accuracy, reproducibility and linearity are subject to the tested Methods analysis of foods and drugs may require much stricter 6/28 METTLER TOLEDOV alidation of Titration Methods3 Steps of Validation and Recommended LimitsThe titrant to be used in this Validation has to be standardised first against a primary standards are commercially available substances with the following characteristics[1], [2], [3]: Clearly defined composition and high degree of purity.

8 Large equivalent mass (minimizing weighing errors). Accurately weighable (not hygroscopic, insensitive to oxygen and/or CO2). Stable in solutions and easily soluble in adequate solvents. Rapid and stoichiometric reaction with the appendix 1 for typical combinations of titrant and primary of AccuracyMultiple series of standard samples or of samples with exactly known concentration are ti-trated. The analyte concentration therein should cover the complete determination range. Thesample size should be varied randomly and result in a consumption of titrant of ca. 30 to 90%of the burette volume. A refilling of the burette should be mean value x of each series represents the result of the Titration .

9 The difference betweenthis mean value and the true value ( the known concentration) allows the determination :Results obtained should not deviate from the true value by more than of PrecisionMultiple series of a sample are titrated. Thereby the analyte concentration in the titrationbeaker should cover the complete determination range. This is done by varying the samplesize randomly so that a titrant consumption of ca. 30 to 90% of the burette volume results. Arefilling of the burette should be outlier test according to Grubbs [1] is performed on the results of these sample series inorder to eliminate distinct outliers. Then a statistical evaluation is performed on each sampleseries to get the mean value and the relative standard deviation RSD.

10 The RSD expresses theprecision of the :The relative standard deviation obtained from individual samples series should not be greaterthan of Titration MethodsMETTLER TOLEDO Page 7 Errors and LinearityTo discover systematic errors and the linearity of the method, the titrant consumption ob-tained in Chapter is plotted against the respective sample size which determines the analyteconcentration per single linear regression is performed on these data. The regression line is described by the for-mula y = a + bx , where a represents the intercept on the y-axis and b is the slope of theregression Definition of Systematic ErrorsSystematic errors of a Titration are for example disturbing influences due to the method itselfor to solvent blank the linear regression according to chapter systematic errors show up as a significantdeviation of the y-axis intercept a of the regression line from the zero point coordinates (seegraph 1), asys is clearly different from :The systematic error asys should be smaller than 15 L.


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