IN-LINE PARTICLE SIZE MEASUREMENTS FOR CEMENT AND OTHER ABRASIVE PROCESS ENVIRONMENTS 1998 A.P. Malcolmson Malvern, Inc. 10 Southville Road Southborough, MA D. J. Holve Malvern/Insitec, Inc. 2110 Omega Road, Suite D San Ramon, CA 94583 For Presentation at the: IEEE/PCA 40 th Cement Industry Technical Conference May 1998 Rapid City, South Dakota 1
1.0 INTRODUCTION Cement manufacturers have historically been interested in implementing process control strategies to aid in production process QA/QC. Real-time measurement of Blaine number is of particular interest, since this is the primary measurement that cement producers use to gauge quality and strength of the final product. The three major hindrances to widespread application of in-line Blaine number measurement instrumentation in the past have been: i) fragility of available instrumentation, ii) inability of existing instrumentation to resolve small changes in material properties, and iii) lack of an effective means to directly measure Blaine number, or functional properties of the Blaine number. A recently introduced ensemble particle size and concentration sensor has successfully addressed these issues, enabling active process control in production environments. 2.0 LIGHT SCATTERING METHODOLOGY Figure 1: The Ensemble Particle Concentration & Size Sensor The process particle measurement technology is based on the now classical ensemble laser diffraction technology, which is widely used in laboratory measurement instruments. This system consists of a ruggedized sensor head, electronics box, and remote computer. The dimensions of the particle flow access region define the particle sensing region or sample volume. Particles may pass anywhere along the length of the exposed laser beam. Particle velocity does not affect the measurement. As particles pass through the laser beam, light scattered in the forward direction is collected by the receiver lens and focused onto a log-scaled annular ring detector. The detector is scanned at high speed by the interface card, which records the signal levels on each ring. These signals are sent over a digital interface and stored for analysis. Each ring on the detector measures total signal intensity. Each particle scatters light on all the rings of the detector. Therefore, the scattered light is the summation of all the light scattered from 2
all the particles. Once a significant number of detector scans is acquired, the software uses a non-linear inversion technique to solve for the relative particle concentration. The instrument matrix for the solution is defined by the theoretical scattering dependent on the refractive index of the particles and carrier. No assumptions are required about the shape of the size distribution, obtained directly from the experimental scattering information. For cement applications a standard process instrument (as shown in Figure 1) is hardened for the corrosive and abrasive nature of the material. The original application of this technology was in process environments involving high value products, such as toners and pharmaceuticals. The primary issue that had to be addressed in developing an instrument specifically for the cement industry was mechanical wear of the surfaces that were exposed to this highly abrasive material. After testing different designs under a range of operating conditions, acceptable component wear life was achieved by incorporating abrasion resistant ceramics in the high velocity sections of the flow system coupled Figure 2: The process interface. with a combination of hardened and tungsten coated steel in other, less abrasive locations. This configuration has eliminated mechanical wear in the regions that could not tolerate abrasion, and has provided acceptable lifetimes (greater than 2 years) for the low cost, replaceable components. The instrument is affixed to the process stream via an auger feeder, which moves a representative fraction of the primary flow from the main process stream (typically an air-slide) to a secondary stream, and hence to a venturi eductor driven by compressed air which moves material from the secondary flow to the sensor head. The venturi functions as both a pump and a dispersion device to ensure that the powder is completely de-aggregated. The material passes through the optical sensor and is returned to the process stream (as depicted in Figure 2). Installed, the instrument is integrated as part of the process line (Figure 3). This method for interfacing the device to the process flow achieves a uniform and representative particle flow to the detector. Automatic valves, controlled by the instrument software are installed at the inlet to the sensor allowing for automatic background measurements and maintenance of the equipment without interrupting the primary process flow. Aside from the abrasion and corrosion resistance requirements, a critical requirement for operation of this instrument is long-term maintenance of clean sensor windows by means of a 3
Figure 3: A Cement Installation with electronics and air controls. 4
pneumatic purge system. The fluid-dynamic design of this interface is important for providing long term operation without dust fouling. The critical elements of this design require avoidance of particulate recirculation near the windows (which are recessed from the powder flow). Once fine particles contact the windows, it is not possible to clean them by air-purging, even at high velocities because of strong electrostatic charging of small particles. Purge velocities are chosen to exceed primary flow velocity and must be maintained at all times. However, if the windows do become contaminated, access is provided to clean the windows with lens paper, an operation that requires about 15 minutes. The purge flow velocity designs have evolved through a combination of intuition and testing. Current cement users report cleaning maintenance periods of one month. 2.1 RANGE AND ACCURACY The in-line instrument gives the user the same degree of measurement accuracy in-line as is achievable using available off-line laboratory particle size analyzers. Figure 4 illustrates measurements of a single type of cement under three different operating conditions. The laser attenuation values of 20%, 50%, and 70% represent increasing particle concentrations that would be expected in typical cement production processes. The data analysis uses a patented algorithm which is capable of measurements over the range of 5%-95% light attenuation. 1,2 Typical laboratory instrumentation is limited to light attenuation less than 50%. In general, this limitation is not critical for laboratory applications because one can dilute the sample appropriately. However, a much broader range of adaptability is important for process applications, where particle concentrations can vary widely in an unpredictable manner. 2.2 QUALITY ASSURANCE TOOL The laser diffraction particle size measurement technique employed by the process instrument varies greatly from the packed-bed pressure-drop method that the typical Blaine number measurement device utilizes. However, a recent measurement sensitivity analysis has verified that the optical instrument was easily able to resolve the 7% variations in Blaine numbers of the samples tested. In addition a good correlation exists between the laser diffraction Blaine and pressure drop Blaine measurements. (Figure 5). To develop this correlation, various samples of a particular type of cement that represented the high acceptable, low acceptable, and average acceptable Blaine characteristics (i.e. the control range of interest) were measured. Blaine apparatus measurements were then performed on these samples by the product manufacturer, and compared with the analysis performed at Insitec using optical technique. The results in Figure 5 indicate that the Blaine number (or Specific Surface Area, SSA) yielded by the instrument can be used as a surrogate for a pressure drop Blaine analysis. The optical instrument determines the specific surface area by effectively integrating the light scattering from individual particles. Note that there is not an exact numerical comparison between the two techniques, and that no error bar uncertainties have been assigned to the measured Blaine numbers. Allen 3 has analyzed the reliability of the Blaine concept and states: The assumptions made in deriving the Carman-Kozeny equation (on which the Blaine number is based) are so sweeping that it cannot be argued that the determined parameter is a surface and The determined surface areas are usually lower than those obtained by other measuring techniques. This last comment is obviously consistent with the current optical results, which give higher values than the Blaine 5
120 100 20% Laser Attenuation 50% Laser Attenuation 70% Laser Attenuation 80 60 40 20 0 0.1 1 10 100 Particle Size (microns) Figure 4: Comparison of Type 20 Cement Particle Size Measurements at Three Different particle concentration conditions. 6
4400 4200 20% Laser Attenuation 50% Laser Attenuation 70% Laser Attenuation 4000 3800 3600 3400 3200 3000 3000 3200 3400 3600 3800 4000 4200 4400 Manufacturer Blaine Measurement Figure 5: Comparison of Optical Blaine Number Measurements With Cement Manufacturer Blaine Apparatus Measurements. 7
number. Dr. Allen points out a range of other limitations for permeametry techniques. Thus we conclude that the precision and accuracy of the Blaine number is limited. From an operational point of view, the Blaine test takes time, which delays optimal mill/classifier adjustment. Over-grinding increases energy consumption, while under-grinding reduces product quality. The ideal goal is to meet quality requirements and maximize production rates (use of capital equipment) with minimum energy consumption. A current optical instrument user has found a 3-fold reduction in product variation from 8-10% down to 3%. Although some customers still require Blaine tests, these measurements are more a confirmation of the optical instrument results. 4 3.0 LONG-TERM COMPARISON OF OPTICAL SSA AND BLAINE MEASUREMENTS These initial successful comparisons of Blaine and SSA measurements encouraged more comprehensive test comparisons. Figure 6 shows the results for a two week test series comparing independent Blaine results and the optical SSA. The SSA values were normalized to the Blaine number results by a constant determined in a previous test series. On this graph we have indicated the Blaine number error bars for one standard deviation (approximately 1.5% as estimated by ASTM for an individual technician. For multiple technicians it is known that different techniques may be used and the standard deviation would be of the order of 2.5%. Note that the two different measurement techniques agree quite well, with a few data points at the beginning and end of the test series showing deviations exceeding 1.5%. We have not applied an error bar to the optical instrument measurements, but let us assume that it is of the same order, namely 1%-1.5%. The error bars of the two sets of measurements would overlap in all cases, indicating that the two techniques are statistically in agreement. That is, there is no statistical discrimination for choosing one method as being more accurate or precise than the other one. However, there remains a natural prejudice that the traditional Blaine number is the de facto standard when a new technique is in disagreement. How can we resolve this question? One of the production parameters that can be correlated with these measurements is the production rate, which is a measure of the mill throughput of clinker. In general, it is well known that a higher throughput of material leads to less milling and thus a smaller SSA, i.e. the material is not ground as finely. This trend is clearly seen in comparing the production rate with SSA or Blaine in Figure 7. The data for production rate has been modified to delete large excursions in the feedrate for better comparison with the two surface area measurements. In other words, for statistical comparison, we have selected only near steady state conditions. We can then perform independent correlations of the productivity with each surface area measurement. Figure 8 shows the comparison with the Blaine measurement, giving an R 2 value of 0.362. Given the Blaine measurement uncertainty of 1.5%, this weak correlation is not too surprising. A similar correlation of production rate with the optical SSA measurements (Figure 9) shows a much tighter correlation with an R 2 value of 0.746. This stronger correlation gives evidence that the SSA is providing superior precision in comparison to the Blaine results. 8
430 Lab Blaine & EPCS SSA vs Time 420 410 SSA(m2/kg) Blaine 400 390 380 370 360 350 8/4/97 0:00 8/6/97 0:00 8/8/97 0:00 8/10/97 0:00 8/12/97 0:00 8/14/97 0:00 8/16/97 0:00 Time (days) Figure 6: Comparison of Blaine Number measurements with Optical SSA over a 12 day period. 9
SSA/Blaine vs. Production 420 60.0 410 400 55.0 390 380 50.0 370 360 350 340 SSA(m2/kg) Blaine Production Rate 45.0 40.0 330 320 35.0 8/4/97 0:00 8/6/97 0:00 8/8/97 0:00 8/10/97 0:00 8/12/97 0:00 8/14/97 0:00 8/16/97 0:00 Time (days) Figure 7: Comparison of cement production rate with Blaine Number and Optical SSA measurements over a 12 day period. 10
Production Rate vs. Blaine 70.0 60.0 50.0 Production rate 40.0 30.0 20.0 y = -0.0914x + 84.843 R 2 = 0.362 10.0 0.0 330 340 350 360 370 380 390 400 410 420 Blaine Number Figure 8: Correlation of production rate with Blaine Number measurements for the data of Figures 5 and 6. 11
Production Rate vs. EPCS SSA 70.0 60.0 50.0 40.0 y = -0.1643x + 112.21 R 2 = 0.7465 30.0 20.0 10.0 0.0 330 340 350 360 370 380 390 400 410 SSA (EPCS) Figure 9: Correlation of production rate with Optical SSA measurements for data of figures 5 and 6. 12
4.0 CONCLUSIONS For many decades the Blaine measurement has provided a reasonable industry standard for predicting ultimate strength of cements. However, improving production efficiency while maintaining even tighter quality control continues to motivate development of better measurement techniques. The real-time monitor provides two specific advantages: Measurement of the complete size distribution in addition to the Blaine or specific surface area. Real time measurement (up to 1 second intervals) for monitoring and/or process control. Even though the real time optical instrument is primarily used as a quality control tool, it is also a productivity tool, which allows for more efficient use of capital resources, and reduction of specific energy consumption. This document last revised 2/24/98 by HNN. This document approved for public release. This document is located at: \\INSITEC2\MAIN\Marketing\EPCS Items\IEEE Cement Paper\In-line Particle Size Measurements for cement and other etc.doc 1 United States Patent #5,619,324 2 T.L. Harvill, J.H. Hoog, and D.J. Holve, In-Process Particle Size Distribution Measurements and Control, Particles & Particle Systems Characterization 12(1995), 309-313. 3 Allen, Terence, Particle Size Measurement, Vols. I&II, 5 th Edition, Chapman and Hall, 1997 4 Powder and Bulk Engineering, Article to be published, Spring 1998 13