Titanium Dioxide in
Masterbatch
Revy Saerang (4005330)
December 9, 2011
Advanced Analytical Chemistry
Buzzword: 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.1
1//www.clariant.com/C125766B004CDFBC/vwWebPagesByID/04872E207B80A989C12568CE003E269A
(accessed on November 29, 2011)
Masterbatch Process
Problem
•
Titanium Dioxide
– Titanium id a refractory metal2.
– Inorganic nanoparticle that is used extensively in masterbatch production as a
white pigment, opacifier for colored systems and UV stability agent.
– Incorporated with additives, resins in colored masterbatch production.
• Titanium Dioxide in Masterbatch industry
– Titanium dioxide is a central ingredient to imparting clean, bright whites, or fine
tuning the shades of color for the right eye appeal 2.
– The actual amount and particle size of TiO2 will affect the shades of the right
appeal due to changes in its scattering efficiency, photocatalytic effect 3.
– Reformulation and remixing need to be done when the batch production does not
meet the right appeal or specification and this affects cost of manufacturing,
production schedule, customers’ satisfaction.
2 www2.dupont.com/Titanium_Technologies/en_US/products/104/R104_Intro_Brochure.pdf
Accesed on (Nov 29, 2011)
3Fisher, J. and Egerton, T.A.2001. Titanium Compounds, Inorganic. Kirk-Othmer Encyclopedia of Chemical Technology
Hypothesis
• Hypothesis
– The actual content and the particle size of titanium dioxide
(pigment) in masterbatch formulation in comparison to other
components (oxidant reagent, wax, resin) has lead to nonhomogeneity of mixing and to cause a hindrance of pigments
to perform optimized coloration and pigmentation.
Possible Analytical Methods
Analytical
Methods
Advantages
Disadvantages
Size Exclusion
Chromatography
Good separation of large and small
molecule, good sensitivity
It is normally combined
with other characteristics
(acidity, charge), limited
number of bands
ICP-MS
Easy sample introduction, quick
analysis, low detection limit,
accurate, capable of trace at part
per trillion level
Expensive, interferences
from plasma gas, matrix
effects
X-ray
Fluorescence
Spectrometry5
High precision, determine major
element, detect several thousands
atoms
Expensive, 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., 44:251-296
ICP-MS
Sample diluted
in HNO3
• The sample is nebulized using a
method of slurry nebulization into
a the inductively coupled plasma,
and a fine mist is created as
high velocity argon, then in hot
plasma the fine droplets are
atomized then ionized. Sample
ions are passed into MS system
at vacuum using quadrapole
mass filter where the ion will be
observed at a specific m/z ratio
at a vacuum chamber
Sample 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 analysis
4Guoqiang
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:1378-1385
Experimental Procedure
• Determine masterbatch productions for ones that always
need reformulation in QC lab.
• Disperse sample in an acidic medium, followed by direct
nebulization of suspension into the ICP.
• Determine how much is the actual content of titanium
dioxide using a quantitative technique.
• Obtain calibration curve for standards for these above
productions using a similar procedure listed above by
ranging the actual content of TiO2 and particle sizes.
– Use this to analyze the current productions and to take measures
on what should be done for future production.
Results
• When using aqueous solution in SN-ICP-MS, the mean
particle is the most important for the analytical
accuracy. Under optimized ICP-MS condition the result
show that maximum scattering visible light (400-700
nm) light occurs for pigment particles of 300 nm and the
scattering efficiency decreases rapidly as the particle
size varies6. Mass spectrometry determines the actual
content of titanium dioxide in masterbatch production
can be quantified and this is significant in optimizing the
formulation of masterbatch production
6 Fisher,
J. and Egerton, T. A. 2001. Titanium Compounds, Inorganic. Kirk-Othmer
Encyclopedia of Chemical Technology
Conclusion
• Best separation technique is Slurry NebulizationInductively Coupled Plasma-Mass spectrometry (SNICP-MS).
– 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.
References
1.
2.
3.
4.
5.
6.
7.
Clariant Corp. Masterbatches Profile. 2011
<//www.clariant.com/C125766B004CDFBC/vwWebPagesByID/04872E207B80A989C12568CE003E269A>
(accessed on November 29, 2011)
Dupont. DupontTM Ti-Pure R-104 titanium dioxide.
<www2.dupont.com/Titanium_Technologies/en_US/products/104/R104_Intro_Brochure.pdf > Accesed on
(Nov 29, 2011)
Fisher, J. and Egerton, T.A.2001. Titanium Compounds, Inorganic. Kirk-Othmer Encyclopedia of Chemical
Technology
Guoqiang 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:1378-1385
Potts, P.J and Webb.P.C. X-ray Fluorescence Spectrometry [Online]. In: G.E.M Hall (Editor).
Geoananalysis. J. Geochem. Explor., 44:251-296
Fisher, J. and Egerton, T. A. 2001. Titanium Compounds, Inorganic. Kirk-Othmer Encyclopedia of
Chemical Technology
Skoog, D.; Holler, F.; Crouch, S. Principles of Instrumental Analysis, 6th ed