Nonferrous Metal Sodium Hydroxide for Alumite Acidxbase titration by Automatic Potentiometric Titrator Standard 1.Abstract Sodium hydroxide of anodizing solution for Alumite is measured by titration with 1mol/L Hydrochloric acid up to the endpoint, which is the maximum inflexion on titration curve. The concentration of Sodium hydroxide is calculated from titration volume of Hydrochloric acid. 2.Reference 1) Experiment and Calculation for Quantitative Analysis Vol.2 by Seiji Takagi from Kyoritsu Publication 3.Cautions in measurement 1) Handle with care when you work on chemicals. 2) Sample liquid though diluted with pure water is still alkali, and corrodes response membrane of glass electrode. Therefore, remove residual sample liquid of electrode completely by stirring in a beaker filled with pure water. TIO-94004 Ver.01 1/4 4.Post-measurement care 1) As noted above, sample liquid is alkali, and corrodes response membrane of glass electrode. Therefore, remove residual sample liquid of electrode completely by stirring in a beaker filled with pure water. 2) Keep the electrode in a beaker filled with pure water after rinsed well. 5.Test equipment Main unit : Automatic potentiometric titrator (Standard preamplifier: STD-) Electrode: Option Glass electrode Option Ceramic type reference electrode Standard Temperature compensation electrode 6.Reagent Titrant : Solvent : Additive : l mo1/L Hydrochloric acid ( f=1.001 ) Pure water 10W/V% Potassium fluoride 7.Measurement procedure ―Measurement― 1) Prepare 5.0mL sample in a 200mL beaker, and add 100mL of pure water. 2) Titrate with 1mol/L Hydrochloric acid to obtain concentration of total concentration of Sodium hydroxide. 3) Add 30mL of 10W/V% Potassium fluoride. 4) Again titrate with 1mol/L Hydrochloric acid to obtain concentration of free Sodium hydroxide. 8.Formula Total Sodium hydroxide ( g/L ) = EP1×FA1×C1×K1 / SIZE Free Sodium hydroxide ( g/L ) = ( EP1-( EP2-EP1) / K2 )×FA1×C1×K1 / SIZE EP1 : Titration volume at EP1 ( mL ) EP2 : Titration volume at EP2 ( mL ) FA1 : Factor of titrant ( 1.001 ) C1 : Concentration conversion coefficient ( 40mg/mL ) ( 1mo1/L HCl 1mL ≡ 40mg NaOH ) K1 : Unite conversion coefficient ( 1 ) K2 : Unite conversion coefficient ( 3 ) SIZE : Sample size ( mL ) TIO-94004 Ver.01 2/4 9.Example of measurement -Ambient condition- Room temperature:25 ℃ Humidity : - Titration parameter [Titration parameter] Titration mode Titration form Titration burette Reagent name Detector number : Auto control : EP Stop : 01 : HCl : 1 [Control parameter] Number of EPs Auto simulation EP sense (Potential) EP sense (Differential) Over titration Gain Control speed : : : : : : : 2 Off 50.0 150.0 0.0mL 1 2.0 50 % Weather : Fair Preamplifier unit Max. volume of burette Auto stirrer Wait time before titration Titration direction : : : : : pH 40.0mL Off 0s Auto Data sampling potential Data sampling volume Separate potential setup Separate potential EP potential setup EP potential : : : : : : 4.0mV 0.5mL Off 0.0pH Off 0.0pH -Titration curve- (The above printout data are obtained from titration by AT-410) TIO-94004 Ver.01 3/4 -Measurement results- Batch calculated results Sample Total NaOH Free NaOH N ( mL ) (g/L) (g/L) Total NaOH Free NaOH 5.0 99.855 141.69 98.902 140.83 Mean (g/L) 1 5.0 SD (g/L) 2 0.997 0.83 100.89 142.49 5.0 RSD (%) 3 0.121 0.59 99.774 141.76 *The above results were obtained by 3 tests of the same sample. 10.Summary Alumite is generic term of Aluminum coating of oxidizing surface as anode by water electrolysis in strong acidity. It is also called Anodizing process. Sodium hydroxide is an inorganic compound with chemical formula NaOH, and is one of the most important basic chemicals for industries. It is designated as deleterious substance by Poisonous and Deleterious Substances Control Law. The sample measurement shows a good repeatability with 0.6% relative standard deviation. Precise and reliable measurement is assured by the automated potentiometry. The concentration of anodizing solution for alumite can be perfectly analyzed by any of the following titration systems manufactured by Kyoto Electronics (KEM). 【AT-610】 Awarded Product of Supreme Technology from Kyoto City • Easy key entry by touch panel of large color LCD (8-inch wide) • Simultaneous titration in parallel • Both potentiometric and Karl Fischer moisture titration (coulometric・volumetric) can be performed at a time. 【AT-510】 • Compact and cost performance model • PC card expands data memory for convenience and versatility. 【AT-500N-1】 • Low cost and high performance • Easy view with back light LCD • GLP/GMP conformed model TIO-94004 Ver.01 4/4
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