Julabo：异氰酸酯NCO中NCO含量的检测

Analysis And Testing Technology Julobo：VISCOAnalysis And Testing Technology Application Application Use This method is applicable for material containing reactive isocyanate groups.The isocyanate is reactedwith di-n-butyl amine to form a urea. Unreacted (excess)amine is determined by backtitration withhydrochloric acid. Appliances Titrator： TL 7000/TL 7750 M1/20 or 50 Basic device Magnetic stirrer TM 235 20/50 mL exchange unit WA 20/50， with amber glass bottle for the titrant， complete Erlenmeyer flask 250 or 300 ml， Syringe 2 or 5 ml for high viscosity samples Electrodes Electrode： N 6480 eth+ TZ 1643 titration tip Electrolyte： L 5034 (LiCl/ethanol) Calibration： n.a. Reagents Titrant： HCl 1 mol/l aqueous or HCI in methanol. Sometimes HCI 0.5 mol/l Titer determination： TRIS (Tris hydroxyl aminomethan) Reagent mixture： Di-n-butylamine solution 1 mol/l Solvent： Toluene dried with molecular sieve 4A Additional solvent： acetone or other suitable solvents Description Determination of the exact concentration of the HCL titrant We recommend ready to use HCl titrant. The exact concentration of the HCL 1.000 mol/l can bedetermined using the titrimetric standard Tris hydroxy amino methane (TRIS). The standard can bedried for 24 h in an exsiccator at room temperature. 1-2 g of the standard are weighed accurately in a 150 mL beaker and dissolved in 80 mL of dist. waterwith stirring. It is titrated with the 1 mol/l HCl solution. Repeat the standardization two times. The average value is stored automatically in the exchangeableunit. Page 1： Curve and result： Titer determination The curve shows the use of an HCI 0.1 mol/l. The sample amount of TRIS should be 10- 15 timeshigher for the 1 mol/l titrant. GLP documentation Titration araph 8.56ml · pH/ml mdCpH/dml Method data Method name：Titre HClTitration duration：3 m 8sEnd date：13.09.12End time：14：39：30Ttation dataSample ID：TRISWeight：0.1038 gStart pH：pH9.590End pH：pH 3.864Start temperature：25.0°℃(m)End temperature：25.0°℃(m)Zero point：pH 6.83/-10.0 mVSlope：100.6%/-59.5mV/pHEQ：8.560 ml/ pH 4.849Titre：0.1001 mol/l Calculation formula Titre： (W*F2)/((EQ1-B)*M*F1)->M103 Mol (M)： 121.14000 Weight(W)： manBlank value (B)： 0.0000 mlOff Factor 2 (F2)： 1000.0000 Factor 1 (F1)： 1.0000 Statistics： Application Page 2： Method parameters Titer determination： Method data overall view Method name： Titre HCl Created at： Method type： Automatic titration Last modification： Measured value： pH Damping settings： None Titration mode： Dynamic Documentation： GLP Dynamic： Steep Measuring speed /drift： Normal： minimum holding time： 02 s maximum holding time： 15 s Measuring time： 02 s Drift： Initial waiting time： O s Titration direction： Decrease Pretitration： Off End value： 2.500 pH EQ： On (1) Slope value： Steep Value： 700 Dosing parameter Dosing speed： 100% Filling speed： 30 s Maximum dosing volume： 50.00 ml Unit values Unit size： 20ml Unit ID： 10039005 Reagent： HCl 0.1 mol/L Batch ID： no Charge Concentration [mol/l]： 0.10070 Determined at： 12/05/11 19：18：45 Expire date： 08/18/12 Opened/compounded： 09/10/11 Test according ISO 8655： 05/10/11 Last modification： 09/13/12 14：35：18 Application Di n-butylamine solution 129 g di-n-butyl amine are weight in a 1 L volumetric flask and filled up to the mark with dried toluene. Titration of the sample There are different procedures. Sometimes the di n-butylamine solution is pipetted first and then thesample is weight in. lin some procedures the sample is weight in first and the reagent mixture is addedafterwards. The ISO 14896 (part A) describes the pipetting of the di n-butylamine solution into an Erlenmeyer flask(250-300 ml) and then the addition of the sample. We are following this procedure. Pipette 50.00 ml using a volumetric pipette into an Erlenmeyer flask with stopper. The sample isweight in using a 2 or 5 ml syringe by different weight. Sample weight should be between 2-5 g. Close the flask with a stopper and gently stir the mixture on the magnetic stirrer until the sample iscompletely dissolved. Wait then additional 15 min for the reaction + 5 - 10 minutes until the mixturecooled down to room temperature. Add 100- 150 ml acetone (or any other suitable solvent) carefully. Place the Erlenmeyer flask on the magnetic stirrer (if not already) and start the titration method. Afterthe titration rinse the electrode and burette tip with ethanol. For each set of samples perform a blanktitration. Result calculation % NCO %NCO=(EQ1-B)*M*T*F1/(W*F2) EQ1： ml consumption at the equivalence point ml consumption for the blank titrationMTW 4.202 equivalent weight including conversation factor to % NCO concentration of the HCI titrant (e.g.1.002 mol/l) sample weight in g F1，F2：：1 Application Blank titration page 1： Curve and result GLP documentation Iitration araph Calculation formula Blank：EQ1-> M01Mol (M)：1.00000Statistics：Off Application Blank titration page 2： method The pre-titration volume can also be changed to 25-40 ml. The end volume can also be changed to 55or 60 ml. Method data overall view Method name：NCO blank titrationCreated at： 11/17/1111：29：35Method type：Automatic titrationLast modification： 06/27/12 10：48：12Measured value：mVTitration mode：DynamicDocumentation： GLPDynamic：SteepMeasuring speed / drift：Normal：minimum holding time： 02 smaximum holding time： 15 sMeasuring time： 02 sDrift： 20 mV/minInitial waiting time：0sTitration direction：IncreasePretitration：10.000 mlDelay time： 10 sEnd value：EQ：Slope value：SteepValue： 700 Dosing parameter Dosing speed： 100 % Filling speed： 30 s Maximum dosing volume： 50.00 ml Unit values Unit size： 20ml Unit ID： 10039060 Reagent： HC 1 mol/l Batch ID： no entry Concentration [mol/l]： 1.00000 Determined at： 06/27/12 16：03：58 Expire date： Opened/compounded： Test according ISO 8655： Last modification： 06/27/12 9：04：36 Application Sample titration page 1： Curve and resultThe result calculation was wrong here for this titration because of using a wrong factor. GLP documentation Iitation araph 10.45 ml155.1 mV ·mV/ml Method data Method name：NCO sampleTitration duration：2 m 11sEnd date：27.06.12End time：11：03：06Ttation dataSample ID：Dummy oneWeight：5.5463 gStart mV：-133.7 mVEnd mV：271.1 mVEQ：10.448 ml/ 155.1 mVfree NCO：942.928% Application Sample titration page 2： method The pre-titration volume can also be changed to 5， 10 or more ml. Method data overall view Method name： NCO sample Created at： Method type： Automatic titration Last modification： Measured value： mV Titration mode： Dynamic Documentation： GLP Dynamic： Steep Measuring speed / drift： Normal： minimum holding time： 02 s maximum holding time： 15s Measuring time： 02 s Drift： 20 mV/min Initial waiting time： 0 s Titration direction： Increase Pretitration： 2.000 ml Delay time： 10 s End value： EQ： Slope value： Steep Value： 700 Dosing parameter Dosing speed： 100 % Filling speed： 30 s Maximum dosing volume： 50.00 ml Unit values Unit size： 20mlnl Unit ID： 10039060 Reagent： HCl 1 mol/l Batch ID： no entry Concentration[mol/l]： 1.00000 Determined at： 06/27/1216：03：58 Expire date： Opened/compounded： Test according ISO 8655： Last modification： 06/27/129：04：36 Application Notes If you have any questions on the application， you can feel free to contact us.. 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