Comparison of Macrostickies Measurement Methods
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Contaminant Catalog Comparison of Macrostickies Measurement Methods Mahendra R. Doshi, Progress in Paper Recycling, Appleton, WI. William J. Moore, Fox Valley Technical College, Appleton, WI. R. A. Venditti, K. Copeland and H-M. Chang, North Carolina State University, Raleigh, NC. Hans-Joachim Putz, Chair, Paper Technology and Mechanical Process Engineering, Darmstadt, Germany. Thierry Delagoutte, Centre Technique du Papier, Fibre Resources Division, Grenoble, France. Carl Houtman, Freya Tan, Lisa Davie and Gregg Sauve, USDA Forest Products Laboratory, Madison, WI. Tim Dahl and Dave Robinson, Stora Enso Duluth Recycled Pulp Mill, Duluth, MN. ABSTRACT ever, we were surprised to see excellent linear correlation among all methods for both laboratory as well as mill Pulp containing PSA was prepared in the laboratory and samples. As a result, we can conclude that any one of the blended with sticky-free pulp in four different proportions. methods seems to be suitable for monitoring stickies con- The four pulps were then dewatered and shipped to four tent but one cannot compare actual values from different laboratories for the evaluation of macro stickies in terms methods as they may vary significantly. of mm2/kg. Also, five pulp samples from specific loca- tions in a deinking mill were dewatered and shipped to the same four laboratories. KEYWORDS Methods used by these laboratories include: Adhesives, Contaminants, Enzyme, INGEDE, 1. Black ink method Macrostickies, Measurement methods, Microstickies, Re- 2. INGEDE method covered Papers, Stickies. 3. Enzyme digestion method 4. Blue dye method INTRODUCTION Details of these methods are presented in Appendices 1 to 4. All laboratories used slotted screens to separate One of the problems in paper recycling is due to stickies - macrostickies and other contaminants from the pulp. adhesives and binders used in coating, printing convert- Screen slot size varied from 80 mm to 150 mm. In addi- ing applications, labels and envelopes. The problem is tion, researchers at FPL made handsheets directly from compounded due to the variety of stickies in terms of chemi- pulp samples without a screening step. Hydrophilic black cal composition and viscoelastic behavior (1). Further- ink, hydrophobic blue dye, or carbon black was used to more, our inability to quantify them hinders the progress improve contrast between contaminants and fibers. in paper recycling. Many quantification methods have INGEDE method used alumina powder to distinguish be- been proposed but we do not yet have a rapid, reliable and tween tacky and non-tacky contaminants. Interfering fi- reproducible method for measuring the concentration of ber bundles were removed by enzyme digestion by stickies. Our objective is to compare some of the methods researchers at the CTP. All methods employed image used for the quantification of macrostickies. analysis to determine the average number and size of con- taminants. The details of the image analysis methods were We prepared synthetic stickies pulp in laboratory and not standardized. shipped to four participating laboratories for analysis. We also took samples from a deinking mill and shipped to the In view of the significant differences in the methods used same four participating laboratories for analysis. The to measure the concentration of macrostickies, it is not sample preparation procedure is described below while surprising to see considerable variations in actual values details of the measurement methods are given in the ap- of stickies area reported by the participating groups. How- pendices. Page 34 Progress in Paper Recycling / Vol. 12, No. 3, May 2003 LABORATORY SAMPLES Avery 8162 Ink Jet Labels (34 mm X 102 mm) were ap- plied to virgin bleached kraft market pulp. Pulp sheets with labels were stored for at least 24 hours followed by shredding by hand and pulping. A high consistency labo- ratory pulper with helical rotor was used to generate sticky pulp. Pulping was carried out at 14% consistency at room temperature - about 20 °C to 25 °C. The procedure was repeated but this time without labels to generate sticky- free pulp. Four pulp samples were prepared by mixing various proportions of sticky-containing pulp and sticky- free pulp as shown in Table 1. We also tried to apply hot melt to virgin pulp but it did not adhere very well. Hot melt containing sheets were pulped together with sheets containing PSA labels. However, the hot melt material came out in the form of large “plastic” pieces. This material was therefore ignored in our analy- sis. After mixing pulp samples in the proportions shown in Table 1, the samples were dewatered and stored in a cold room prior to shipping. All participants were asked to dilute each pulp sample to less than 1% consistency prior Figure 1. Block flow diagram for Stora Enso Duluth to withdrawing the necessary amount for stickies measure- Recycled Pulp Mill, Duluth, MN. (See Table 2 for the ment. All participants were requested to make description of sample points identified as PCF, PFF, LCA, macrostickies measurements in triplicate. PFA and DIP.) Table 1. Laboratory sticky pulp samples Table 2. Samples collected at Duluth Re- Weight % Weight % cycled Pulp Mill Sample Sticky Pulp Sticky-Free Pulp Mill Description Sample 1 Samples 1-Lab 100 0 PCF Primary coarse Screen Feed 2-Lab 75 25 FFF Primary Flotation Feed 3-Lab 50 50 LCA Light Cleaner Accepts 4-Lab 25 75 PFA Primary Fine Screen Accepts DIP Deinked Pulp MILL SAMPLES MACROSTICKIES MEASUREMENT METHODS Five pulp samples were collected from an office paper deinking plant in Duluth. A block flow diagram of Stora Four methods, described in detail in Appendices 1 to 4, Enso DRPM (Duluth Recycled Pulp Mill) is the same as were used to measure the concentration of macrostickies that published earlier (2) and is shown in Figure 1 to- in pulp samples. In the first method, Black Ink Method gether with sample points. Note that four of the five pulp (Appendix I), Pulmac 150 µm (0.006”) slotted screen re- samples were taken before dispersion while only one pulp jects are collected on a white filter paper and dried. The sample was taken after dispersion due to a relatively in- filter paper is then dyed with black hydrophilic ink. Cel- significant variation in macrostickies content after that lulose fibers appear black while hydrophobic stickies par- point. Samples are designated as shown in Table 2. ticles appear light colored in a black background. Samples were dewatered and shipped to all participants. As in the analysis of the laboratory samples, participants The first few steps of the INGEDE method (Appendix 2) were advised to dilute each pulp sample to less than 1% are same as the above Black Ink Method, namely, collect consistency prior to withdrawing the necessary amount for rejects on a white filter paper and dye them with water stickles measurement. All participants were requested to soluble black ink. To distinguish between sticky and non- make macrostickies measurements in triplicate. sticky particles white alumina powder is sprinkled on the Progress in Paper Recycling / Vol. 12, No. 3, May 2003 Page 35 filter paper. It is then covered with a heavy plate and dried RESULTS AND DISCUSSION in an oven to fix alumina powder to stickies. Excess alu- mina powder is then lightly brushed off and white specks Three sets of data were used to compare several against black background are measured. macrostickies analysis methods. The first two sets were generated by using the various methods to measure the I In the CTP Enzyme Method (Appendix 3), 25 g of pulp is macrostickies levels in the four laboratory-generated pulps. digested with cellulases for 12 hours. The pulp is then The area and number of stickies for these pulps are shown screened using an 80µm slotted screen plate. The screen in Tables 3 and 4. A third set of measurements was on rejects are collected on a filter paper, dried and non-tacky five pulps samples taken from process streams in the recy- contaminants are brushed off. Black carbon powder is cling mill. This data set is shown in Table 5. Results are sprinkled over the filter paper to enhance the contrast be- also displayed in Figure 2 for laboratory samples and Fig- tween stickies and the background. ure 3 for mill samples. Methods are designated as fol- lows: Hydrophobic Morplas blue dye is used by researchers at FPL (Appendix 4) to distinguish stickies from a white fi- A: Stora Enso modified INGEDE Method with air and ber background. They measure stickies on 150 µm (0.006”) brush (used only with mill samples). slotted Pulmac screen rejects as well as directly on B: Stora Enso modified INGEDE Method with air (used handsheets without the screening step. only with mill samples). C: CTP Enzyme Method. The team at the Stora Enso Duluth mill modified the D: INGEDE Method. INGEDE method by using pressurized air to blow off ex- E: Black Ink Method. cess alumina powder followed by light brushing. Image F: Blue Dye Method (using Pulmac Screen). analysis measurements were taken both before and after G: Blue Dye Method (without using Pulmac Screen). the brushing step. They used 17 g to 25 g pulp samples in a Pulmac 100 µm (0.004”) slotted screening process. The sticky area data, shown in Table 3 and Figure 2, were analyzed using linear regression, t-testing, and F-testing. The pulp samples were generated Table 3. Average sticky area (sq. mm/kg) analysis results for four laboratory- using mixtures of differing propor- generated samples using five methods. tions of sticky-containing and clean Sample % of Analysis Method pulp. Because the sample variance introduced during the production of Sample 1 C D E F G the samples was likely very small, 1-Lab 100 8,350 27,266 18,041 9,063 28,682 an assumption was made that all the 2-Lab 75 6,835 25,455 11,634 6,989 11,614 observed variance was due to the 3-Lab 50 4,450 13,679 6,894 5,316 5,199 analysis methods.