In-line measurement and correction of Color and physical properties Symposium on Color and Appearance Instrumentation April 15-16, 2003 Chicago, IL Girish Malhotra, President, EPCOT International, Pepper Pike, OH, USA Carlos Arthur Peixoto, Process Engineer, Eduardo Schotgues, Software Engineer, Paulo R. Pfeil Instrument Engineer- NTP Production Technology Center, Renner Herrmann SA, Porto Alegre, Brazil

CHARACTERISTICS MEASURED COLOR PHYSICAL PROPERTIES DISPERSION PARTICLE SIZE It is necessary to measure and match color and other properties for the production of any colored liquid. A sample is taken off-line and the necessary tests are done to determine deviation from the goal. Adjustments are made and the test process repeated till the specifications are met. This repeated process can and does prolong the batch cycle time. If the solvent is lost after the specifications have been met, it may add additional complexity. All these add cost to the product. Once the specifications are met the batches are not checked and if there is specification variation, no adjustments are made to meet specifications.

IF SPECS CAN BE CORRECTED AND MET WITHOUT SAMPLING BENEFITS WILL BE: REDUCED PROCESS CYCLE TIME IMPROVED PROFITABILITY HIGHER AND CONSISTENT QUALITY In today world the specifications are checked by taking a sample off-line. If the colored liquid specifications can be measured in line as the product is being produced, the user of our technology will improve profitability by reducing the batch cycle time. The user can also improve quality of their products.

TECHNOLOGIES COLORCELL (REFLECTION ONLY) MULTICELL (TRANSMITION AND REFLECTION) We have two technologies that can allow one to measure the characteristics of the colored liquids without taking a sample off-line.

COLORCELL TECHNOLOGY SCHEMATIC Spectrophotometer Reflection Fixed Plate WIPER Liquid Fixed Plate Colorcell Technology is a reflection only technology. The liquid passes between two fixed plates and the color of the liquid is read using a commercially available spectrophotometer. There is a wiper in the cell that cleans the glass periodically to keep it clean. Figure 1

MULTICELL TECHNOLOGY SCHEMATIC Spectrophotometer Transmission Reflection Fixed Plate WIPER Liquid Movable Plate Transmission Multicell Technology also has two plates but the lower plate is a movable plate. It can move between 20 to 3000 microns to create a liquid film. A white light passes through the film and it transmission is measured. We can also measure the reflection of the liquid. Thus this technology can read transmission and reflection. Wiper are used to prevent any build up of the coating on the glass substrate. White Light Figure 2

MULTICELL Figure 3 Electronic finger print is created and matched. Multicell creates a three dimensional finger print for a liquid. This is matched as the product is produced. Electronic finger print is created and matched. Figure 3

TECHNOLOGY APPLICABILITY COATINGS (ARCHITECTURAL, AUTOMOTIVE, WOOD, INDUSTRIAL, PAPER) PRINTING INKS PIGMENT AND DYE DISPERSIONS TEXTILES COLORANTS COSMETICS FOOD MINERALS Our technology can be used in these businesses.

MULTICELL TECHNOLOGY WHITE LIGHT vs. WHITE BASE REFLECTION AND TRANSMISSION THROUGH FILM MEASURED CONTINUOUSLY ELIMINATES USE OF WET STANDARDS CONTINUOUS COLOR, STRENGTH AND HIDING POWER MEASUREMENT CONTINUOUS VISCOSITY, DENSITY AND TEMPERATURE FEED RATES ADJUSTED IN LINE TO PRODUCE QUALITY The Multicell technology uses a white light vs. white base. Use of white light eliminates human intervention and errors. This eliminates the use of wet standards, another potential source of human error. We measure reflection and transmission continuously for a product (batch or continuous). This allows us to continuously control the desired performance and physical properties. This is accomplished by adjusting feed rates of various liquids and only QUALITY is produced. Since we have eliminated significant human intervention, our technology reduces batch cycle time. This not only reduces costs i.e. improves profitability, it also increases plant throughput with minimal or no investment. ROI is very high.

TECHNOLOGY (cont.) DEVELOPED BY RENNER HERRMANN, S. A. COMMERCIAL Du Pont Performance Coatings Automotive refinish coatings (Brazil) E. I. du Pont - Mt Clemens Automotive primers (Michigan) Renner Sayerlack (Brazil) CADAM ( Caulin do Amazonas ) Other installations underway

FINANCIAL IMPACT INVENTORY INTEREST OBSOLESCENCE MANUFACTURING COST REDUCED WASTE SERVICE AND QUALITY These factors influence profitability of a company using our technology to produce coatings, colorants, inks, dyes, pigments, cosmetics.

FINANCIAL IMPACT Savings 15-25% We believe that companies using our technology can achieve savings of about 15-25%. These savings are business dependent.

MANUFACTURING CONFIGURATION Final Product MANUFACTURING CONFIGURATION Liquid 2 Liquid 1 Liquid 3 Tank MULTICELL Liquid 4 MIXER Liquid 5 Various liquid ingredients are metered to a small agitated mixer. A small volume of the mixed liquid is sent to the cell where its color characteristics are compared against the standard. If different from the standard, automatic flow rate adjustments are made to the flow rate of the liquids going to the mixer. Majority of the flow from the mixer is sent to the Recycle Tank. This liquid is also sent to the mixer and its flow is controlled. As soon as the specifications are matched, the liquid being sent to the Recycle Tank is diverted to its final destination. The liquid in the Recycle Tank is fed to the mixer so that at the end of the run there is nothing left in the tank. We measure and control physical properties so that besides color we have control of viscosity and density also. As long as the product is being produced a small portion is sent to the cell for quality check. Advantages of this method are no waste is produced. Quality from the first to the last can or drum is exactly the same. The system is cleaned very quickly and a new product of any desired color can be produced. Liquid 6 Liquid 7 Recycle Tank Liquid 8 Figure 4

TEST RESULTS Some results of the measurement using the Colorcell and the Multicell are shared.

KAOLIN We tested different composition kaolin slurries through the Colorcell. Table 1

CONVENTIONAL DRY METHOD Reflectance results using the conventional dry method are illustrated. Figure 5

WET METHOD USING COLORCELL We can measure and differentiate each of the slurries. This allows us to control the exact composition of kaolin in wet state giving manufacturing greater control on the manufacturing process, quality and costs. Figure 6

Figure 7 Wet DE =0.24 Dry DE =0.22 Yellow solvent coating This slide shows the results of a yellow solvent based coating using Colorcell. The wet and dry method results are compared. The difference between the samples and their standards is negligible. However the wet liquid testing allows the product specifications to be met in much shorter time. Corrections are done as the product is produced rather than after all has been mixed. The dry testing may require multiple corrections. Wet DE =0.24 Dry DE =0.22 Yellow solvent coating Figure 7

Figure 8 Wet DE =0.27 Dry DE =0.28 Blue solvent coating This shows reflectance of a blue solvent based coating. Wet DE =0.27 Dry DE =0.28 Blue solvent coating Figure 8

WOOD COATING DYE Figure 9 Reflection Dry Curves 100 90 80 70 60 %R 50 STANDARD 70 BATCH 60 %R 50 40 30 20 The next three slides show the results for a wood coating using the Multicell. Fig. 9 shows the reflectance using the conventional method. We added 1% dye to the standard and measured the batch reflectance. 10 400 450 500 550 600 650 700 NM Figure 9

WOOD COATING DYE Figure 10 Multicell Transmission (20µm) 100 90 80 Standard 70 Batch 60 %T 50 40 30 20 This slide shows the transmission of the same two liquids using a 20 micron path length. The samples were measured as is, without dilution. 10 400 450 500 550 600 650 700 NM Figure 10

WOOD COATING DYE Figure 11 Conventional Method 100 90 80 70 60 %T Standard 50 Batch 40 30 20 10 This slide shows the transmission using the conventional method. In the conventional method the samples have to be diluted. 400 450 500 550 600 650 700 NM Figure 11

WOOD COATING DYE Figure 12 Relation between Kstd and Kb 2.50 2.00 1.50 Kstd/Kb(Multicell) Kstd/Kb (Conventional) 1.00 0.50 0.00 Figure 12 compares the absorption coefficient (Lambert-Beer’s Law) for the Multicell vs. the conventional method. The results are very comparable. Since we have an excellent correlation between the two test methods, the wet test method would be a preferred method as it will improve profitability by reducing cycle time, waste and inventories. The K (absorption coefficient) for the two samples calculated by the equation: T = e-K*C*X Where: T = Transmittance C = Concentration X = Path length thickness K = absorption coefficient 400 450 500 550 600 650 700 NM Figure 12

COLORANT EXPERIMENT ITERATION USING MULTICELL This table shows results for a colorant. This table shows how we started with a hypothetical formula to meet a certain specification. The liquid “uncorrected” was passed through the cell. Based on the standard stored in the system, the software made a correction shown in the next column. The first correction shows proximity to the standard as illustrated by Dtransmission , Dreflection and strength. Table 2

This graph shows the comparison of the standard, uncorrected and first correction sample. The speed and accuracy illustrates the value of the technology to the manufacture of colored liquids. Figure 13

SUMMARY TECHNOLOGY IS COMMERCIAL. PRODUCTS DEVELOPED IN ANY PART OF THE GLOBE CAN BE PRODUCED AT THE MOST COST EFFECTIVE PLACE. TECHNOLOGY CAN BE RETROFITTED IN EXISTING PLANTS. MARKET AND PRODUCT DEVELOPMENT TIME IS SIGNIFICANTLY REDUCED.

QUESTIONS THANK YOU VERY MUCH. CONTACT: Girish Malhotra, P.E. EPCOT International 29150 Bryce Road Pepper Pike, OH 44124 epcotint@ix.netcom.com 216-292-0626(P) 216-591-0932(F) http://www.epcotint.com Profitability through Simplicity