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U of M CHEM 4101 - Titanium Dioxide in Masterbatch

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Titanium Dioxide in MasterbatchBuzzword: Masterbatch What is it?BackgroundHypothesisPossible Analytical MethodsSample Preparation4ICP-MS (Inductively-Coupled Plasma with Mass Spectrometry)Agilant 7500a ICP-MS7ResultsAlternative TechniqueConclusionReferencesTitanium Dioxide in MasterbatchRevy Saerang (4005330)December 9, 2011Advanced Analytical ChemistryBuzzword: Masterbatch What is it?•Color-pigmented material for plastic industry–Packaging (Food, beverage, cosmetic), computer hardware, automotive parts, etc. Use to insert colors and impart special properties to plastic products.–1-2 % contribution in cost of production but master batch drives the quality, durability of the plastic product.11Clariant Corp. Masterbatches Profile. 2011 <//> (accessed on November 29, 2011)Background•Titanium Dioxide in Masterbatch Industry–Inorganic nanoparticle. –It is used extensively in masterbatch production as a white pigment, opacifier for colored systems and UV stability agent3.–a central ingredient to imparting clean, bright whites, or fine tuning the shades of color for the right eye appeal2.2 Dupont Titanium Dioxide Ri-104 Brochure. Dupont Corp. Accesed on (Nov 29, 2011)3Fisher, J. and Egerton, T.A.2001. Titanium Compounds, Inorganic. Kirk-Othmer Encyclopedia of Chemical TechnologyHypothesisThe actual content and the particle size of titanium dioxide in masterbatch formulation has a significant effect in non-homogeneity of mixing of masterbatch formulation and to cause to reduce optimized pigment colorationProblemReformulation of masterbatch production when the batch production does not meet the right appeal or specification and this affects cost of manufacturing, production schedule, customers’ satisfaction.Possible Analytical MethodsAnalytical MethodsAdvantages DisadvantagesSize Exclusion ChromatographyGood separation of large and small molecule, good sensitivity, CheapIt is normally combined with other characteristics (acidity, charge), limited number of bandsICP-MS Easy sample introduction, quick analysis, low detection limit, accurate, capable of trace at part per trillion levelExpensive, interferences from plasma gas, matrix effectsX-ray Fluorescence Spectrometry5High precision, determine major element, detect several thousands atomsLow cost, space limitation on sample, high scattering, low detecting intensities 5 Potts, P.J and Webb.P.C. X-ray Fluorescence Spectrometry [Online]. In: G.E.M Hall (Editor). Geoananalysis. J. Geochem. Explor., 44:251-296Sample Preparation4•Collect sample powder and dilute with nitric acid to give required acid concentration and add distilled water to adjust volume.•Add 0.01% (m/v) of PVA (Poly Vinyl Alcohol) as a dispersion agent and stabilizer•In a beaker, use magnetic stirrer and stir for 10 minutes to ensure homogenization before it is nebulized.•Use an ultrasonicator and shake the flask vigorously for around 30 minutes prior to analysis4Guoqiang X, Bin H, Zucheng J and Chuqing. A comparison of slurry sampling electrothermal vaporization and slurry nebulization inductively coupled plasma mass spectrometry for the direct determination of trace impurities in titanium dioxide powder. Journal of Mass Spectrometry. 2006:41B:1378-1385ICP-MS(Inductively-Coupled Plasma with Mass Spectrometry)•Fine mist is extracted using high velocity Argon (14-18 L/min)12•Atomization and ionization process at ICP torch•Couple with MS, ions are passed at vacuum condition•Through mass filter, ions separate at specific m/z ratio.•A detector receives an ion signalproportionalto the concentrationSlurry nebulized sampleFine droplets of mistTemperature of plasma at the order of 10,000 K10 Inductively Coupled Plasma Mass Spectrometry. Advanced Technologies Department. [Online].2011 <> Accessed on Dec 7, 2011Agilant 7500a ICP-MS7•Dynamic Range>1000 ppm•Wide range of detection limit•Extreme Sensitivity > 500 Mcps/ppm•Price: $64,00088 Agilant Technologies. Agilant 7500a ICP-MS brochure.<> Accessed on Dec 3, 2011.9 Agilant Technology. Agilant 7500a ICP-MS pricing.<> accessed on Dec 3, 2011SpecificationsICP Source: 27.12 Mhz (max.1600 W)Mass analyzer: QuadrapoleDetector: Electron multipierPressure: Vacuum systemMass range: 2-260 amuResults•The bar chart show how the particle size of titanium dioxide affect the relative signal intensity4 (intensity  content of titanium dioxide)•Scattering efficiency decreases rapidly as particle size varies (Figures with masterbatch with different particle size)66 Fisher, J. and Egerton, T. A. 2001. Titanium Compounds, Inorganic. Kirk-Othmer Encyclopedia of Chemical Technology12 DuPont Ti-Pure titanium dioxide. DuPontTM<> accessed Dec 8, 2011 Particle size12B/R=Blue/Red reflectence valuesAlternative Technique•X-Ray Fluorescence SpectrometryLow cost (~$4000)Rapid analysisConvenient for solid sample: disk sample11Precise, comparably sensitiveMore complex detection and calibration method11X-Ray Fluorescence Spectroscopy Unit. Network of Research Supporting Laboratories <> accessed on Dec 7, 2011Conclusion•Slurry Nebulization-Inductively Coupled Plasma-Mass spectrometry (SN-ICP-MS) can be used to quantify the actual content of Titanium Dioxide and recognize the particle size effect.•Particle size of titanium dioxide and the actual content of titanium dioxide in one formulation of masterbatch production is significantly important in determining the right shade of color appeal due to its photocatalytic effect, scattering efficiency, and other optical properties.References1. Clariant Corp. Masterbatches Profile. 2011 <//> (accessed on November 29, 2011)2. Dupont. DupontTM Ti-Pure R-104 titanium dioxide. < > Accesed on (Nov 29, 2011)3. Fisher, J. and Egerton, T.A.2001. Titanium

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